Document 44BeVvRzYMDx8XJG022vyjbvx

/=9a^ ' 73 ^ % - PPG INDUSTRIES INDUSTRIAL CHEMICAL DIVISION LAKE CHARLES, LOUISIANA Subject3- rL L. ' ... j V:.- TRI-ETHANE & VDCM OPERATING MANUAL Orr?ej> FEBRUARY, 1971 SL 009959 MANUAL# .< CONFIW-;; OfS1u4btjhecJt utdoicFiraolLcD* istrict CoutV- No. 91-1145 TABLE OF CONTENTS Page INTRODUCTION ............................................................................................................ 1- 1 SAFETY.......................................................................................................................... 2- 1 Introduction .................................................................................................. General Safety Rules ................................................................................ Chemicals in the Area........................................................................... Special Safety Hazards ........................................................................... Emergency Horns......................................................................................... Fire Protection ..... .................................................................. Fire Extinguishers ..................................................................................... Safety Inspections................................ Vapor Detector System . ....................................................................... Equipment in the Area........................................................................... Clearing of Tanks and process Vessels ...................................... Safety Equipment................................................... Gas Masks....................................................................................................... Control Building............................ .... .............................................. . . Lab and Lab Hood Fan ................................................................................ 2- 1 2- 2 2- 4 2-49 2-52 2-53 2-55 2-55 2-55 2-57 2-58 2-58 2-59 2-59 2-59 GENERAL PROCESS DESCRIPTION ....................................................................... 3-1 DETAILED PROCESS AND EQUIPMENT DESCRIPTION TCE Section................................. ................................................................ Chemical Reactions ........................................................................... EDC Feed System................................................................................ Chlorine Feed System...................................................................... Ethylene Feed System...................................................................... TCE Reactor System........................................................................... HCl Purification and Distribution ...................................... Absorber Bottoms System ............................................................. Lights Still System ....................................................................... Relation of TCE Rx. Chlorination with Lights Still . Heavies Still System ....................................................................... Toxicity of Heavies Still Bottoms ...................................... TCE Rework Line................................................................................ 4- 1 4- 1 4- 2 4- 3 4- 6 4- 6 4-10 4-13 4-16 4- 20 4-21 4-26 4-27 VDC Section................................................................................................... Chemical Reactions ........................................................................... VDC Reactor and Still System.................................................... VDC Reactor Control....................................................................... VDC Still.............................................................................................. HQMME System......................................................................................... VDC Still Operating Conditions ............................................... VDC Drying System .................................................... ..... 4-28 4-28 4-30 4-36 4-37 4-39 4-39 4-40 SL 009960 CONFIDENTIALJ Subject to Protective Order of 14th Judicial District Court No. 91_li^5 page MC Section........................................................................................................ Chemical Reaction ........................................................................... MC Reactor System........................................................................... 1. VDC Vaporizer System....................................... . . 2. MC Reactor System..................................... 3. MC Reactor Operating Conditions ........................ Flasher - Dopp Kettles System............................................... Flasher - Dopp Kettle Operating Condition ................... MC Stripper System........................................................................... Stripper Operating Conditions ............................................... Topping Still System ....................................................................... Neutralizer - MC Drier System ............................................... MC Rework System................................................................................ 4-46 4-46 4-48 4-50 4-51 4-53 4-56 4-62 4-63 4-66 4-67 4-70 4-74 Tri-Ethane Stabilization and Storage Section ........................ Type 324 Stabilization System ............................................... Specialty Stabilization System .... ............................. Stabilizer Storage ........................................................................... Tri-Ethane Dock Storage ............................................................. 4-76 4-80 4-83 4-85 4-86 VDCM Section................................. .... ............................................................ VDCM Reactor System...................................................................... VDCM Still System........................................................................... VDCM Still Operating Conditions . . . ............................. VDCM Day Tank and Storage Tank System............................ 4-87 4-87 4-89 4-93 4-96 Utilities and Auxiliary Equipment ............................................... Steam and Condensate System.................................................... Cooling Tower Water System ........................................................ Well Water Recovery Tank............................................................. Nitrogen System................................................................................ Instrument Air System.................................................................. TCE Section Refrigeration System .......................................... Operation..................................................................................... Freon Flow..................................................................................... Oil Flow......................................................................................... Compressor Oil Flow............................................................. Compressor Safety Shutdowns ........................................... MC Section Refrigeration System .......................................... Special Discussion of Lapp Pumps .......................................... 4-99 4-99 4-101 4-102 4-103 4-104 4-105 4-106 4-108 4-110 4-113 4-114 4-117 4-118 STARTUP AND SHUTDOWN SECTION ...................................................................... TCE Section................................................................................................... 5- 1 5- 2 VDC Section................................................................................................... MC Section....................................................................................................... 5-12 5-13 SL 009961 r APPENDIX CONFIDENTIAL: Subject: to Protective Order f l4th `Judicial District Court No. 91-114 5 Tri-Ethane Process Flow Sheets Tri-Ethane Mechanical Flow Sheets VDCM Process Flow Sheet VDCM Mechanical Flow Sheet Well Water Recovery Flow Sheet Steam Traps in Tri-Ethane Plant Steam Traps in VDCM Plant DCA-MPN Reaction at 130F DCA-MPN Reaction at 93F MPN Requirement versus DCA Content Freezing Points of HQMME-VDC Mixtures SL 009962 CONFIDENTIAL: Subject to Protective Order t>f 14th Judicial District Court No. 91-1145 INTRODUCTION 1-1 The Tri-Ethane and VDCM areas are complex. The thorough understanding of safety and operating principles will make the work of all of us safe and profitable. This operating manual has three basic purposes: 1. To aid personnel in becoming familiar with the equipment, chemicals and operating procedures. 2. To serve as a ready source of reference. 3. To serve as a basic building block on which further improvements can be made. The manual has been arranged so that the Safety Section is at the front. This "Safety First" is the attitude of management and should be the attitude of each of us. The safe, successful operation of the plant depends on hpw each one of us performs. Revisions to the manual should be recorded on the next page. The date and reasons for the changes should also be recorded. SL 009963 Date Change No. TRI-ETHANE AND VDCM OPERATING MANUAL RECORD OF CHANGES Description Originator SL 0139964 2-1 safety section for tri-ethane and vdcm Introduction: This section is designed to cover the safety rules and pre cautions which must be adhered to while working in the Tri-Ethane and VDCM area. It is worthwhile to spend some time on the more general topic of workers attitude. The development of a safe operating plant and a work force of people who are safety conscious is based on the attitude of the people involved. Our attitude must be positlve--we must continually strive to do things safely. Our work must include continually looking for safer ways to do things. We must learn to care and watch out for others working with us. I may be aware of a safety hazard, but unless I correct the safety problem or properly worn all others of the problem I have not done my job. Safety is a continuing and vitally necessary part of every jpb we perform. We must recognize our responsibility, use our powers of observation and perception to seek out safety hazards and act to get problems solved. Each one of us must TAKE PART. CONFIDENTIAL: Subject to Protective Order of 14th Judicitil District Court No. 91-1145 Si- 009965 2-2 GENERAL SAFETY RULES FOR THE TRI ETHANE-VDCM AREA The following list of general safety rules is applicable to the Tri-Ethane area. They are to be used in conjunction with the Employee's Safety Manual until further revisions are made. The Tri-Ethane area has been included in Zone No. 16 in the present zone system along with EDC. The Directional Center will be located inside the east door of the Control Building. Rules 1. Personnel entering the Organics area will deposit lighters, matches, regular flashlights, etc., at the gate to this area. 2. Smoking will be permitted in the control room only. Permanent lighters will be supplied at this location. 3. The usual safety equipment will be required in the Organics area that is: a. Safety hats b. Chemical goggles (safety glasses under the goggles are optional) c. Respirators d. Plastic-coated gloves 4. The established plant tagging procedure will apply in the Organics Area. 5. Company vehicles only will be allowed to travel the road to the Control Building without a permit. 6. A vehicle permit signed by the operating supervisor or lead operator will be required for any vehicle to go north of the main pipe rack in the area. 7. An equipment permit signed by the operating supervisor will be required before the following equipment can be carried into the Organics area: a. Welding machines, b. Cutting torches c. Electrically driven drills d. Any electrical equipment except explosion-proof flashlights 8. Only explosion-proof flashlights will be permitted in the Organics Area. 9. Regular plant utility hoses are not to be used for handling organics. For Organics use Teflon lined hoses equipped with proper quickconnect fittings and bleed-off valve. CONFIDENTIAL: of S1u4btjhecJtuuttddooiiccipPi,aroi i:r"''-"4M- ivve Order No. 91- j. 2-3 10. All light circuits outside the Control Building must be off and tagged out before relamping of the area. 11. The grounding system for electrical equipment is inside the feeder conduit. This ground must be connected before the connection cover is installed. 12. Do not dump flammable organics into trapped sewers or openings where harmful vapors could be evolved. 13. Do not leave an open sample or container of organics sitting around to give off vapors. 14. Use Full-Face or Scott Air-Pak mask for protection against organic vapors. 15. Do not trap liquid chlorine in the vaporizer or surge drum. 16. Clothing that has been wet with organics should be removed immediately and the body thoroughly washed with soap and water. These clothes should be properly laundered before they are used again. 17. Do not permit air to enter any of the process equipment that contains organics. 18. In case of an emergency warning, all vehicles and equipment in the area on permits will be shut off immediately. 19. All steam-out nozzles or hose and purge equipment must be properly grounded to prevent the possibility of an arc from accumulated static charge. 20. Do not permit chlorine to be heated above 300F due to decomposition and reaction with metals, 21. No smoking or open flames will be allowed in the control laboratory. 22. The laboratory hood fan is to operate continuously. Do not attempt to run analyses without the fan being in service. 23. Always put liquid organics into tanks through standlegs or through bottoms nozzles. Falling liquid can generate static electricity. SL 009967 e, . CONFIDENTIAL: of 14th to Protective Judicial nistti. No, 91-1145 Order - Ccurt 2-4 CHEMICALS IK THE TRI-ETHANE AND VDCM AREA Name Abbreviation Acetaldehyde 1,1-Dimethyhydrazone ADH Azobisisobutyronitrile AIBN 1,2 Butylene Oxide BLM Calcium Chloride ChC I2 Caustic Soda (lye) NaOH Cell Liquor/Press Wash NaOH-aqueous Chlorodiflouromethane Freon 22 Chlorine cl2 Dichloroacetylene DCA 1,4 Dioxane DOX Dioxolane DOL Ethylene - c2h4 Ethylene Dichloride EDC Ethylene Glycol Dimethyl Ether DOE Ferric Chloride FeCl3 Hydrogen Chloride HC1 Hydroquinone Monomethyl Ether HQMME Isobutanol IBL Methyl Chloroform MC Methyl Ethyl Ketone bte' Monochloroacetylene MCA Morpholine Nitrogen MPN n2 Nitromethane nre Normal Propanol SL 009968 CONFIDENTIAL: f tD Prote^tjve Order of 14th Judicial District Court Ko. 91-1145 Page 2-7 2-8 2-9 2-10 2-11 2-12 2-21 2-13 2-14 2-15 2-16 2-17 2-18 2-19 2-20 2-22 2-23 2-24 2-25 2-26 2-27 2-28 * 2-29 2-30 2-30a Name _____________________________ Orthodichlorobenzene Pentach1oroe thane Phenol Propargyl Alcohol 1,1,2 Trichloroethane Secondary Butyl Alcohol Symmetrical and Unsymetrical Tetrachloroethane Toluene Tertiary Amyl Alcohol Tertiary Butyl Alcohol Tricresyl Phosphate Triphenyl Phosphite Vinylidene Chloride Abbreviation 0-DCB PCE Same PPL TCE SBL s-TeCE u-TeCE TLE TAL TBL TCP Tpp VDC 2-5 Page 2-31 2-32 2-33 2-36 2-37 2-38 2-39 2-43 2-44 2-45 2-46 2-47 2-48 confidential; Subject to Frotecti^ orl,:r t Of 14th SL 009969 2-6 DEFINITION OF TERMS USED Some of the terms used in the following discussion are defined below: 1. Flash point: The flash point of a solvent is the lowest temperature at which a vapor is given off in sufficient quantities so that the vapor-air mixture above the surface of the solvent will propagate a flame away from the source of ignition. It is the temperature below which a solvent may be used or stored in open containers without formation of an explosive vapor-air mixture. 2. Explosive limits: When combustible vapor is mixed with air in the proper proportions, ignition will produce an explosion. The vaporair mixture which will form this proper proportion is called the explosive range. The explosive range includes all concentrations of a mixture of flammable vapor or gas in air in which a flash will occur or a flame will travel if the mixture is ignited. The lowest percentage at which this occurs is the lower explosive limit and the highest percentage is the upper explosive limit. Explosive limits are expressed in percent by volume of vapor in air. 3. Maximum Allowable Concentration (MAC): The maximum allowable concen tration for a material is the maximum concentration of that material that can be tolerated by personnel for a continuous 8 hour exposure with no ill effects. CONFIDENTIAL: Subject to Protective Order Judicial District Court of 14th Mo. 91-U45 SL 009970 2-7 NAME: Acetaldhyde 1,1 Dimethyhydrazone (ADH) FORMULA: -(CH3)2 N-NCHCH3 MOLECULAR WEIGHT: 86 BOILING POINT: VAPOR PRESSURE: FREEZING POINT: LIQUID DENSITY: RELATIVE VAPOR DENSITY: FLASH POINT: EXPLOSIVE LIMITS: t MAXIMUM ALLOWABLE CONCENTRATION: DETECTABLE ODOR CONC.: HAZARDOUS PROPERTIES: ADH is poisonous. It is fatal by absorbtion through the skin, from the lungs or in open wounds. It is not fatal if it is washed off of the body immediately. Inhalation of the fumes can be fatal, unless you are using an activated carbon respirator. ADH is re ceived in a mixture of trichloroethylene, but is still concentrated to make all the hazardous properties apply. TREATMENT: Remove contaminated clothes and wash contacted area immediately with soap and water. Do not wear clothes splashed with ADH until they have been thoroughly washed. If the eyes become contaminated flush them immediately with water for 15 minutes. For inhalation, remove patient from contaminated area. Give artificial respiration. Give oxygen, if necessary. Report to First Aid in all cases. SL 009971 order 9SthCt^to i#9i.pnis-- r r ct court of NO 2-8 NAME: Azobisisobutyrcmitrile (AIBN) FORMULA: CH3 CH3 CH3 - - N = N - t - CH3 ch3 ch3 (CH3)3 C-N=N-C(CH3)3 MOLECULAR WEIGHT: 142 BOILING POINT: Solid VAPOR PRESSURE: Solid FREEZING POINT: Solid LIQUID DENSITY: Solid RELATIVE VAPOR DENSITY: Solid FLASH POINT: Unknown EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONCENTRATION: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Avoid heating AIBN in the open because it decomposes, releasing nitrogen and highly toxic by-products. AIBN should be stored at temperatures not exceeding 75F. It is classified as a flammable solid. Solid material in bulk form will not detonate or explode on impact nor can it be ignited by an instantaneous electrical spark. Self-heating begins in sealed fiber drums to about 1,20F with momentary ignition and mild explosion occurring as the temperature reaches 140F. Dry, solid AIBN can be ignited readily with an open flame or a continuous electrical arc. AIBN dispersions in air are explosive. They are extremely easy to ignite, and, in comparison with organic dusts, develop more forceful decomposition at exceedingly rapid rates. TREATMENT: Wash contaminated area with soap and water. Remove contaminated clothing. Flush eyes with water for a minimum of 15 minutes. If inhaled, remove patient from contaminated area. SL 009972 2-9 NAME: 1,2-Butylene Oxide (BLM) FORMULA: CH2-CHCH2CH3 0 MOLECULAR WEIGHT: 72.1 BOILING POINT: 148F VAPOR PRESSURE <a 75F: 198 mm FREEZING POINT: LT -76F <* LIQUID DENSITY <a 77F: 6.87 #/gal., 0.826 gm/ml RELATIVE VAPOR DENSITY: 2.49 (air =1.0) r FLASH POINT: -25F Open Cup, -15F Closed Cup EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Butylene oxide is moderately toxic upon oral intake. This material is moderately irritating to the eyes, resulting in slight pain and transient corneal injury upon contact. It is markedly irritating and damaging to the skin, especially when confined as when contaminated shoes and clothing are worn. Contact with uncovered skin may cause no more than a mild reddening and some drying of the skin. The vapors are quite irritating, and, if present in the atmosphere in high enough concentration, can cause acute and severe upper respiratory irritation resulting in breathing difficulties. Butylene oxide is extremely flammable and a dangerous fire hazard. It is also capable of violent reactions when in contact with acids, bases and certain metal salts so care should be taken to avoid mixing butylene oxide with any unknown materials or handling it in contaminated containers. TREATMENT: Remove and wash contaminated clothing. Wash exposed body surfaces thoroughly with soap and water. If eye contact is experienced flush with copious quantities of water for 15 minutes. Notify a physician immediately. SL 009973 2-10 NAME: Calcium Chloride FORMULA: CaCl2 MOLECULAR WEIGHT: 110.99 BOILING POINT: 1600C MELTING POINT: 772C SOLUBILITY IN WATER: 59.5 parts CaCl2/100 parts H20 at 9 C 347 parts CaCl2/100 parts H2O at 260 C DENSITY: 2.512 g./cc. at 25C RELATIVE VAPOR DENSITY: Normally a solid FLASH POINT: None EXPLOSIVE LIMITS: None HAZARDOUS PROPERTIES: Generally speaking, calcium compounds should be con sidered toxic only when they contain a toxic component (such as arsenic, etc.) or as calcium oxide or hydroxide. The hydration of the anhydrous salt is exothermic (21.7 cal./mole to form the hexahydrate). Thus, when driers are being flushed out with water there is the possibility of heat and some splashing which may carry CaCl2 solution into the operator's eyes. If CaCl2 solution enters the eye(s), a sustained water flush will be most effective in removing the material. Flush at least 15 minutes, then report to First Aid. SL 009974 2-11 NAME: Caustic Soda (lye) FORMULA: NaOH MOLECULAR WEIGHT: 40.01 BOILING POINT: 2532F CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 VAPOR PRESSURE: Normally a solid, but can be mixed with water to form a solution. FREEZING POINT: 604F HAZARDOUS PROPERTIES: When mixed with water, will react violently, splashing caustic solution on anyone nearby. Caustic soda in the form of solid, flake, or liquid attacks any tissue upon contact. The degree of injury depends upon the extent and duration of contact, temperature of the materials, and concentration of the materials. TREATMENT: Flush the contacted area immediately with an abundance of water. Remove any clothing or equipment that has been saturated with caustic. After thoroughly flushing the contacted area of the body with water, report to First Aid for further treatment. Eyes should be irrigated at once with plenty of warm water for at least 15 minutes anytime caustic comes in contact with the eye. SL 009975 2-12 NAME: Cell Liquor/Press Wash FORMULA: Aqueous solution of NaOH LIQUID DENSITY @ 77F: 100 #/gal., 1.1 gm/ml HAZARDOUS PROPERTIES: Cell liquor is an aqueous solution of sodium hydroxide (caustic) and salt and as such should be handled with the caution given any caustic solution. This material has a markedly corrosive action upon all body tissues, and skin contact may result in moderate to severe chemical burns if the exposed surface is not washed immediately. Eye contact is quite painful and can result in impairment of vision, TREATMENT: Speed in removing cell liquor from contact with the body is important to avoid injury. Removal of all contaminated clothing and thorough washing of the exposed surface is essential. If the eyes are involved they should be irrigated at once with plenty of warm water for 15 minutes. Call a physician. CONFIDENTIAL: Subject to Protective Order Of 14 th Judicial District Court No. 91-1145 SL 009976 2-13 NAME: Chlorine (CI2) FORMULA: Cl2 MOLECULAR WEIGHT: 70.91 BOILING POINT: -30F VAPOR PRESSURE @ 75F: 92 psig > / CONFIDENTIAL: Subject to Protective Order 14th Judicial District Court No. 91-1145 FREEZING POINT: -148F LIQUID DENSITY @ 77F: 11.6 #/gal., 1.391 gm/tnl RELATIVE VAPOR DENSITY: 2.45 (air =1.0) FLASH POINT: None EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC: 0.35 to 2 ppm DETECTABLE ODOR CONC: 3.5 ppm HAZARDOUS PROPERTIES: Liquid chlorine is very dangerous to the eyes as is chlorine gas. High concentrations of chlorine gas can cause pneumonitis and edema of the lungs. Lung irritation is one of the most serious effects of chlorine. CI2 is about 2 1/2 times as heavy as air, therefore, it has a tendency to collect in the low spots or stay near the ground. TREATMENT: Remove patient from toxic area and loosen all constrictive clothing about the neck. Oxygen should be administered in all cases to prevent cyanosis and relieve the pain of deep respiratory effort. Notify a physician. SL 009977 2-14 NAME: Dichloroacetylene (DCA) FORMULA: C2CI2 MOLECULAR WEIGHT: 94.94 BOILING POINT: 32C (89.6F) VAPOR PRESSURE FREEZING POINT: -65C (-85F) LIQUID DENSITY RELATIVE VAPOR DENSITY: EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONCENTRATION: Unknown DETECTABLE ODOR CONCENTRATION: Unknown HAZARDOUS PROPERTIES: Dichloroacetylene is a gas with a disagreeable sweetish odor, narcotic and poisonous and causes nerve and eye symptoms. Naval personnel exhibited severe nausea and facial sensory disturbances while exposed to traces of DCA in a test chamber. Dichloroacetylene is explosive and spontaneously flammable in air, burning to release phosgene. It is an explosive hazard when shocked or exposed to heat. When heated to decomposition or in contact with acid or acid fumes, it emits highly toxic fumes of chlorides. It can react vigorously with oxidizing materials. TREATMENT: Remove patient from the area and consult a physician immediately. 009978 2-15 NAME: 1,4 Dioxane (DOX) FORMULA: ^ch2 ch2 n 00 nch2 ch2x MOLECULAR WEIGHT: 88.11 BOILING POINT: 214 VAPOR PRESSURE AT 68?F: 27 mm Hg FREEZING POINT: 53F 0t W* LIQUID DENSITY: 8.64 #/gal. @ 68F RELATIVE VAPOR DENSITY: FLASH POINT: EXPLOSIVE LIMITS: L.E.L. 2.07= (Vol.) U.E.L. 227= (Vol.) MAXIMUM ALLOWABLE CONC: 100 ppm per 8 hour day DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: Dioxane is a volatile and flammable ether. It should be stored under a nitrogen atmosphere for two reasons: 1. To prevent formation of an explosive vapor-air mixture, 2. To minimize peroxide formation by exclusion of oxygen. Inhalation in large doses is hazardous. Oral ingestion is moderately hazardous. Kidney damage can result after massive or prolonged skin contact. Skin irritation can result from short duration contact by Dioxane. Eye damage can result from liquid entering the eye. TREATMENT: Remove patient from area. Wash any contaminated area thoroughly with soap and water. If DOX is splashed in the eyes, flush thoroughly with water for 15 minutes. Notify a physician immediately. SL 009979 2-16 NAME: Dioxolane (DOL) FORMULA: OCH2CH2OCH2 MOLECULAR WEIGHT: 74 BOILING POINT: 168F VAPOR PRESSURE @ 68F: 79 mm Hg 0 *"* Nw- FREEZING POINT: -143F LIQUID DENSITY: 7.77 if/Gal. (DOL/IBL Mixture) at 68F FLASH POINT: 56F EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Dangerous fire hazard when exposed to heat or flame can react vigorously with oxidizing materials.* DOL burns violently and can form explosive vapor-air mixture. It is moderately toxic. TREATMENT: Remove contaminated clothing and flush affected area with copious quantities of water. If the eyes become contaminated, flush them immediately with water for 15 minutes. For inhalation, remove patient from contaminated area. Report to First Aid. *Note: DOL will form explosive peroxides on contact with air. SL 009980 2-17 NAME: Ethylene FORMULA: C2H4 MOLECULAR WEIGHT: 28.05 BOILING POINT: -155F FREEZING POINT: -273F RELATIVE VAPOR DENSITY (air -1.0): 0.98 AUTOIGNITION: 1009F EXPLOSIVE LIMITS: 3 - 29% (Volume) ODOR: Sweet HAZARDOUS PROPERTIES: Ethylene is a flammable gas. It is a very dangerous explosion hazard upon exposure to heat or flame. It can react vigorourly with oxidizing materials. Ethylene is moderately toxic, but the slight effects disappear as soon as the patient is removed from the exposure. The main danger with C2H4 is asphyxiation. The ethylene will displace the oxygen of the air causing the victim to suffocate. TREATMENT: Remove the patient from the area, perform artificial respiration if breathing has stopped. Report to First Aid. SL 009981 2-18 NAME: Ethylene Dichloride (EDC) FORMULA: CH2ClCH2Cl MOLECULAR WEIGHT: 98.97 CONFIDENTIAL: BOILING POINT: 182.3F VAPOR PRESSURE @ 75F: 75 mm FREEZING POINT: -31,8F LIQUID DENSITY <? 68F: 10.45 #/gal., 1.253 gm/mls RELATIVE VAPOR DENSITY:, 3.41 (air = 1.0) FLASH POINT: 65F Open Cup; 55F Closed Cup EXPLOSIVE LIMITS: 6.2 to 15.9% by vol. in air MAXIMUM ALLOWABLE CONC: 75 to 100 ppm DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Ethylene dichloride is a flammable liquid and a dangerous fire hazard.' It is toxic by inhalation, by prolonged or repeated contact with the skin or mucous membranes, and by ingestion. Excessive contact gives rise to symptoms such as headache, depression, mental confusion, fatigue, loss of appetite, nausea, vomiting, cough, loss of sense of balance, and visual disturbances. It has an anesthetic effect, and, in high concentrations, is immediately irritating to the eyes, skin, nose, and throat. It can cause dermatitis upon prolonged or repeated contact with the skin. Ethylene dichloride can cause serious eye damage. TREATMENT: Quick removal from exposure is important. Ethylene dichloride should be removed from the patient's person, his respiratory tract, skin, or gastrointestinal tract as quickly as possible. If breathing has ceased, start artificial respiration. If material gets in the eyes, wash promptly with copious quantities of water. If ingested, the patient should be made to vomit. Notify a physician. SL 009982 2-19 NAME: Ethylene Glycdl Dimethyl Ether (DOE) FORMULA: CH3OCH2GH2OCH3 MOLECULAR WEIGHT: 90.12 BOILING POINT: 185F VAPOR PRESSURE @ 68F: 48 mm Hg FREEZING POINT: -92F LIQUID DENSITY @ 68F: 7.24 #/gal., 0.8683 gm/ml RELATIVE VAPOR DENSITY: 3.11 (air =1.0) FLASH POINT: 34F Open Cup EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: The hazardous properties of ethylene glycol dimethyl ether have not been fully evaluated. Consequently caution should be taken when handling this material. Avoid skin contact and inhaling the vapors. One important hazard involved with DOE is the formation of peroxides when it contacts air for an extended period of time. This is the same hazard that is encountered with VDC. Always keep the DOE drums under a nitrogen pad when in use and do not store partially full drums. Flush all empty drums and equipment that has come in contact with DOE with water. TREATMENT: Handle as any other toxic organic compound. Remove any con taminated clothing and wash exposed surfaces with soap and water. Flush eyes thoroughly with water. Administer artificial respiration if victim is overcome by vapors. Notify a physician immediately. 2-20 NAME: Ferric Chloride FORMULA: FeCl3 MOLECULAR WEIGHT: 162.2 BOILING POINT: 590F VAPOR PRESSURE @ 75F: nil SUBLIMATION POINT: 572F SPECIFIC GRAVITY: 2.8 RELATIVE VAPOR DENSITY: Normally a solid FLASH POINT: None EXPLOSIVE LIMITS: None HAZARDOUS PROPERTIES: Ferric chloride presents no particular problem in handling. However, in the anhydrous form, it may be injurious to clothing, and all contamination of both skin and clothing should be washed off immediately. In the case of eye contact, flush immediately and thoroughly with water and then rinse with a weak solution of sodium bicarbonate or boric acid. A physician should always be con sulted in such cases. Ferric chloride will seriously stain clothing and skin when it is contacted so it is advisable to wear gloves and aprons when handling it. Ferric chloride is extremely hygroscopic (absorbs water), and when this takes place, heat release occurs.* When taking material from a drum, remove the desired quantity as quickly as possible and immedi ately seal the drum to prevent it from absorbing moisture from the air. *Remove the drum lid carefully to relieve any pressure that may be built up inside. 0099&A 2-21 NAME: Freon-22 (chlorodifloromethane) FORMULA: C1HCF2 MOLECULAR WEIGHT: 86.465 BOILING POINT: -40.8C MELTING POINT: -146C VAPOR PRESSURE: @ 24C., 7,600 mm. Hg. RELATIVE VAPOR DENSITY: 3.87 (air =1.0) FLASH POINT: None EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC.: Unknown DETECTABLE ODOR CONC.: Unknown HAZARDOUS PROPERTIES: Freon-22 is very dangerous when heated to decomposi tion. It emits highly toxic fumes of chlorides and fluorides. Never allow any open flames to come in contact with Freon-22 or any vessels containing it. su 009985 2-22 NAME: Hydrogen Chloride FORMULA: HC1 MOLECULAR WEIGHT: 36.47 BOILING POINT: -121F VAPOR PRESSURE @ 75F: 36,000 mm FREEZING POINT: -174F LIQUID DENSITY: Normally a gas RELATIVE VAPOR DENSITY: 1.26 (air = 1.0) FLASH POINT: None EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC: 10 ppm for 8 hour working day DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Anhydrous hydrogen chloride is a gas which has a corrosive action upon the skin or mucous membranes. In this form, it will cause rapid and severe burns. It is particularly dangerous to the eyes. It is not flammable; however, the gas is highly soluble in water forming hydrochloric acid, which attacks most metals with the evolution of explosive hydrogen. TREATMENT: Immediate removal from the toxic area and thorough flushing of the patient's body and/or eyes with large quantities of water is of primary importance. Contaminated clothing should be removed from patient while he is being showered with water. It is essential that all affected body surfaces be washed with copius quantities of water for a sufficient time to remove all hydrochloric acid. No attempt should be made to neutralize the acid with alkaline solutions. Medi cal assistance should be summoned at the earliest possible moment. 0099&& 2-23 NAME: Hydroquinone Monomethyl Ether (HQMME) SYNONYMS: p-Methoxy phenol MOLECULAR WEIGHT: (theoretical) 124.13 APPEARANCE: White crystals MELTING POINT: 129 - 132F BOILING POINT: 470F FLASH POINT OPEN CUP: 270F HAZARDOUS PROPERTIES: Prolonged skin contact may cause irritation or burns. Systemic intoxication from industrial use is unlikely, but heavy dust exposure should be avoided. General body contact should be avoided. TREATMENT: In case of body contact, wash thoroughly all skin areas with water. Clothing should be removed only if completely saturated with dust or crystals. Laundry before reusing. In case of eye contact, prompt irrigation with water should prevent injury. Note: A solution of HQMME in VDC has caused severe chemical burns. cL 009987 2-24 NAME: Isobutanol (IBL) FORMULA: (CH3)2CHCH2OH MOLECULAR WEIGHT: 74 BOILING POINT: 226F VAPOR PRESSURE: 8 mm ( 68F FREEZING POINT: -162F LIQUID DENSITY: 7.77 #/gal. (DOL/IBL Mixture) at 68F RELATIVE VAPOR DENSITY: FLASH POINT: 95F Auto ignition temp, is 800F EXPLOSIVE LIMITS: LEL 1.68 MAXIMUM ALLOWABLE CONC: DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: Moderate fire hazard when exposed to heat or flame. Moderate explosion hazard in the form of vapor when exposed to heat or flame. Emits highly toxic fumes when heated. TREATMENT: Remove contaminated clothing and flush with copious quantities of water. If eyes are contaminated flush with water for 15 minutes. For ingestion, induce vomiting. ' Report to First Aid. SL 009988 2-25 NAME: Methyl Chloroform (MC) also known as 1,1,1 Trichloroethane FORMULA: CCI3CH3 MOLECULAR WEIGHT: 133.42 BOILING POINT: 165F VAPOR PRESSURE @ 77F: 125 mm FREEZING POINT: -22.7F LIQUID DENSITY @ 77F: 11.1 #/gal., 1.3314 gm/tnl RELATIVE VAPOR DENSITY: 4.60 (air =1.0) FLASH POINT: None EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC: 500 ppm for 8 hour exposure DETECTABLE ODOR CONC: 20 - 100 ppm HAZARDOUS PROPERTIES: Methyl chloroform is not as toxic as other chlorinated hydrocarbons such as aarbon tetrachloride; however, it can still cause damage to the body upon repeated or continuous exposure to large quantities of vapors or liquid.' Moderate exposure is unlikely to produce injury. Methyl chloroform is readily absorbed through the lungs. In acute ex posure, the most important toxic action is a functional depression of the central nervous system leading ultimately to respiratory failure. As With most solvents, dermatitis may result from repeated skin con tact, but methyl chloroform is only poorly absorbed through the skin. Eye contact may result in pain and discomfort, but no impairment of vision is likely. TREATMENT: As with other materials of this nature, remove the victim to an uncontaminated atmosphere and apply artificial respiration if breathing has stopped. Remove wet clothing and do not allow it to be reworn until it is thoroughly dry. If eyes are contaminated, they should be flushed with large amounts of water. Notify a physician immediately. SL 009989 2-26 NAME: Methyl Ethyl Ketone (BTE) FORMULA: CH3COC2H5 MOLECULAR WEIGHT: 72.1 BOILING POINT: 175F VAPOR PRESSURE: 70 ram @ 20C FREEZING POINT: -277F LIQUID DENSITY: 6.71 #/gal. @ 68F RELATIVE VAPOR DENSITY: FLASH POINT: Unknown EXPLOSIVE LIMITS: 1.81% - 11.5% MAXIMUM ALLOWABLE CONC: 250 ppm DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: BTE is a dangerous fire hazard when exposed to heat or flame; it can react with oxidizing material. BTE is a low flash flammable liquid and its vapors form explosive mixtures with air over a fairly wide range of concentrations. It is also quite volatile and the vapor is heavier than air. TREATMENT: Remove contaminated clothing and wash affected area with warm water and soap. Wash eyes with water for 15 minutes. Induce vomiting if swallowed. Remove patient from area. Give artificial respiration if required. Report to First Aid. SL 009990 2-27 NAME: Monochloroacetylene (MCA) FORMULA: C2HC1 MOLECULAR WEIGHT: 60.483 BOILING POINT: -31C (-23.8F) VAPOR PRESSURE FREEZING POINT LIQUID DENSITY RELATIVE VAPOR DENSITY: EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONCENTRATION: Unknown DETECTABLE ODOR CONCENTRATION: Unknown HAZARDOUS PROPERTIES: MCA is an explosive gas which is spontaneously flammable in air. Monochloroacetylene forms an explosive yellowish-red salt with ammonical cuprous solution. Aqueous solutions in contact with air display luminescence. MCA gas is colorless, has a nauseating odor, is irritating to the respiratory tract and is highly toxic. TREATMENT: Remove patient from the area and consult a physician immediately. SL 009991 2-28 NAME: Morpholine (MPN) FORMULA: C4Hg-ONH MOLECULAR WEIGHT: 87.12 BOILING POINT: 264F VAPOR PRESSURE @ 70F: 7.0 mm Hg FREEZING POINT: 23F SPECIFIC GRAVITY (<3 68F: 1.0017 WEIGHT AT 68 F., lbs./gal.: 8.3 HAZARDOUS PROPERTIES AND TREATMENT: Undiluted morpholine is moderately irritating to skin and very irritating to eyes. As with other caustic materials, dilution with water reduces this hazard, and only minor irritation would be expected from dilutions lower than 15%. Neverthe less, all spills on the skin should be washed off promptly with soap and water. If clothing has become saturated, it should be removed at once and affected skin areas thoroughly washed with soap and water. In case of eye contact, the eye should be continuously irrigated with water for at least 15 minutes. A physician should see all cases in which undiluted morpholine has splashed into the eye. Vapor concentrations of morpholine that are likely to develop under ordinary working conditions would constitute little immediate hazard to health. Acutely dangerous exposures might be expected to occur only after massive spills in closely confined areas. Although no threshold limit for morpholine vapor has been established, the breath ing of high concentrations should be avoided. A chemical cartridge respirator or gas mask,^offering protection against organic vapor, should be worn when entering vessels that have contained morpholine for purposes of cleaning or maintenance unless thoroughly flushed with water beforehand. SL 009992 C'ONF J DENT T a r.. Subject Of i144 tiil JJuU 2-29 NAME: Nitrogen FORMULA: N2 MOLECULAR WEIGHT: 28.02 PHYSICAL APPEARANCE: Colorless, Odorless, Inert Gas SPECIFIC GRAVITY: 1.0 with relation to air. (Air is 78% N2) HAZARDOUS PROPERTIES: Even though nitrogen is a very safe, inactive gas, it has some inherent dangers since it is used so universally through out the plant. Its prime use is for padding and sweeping of equipment that has, or has had, flammable organics in it. The hazard involved is that a vessel may have insufficient oxygen or that nitrogen is used to purge the vessel instead of air, before man-entry. Therefore, in the MC plant, every vessel that is entered not only must be first checked for flammability, etc,, it must also be checked for sufficient oxygen. Not only that, nitrogen lines, as well as toxic lines must be isolated from the vessel before entry and a clean air sweep provided. TREATMENT: Remove person from the oxygen deficient area. Administer artificial respiration if necessary. 00^3 2-30 NAME: Nitromethane (NEE) FORMULA: CH3N02 MOLECULAR WEIGHT: 61.04 BOILING POINT: 214F VAPOR PRESSURE @ 77F: 35.5 mm Hg FREEZING POINT: -20F LIQUID DENSITY @ 68F: 9.48 #/gal., 1.139 gra/ml RELATIVE VAPOR DENSITY: 2.11 (air = 1.0) FLASH POINT: 112F Open Cup, 95F Closed Cup EXPLOSIVE LIMITS: Lower Limit 7.3% MAXIMUM ALLOWABLE CONC: 100 ppm for 8 hour exposure DETECTABLE ODOR CONC.: 100 ppm HAZARDOUS PROPERTIES: Data on the effects in humans to repeated exposure over long periods is lacking. Absorption by the body is chiefly from inhalation. High concentrations produce evidence of mild respiratory tract irritation, then narcosis followed by death. The primary area of attack is the liver and kidneys. There is no evidence of skin absorption although mild irritations can occur due to its solvent action. While nitromethane is normally quite stable, it has been detonated by violent shock. Drums should be handled with care to avoid dropping and extreme rough handling. Violent explosive reactions can occur when nitromethane is mixed with some organic materials or metal oxides so care should be taken that it is never mixed with an unknown material and that any container into which nitromethane is put is absolutely clean. Do not expose NRE to dry caustic.* TREATMENT: Removal of the patient from the contaminated area is of utmost importance. Administer artificial respiration if breathing has stopped. Notify a physician. *Do not allow solution of NRE in bases to become dry. Certain mixtures of NRE and amines are sensitive. Some terniery mixtures of NRE, amines and heavy oxides can be very hazardous. SL 009994 2-30-a NAME: N-Propanol FORMULA: CH3CH2CH2OH MOLECULAR WEIGHT: 60.1 BOILING POINT: 97.19C VAPOR PRESSURE: 10 mm at 14.7C FREEZING POINT: -127C LIQUID DENSITY: 0.8044 at 20/4C VAPOR DENSITY: 2.07 o* FLASH POINT: 90F (O.C.) EXPLOSIVE LIMITS: 2.6% (lower; 13.5% (upper) in air MAX. ALLOWABLE CONCENTRATION (OR THRESHOLD LIMIT): 200 ppm DETECTABLE ODOR CONCENTRATION: Alcohol-like odor HAZARDOUS PROPERTIES: Flammable. Dangerous fire explosion and disaster hazards when exposed to heat or flame. Slightly toxic with no cumulative effect. TREATMENT: Skin: Remove contaminated clothing and wash with water, then soap and water. Eyes: Flush with copious quantities of water. Swallowing: Report to First Aid. Inhalation: Remove patient from contaminated area. Give artificial respiration. Give oxygen if necessary. Report to First Aid. SL 009995 2-31 NAME: Ortho Dichlorobenzene FORMULA: CgH^C^ MOLECULAR WEIGHT: 147 BOILING POINT: 357F VAPOR PRESSURE: 1.2 mm @ 77F FREEZING POINT: +0.5F LIQUID DENSITY: 10.8 #/gal. <? 68F RELATIVE VAPOR DENSITY: v ec. <-<0* v&- Cv A 9V ,vv FLASH POINT: 166F MAXIMUM ALLOWABLE CONC: 50 ppm DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: Moderate fire hazard when exposed to heat or flame. At elevated temperatures, flammable vapors are given off. When heated to decomposition, it emits toxic fumes of chlorides; can react vigorously with oxidizing materials. TREATMENT: Remove contaminated clothing. Flush skin with water, then wash with soap and water. Flush eyes immediately with water for 15 minutes. If ingested, induce vomiting. In the case of inhallation, remove patient to fresh air and keep warm. Use artificial respiration if necessary to restore breathing. In all cases report to First Aid. SL 009996 2-32 NAME: Pentachloroethane (PCE) FORMULA: CCI3CHCI2 MOLECULAR WEIGHT: 202.31 BOILING POINT: 321F VAPOR PRESSURE <a 75F: 4 mm FREEZING POINT: -20F LIQUID DENSITY @ 77C: 14.0 #/gaI., 1.681 gm/ml RELATIVE VAPOR DENSITY: 6.98 (air =1.0) FLASH POINT: None EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC: Below 121 ppm DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Pentachloroethane is a nonflammable and toxic liquid. It has a chloroform-like odor and can cause chronic intoxication. It is considered a stronger narcotic than chloroform and is about as poisonous as tetrachloroethane, which it resembles in its action as a metabolic poison. It has a pronounced irritating effect upon the mucous membranes, causing an inflammation of the nose, throat, and respiratory passages. Chronic poisoning causes fatty degeneration of the liver, inflammation of the kidneys, bronchitis, pronounced hypej-emia of the lungs, and puru lent pneumonia. TREATMENT: As described under tetrachloroethanes. Notify a physician. SL 009997 2-33 NAME: Phenol FORMULA: C6H5OH MOLECULAR WEIGHT: 94.11 BOILING POINT: 359F VAPOR PRESSURE @ 75F: L.T. 1.0 FREEZING POINT: 107F LIQUID DENSITY @ 122F; 8.76 #/gal., 1.051 gm/ml RELATIVE VAPOR DENSITY: 3.24 (air =1.0) FLASH POINT: 185F Open Cup, 174F Closed Cup EXPLOSIVE LIMITS: None Reported MAXIMUM ALLOWABLE CONC: 5 ppm DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Phenol is highly toxic and dangerous when handled im properly. In liquid form, solid fqrm, or as a solution, it (1) exerts a local corrosive effect and (2) is readily absorbed through the skin and mucous membranes (either broken or intact), through the gastro intestinal tract, or through the lungs (either as a vapor or in droplet form) . After absorption, the toxic effects are exerted primarily on the central nervous system, but following sufficient exposure there may also be edema of the lungs, kidneys, liver, pancreas, and spleen. Exposure to fatal amounts usually results in death within a half hour after absorption. The signs and symptoms of absorption may develop rapidly, i.e., with in 20 to 30 minutes. Toxic manifestations are; profound muscular weakness, headache, dizziness, dimness of vision, ringing of the ears, irregular and rapid respiration, weak pulse, and difficult breathing, following occasionally by mental confusion, muscular twitching, loss of consciousness, and, in rare cases, death from respiratory failure. When taken internally, there is also nausea, with or without vomiting, and severe abdominal pain. Phenol has a marked corrosive action on any tissue upon contact. A serious burn may result unless the chemical is removed promptly and thoroughly. In case of failure to wash the phenol completely from all contaminated areas of the body in the very minimum of time, death may result, the possibility of this outcome depending upon the amount of phenol absorbed and the individual susceptibility to the toxic SL 009998 CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court Wo. 91-1145 2-34 effects of phenol. Although there is often no immediate sensation, prickling and intense burning appear after a few moments. This is followed by local anesthesia. Affected tissues show white discolora tion, wrinkling, and softening, initially, subsequently they become red, then brown or black (signs of gangrene). Absorption of the chemical following extensive burns may produce the general symptoms of toxicity enumerated above. Chronic poisoning from absorption of phenol through the skin, mucous membranes, or respiratory tract may occur following exposure to low concentrations for a prolonged period. Symptoms and signs of chronic poisoning are; digestive disturbances (vomiting, difficulty in swallow ing, excessive salivation, diarrhea, loss of appetite), nervous disorders (headache, fainting, dizziness, mental disturbances), and skin eruptions. Chronic poisoning may terminate fatally in those cases where there is extensive damage to the liver or kidneys. TREATMENT: SPEED IN REMOVING PHENOL IS OF PRIMARY IMPORTANCE 1 First aid should be started at once in all cases of contact with phenol in any form, or serious injury may result. Refer all injured persons to a physician immediately, even when injury appears to be slight. Give the physician a detailed account of the accident. Should respira tion cease, immediately start effective artificial respiration, such as that obtained by the Eve rocking method or by the prone pressure method. When phenol contacts the skin, remove ALL clothing to prevent further absorption of the chemical, i.e., to permit thorough removal of all phenol. Wash all affected areas with large quantities of water to which soap has been added, if it is immediately available; continue washing until all odor of phenol has disappeared. Keep patient warm, but not hot. No salves or ointments should be applied to chemical burns during the 24 hour period following the injury. For other than extremely minor burns, consult a physician at once. If phenol has entered the eyes, they should be washed promptly with copious quantities of water for at least fifteen minutes. A drinking fountain may be used for the initial, emergency irrigation, if necessary. However, it is advisable to irrigate the eyes gently with water at room temperature in order to minimize pain and discomfort. Consult a physician at once. Experience has shown that as little as 8.5 grams (0.3 ounce) of phenol taken internally and not removed may cause death. Therefore, call a physician immediately. Phenol taken internally is an extremely violent poison for which there is no known satisfactory antidote. It is of the utmost importance that large quantities of liquid (salt water, weak sodium bicarbonate solution, milk, or gruel) followed by a demulcent, such as raw egg whites or corn starch paste, be swallowed by the patient. SL 009999 2-35 and that profuse vomiting follow immediately thereafter. If the patient does not vomit spontaneously, give a mild emetic (e.g., a tablespoonful of mustard in a glass of warm water), or tickle the back of the throat. Repeat this procedure until the vomitus is free of the odor of phenol. It is advisable to leave some of the demulcent in the stomach after vomiting to act as a diluent and to "fix any residual acid, thus pre venting additional injury." Keep the patient comfortably warm. A physician should be consulted immediately. Tf quantities of phenol vapors have been inhaled, the patient should be removed immediately from the toxic vapor, or mist, to fresh air or an uncontaminated atmosphere. 010000 2-36 NAME: Propargyl Alcohol (PPL) H FORMULA: HO-C-C&C-H (2-Propyn-l-ol) H MOLECULAR WEIGHT: 56.06 BOILING POINT: 239F VAPOR PRESSURE: @ 68F 11.6 mm Hg FREEZING POINT: -61F e 0^' LIQUID DENSITY: 7.7 #/gal. RELATIVE VAPOR DENSITY: FLASH POINT: 97F kP^ 5v- * \. EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Propargyl Alcohol is a primary skin irritant and a severe eye irritant and as such the use of rubber gloves and safety goggles or a face shield is advised. As a lachrymater, PPL should be handled and stored only in well ventilated areas. PPL is toxic and accidental ingestion must be avoided. Contact with any alkaline materials at room or higher temperature should be avoided unless Propargyl Alcohol is dissolved in a solvent. Such conditions can promote uncontrollable decomposition resulting in explosions. If Propargyl Alcohol is dried with an alkaline drying agent (i.e., KOH, K2CO3), it should not be distilled without first acidifying slightly with succinic or acetic acid. Distillation of Propargyl Alcohol should not be carried to completion because the residues continuously become richer in easily decomposable materials. TREATMENT: Remove and wash contaminated clothing, Wash exposed body surfaces thoroughly with soap and water. If eye contact is experienced, flush with copious quantities of water for 15 minutes. Notify a physician immediately. SL 0)0001 2-37 NAME: 1,1,2-Trichloroethane (TCE) FORMULA: CHCl2CH2Cl MOLECULAR WEIGHT: 133.41 BOILING POINT: 237F VAPOR PRESSURE @ 75F: 22 mm FREEZING POINT: -34F LIQUID DENSITY & 77F: 11.93 #/gal., 1.4319 gtn/ml RELATIVE VAPOR DENSITY: 4.6 (air =1.0) FLASH POINT: None O*' v-X, EXPLOSIVE LIMITS: None MAXIMUM ALLOWABLE CONC: 25 to 100 ppm o* DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Trichloroethane can cause burns of the eyes and has a seriously harmful effect upon the liver. It has a local irritating effect upon the mucous membranes, particularly of the eyes and nose. All contact with the eyes and skin should be avoided. This material should generally be handled with caution, because its toxicological properties have not as yet been adequately evaluated. TREATMENT: Remove patient from toxic area. Remove all contaminated clothing and wash all exposed skin surfaces thoroughly with soap and water. Flush eyes with copious quantities of water. Notify a physician. SL 010002 2-38 NAME: Secondary Butyl Alcohol (SBL) FORMULA: CH3CH2CHOHCH3 MOLECULAR WEIGHT: 74.12 BOILING POINT: 212F VAPOR PRESSURE @ 75F; FREEZING POINT: -175F LIQUID DENSITY @ 68F: 6.74 #/gal., 0.808 gm/ml RELATIVE VAPOR DENSITY: 2.56 (air = 1.0) FLASH POINT: 75F Closed Cup EXPLOSIVE LIMITS: MAXIMUM ALLOWABLE CONC: 25 ppm DETECTABLE ODOR CONC: Less Than 25 ppm HAZARDOUS PROPERTIES: This material is a dangerous fire hazard. Secondary butyl alcohol can cause narcosis, dermatitis, liver degeneration and an increase in red blood cells. Excessive contact with the vapors causes inflammation of the eyes which can be quite painful. Symptoms of intoxication are irritation, dermatitis, coughing, as well as an unusual type of keratitis (deterioration of fingernails and hair). TREATMENT: Remove the patient from exposure and the symptoms will usually clear up. If it has been ingested, or if the patient has been overexposed to this material, consult a physician. SL 010003 CONFIDENT! M,: Subject t > FrotrTCivp of 14th ju:Ucj.-0 nO Order Court 2-39 NAME: Symmetrical and Assymmetrical Tetrachloroethane (S.TeCE & A.TeCE) FORMULA: CHC12CHC12 and CCl3CH2Cl MOLECULAR WEIGHT: 167.86 BOILING POINT: S.TeCE 295F; A.TeCE 267F VAPOR PRESSURE @ 73F: S.TeCE 4mm; A.TeCE 13 mm FREEZING POINT: S.TeCE -47F; A.TeCE -97F LIQUID DENSITY @ 77F: S.TeCE 1.588 gm/ml; RELATIVE VAPOR DENSITY: 5.78 (air - 1.0) FLASH POINT: None EXPLOSIVE LIMITS: None A.TeCE 1.533 gm/ml >V,'Acx V'1 CK'.o V -c' Vv0 '" MAXIMUM ALLOWABLE CONC: 5 ppm for 8 hour exposure DETECTABLE ODOR CONC: Approximately 5 ppm v HAZARDOUS PROPERTIES: The tetrachloroethanes are not flammable or explosive but are the most toxic of the chlorinated ethanes that will be handled in the plant. The tetrachloroethanes are toxic by inhalation, by prolonged and repeated contact with skin or mucous membranes or by oral intake. Although toxic, tetrachloroethanes may be handled safety if proper precautions are constantly observed. Prolonged or repeated exposures to the product in any form are hazardous. The signs and symptoms of excessive absorption usually appear gradually and only after repeated exposures. In order of appearance they commonly are unusual fatigue, loss of appetite and weight, sick stomach and vomiting, constipation, abdominal pain, jaundice, drowsiness, going on in severe cases to unconsciousness and death. Some cases show marked involvement of the nervous system with headache, numbness and tingling in fingers and toes, trembling and twitching of muscles and even paralysis of some muscles. The signs and symptoms of tetrachloroethane poisoning given above are due to systematic poisoning characterized by marked damage to the liver, kidneys, heart, blood cells, and nervous system. The clinical picture varies with the type of exposure and the amount of the material which has been absorbed either at one time or at repeated times. Most serious effects are usually on the liver and the blood. The principal route of absorption is by breathing the vapor, although it may be absorbed by the skin. Tetrachloroethane is currently considered the most toxic of the chlorinated hydrocarbon solvents in industrial use. SL 010004 CONFIDENTIAL: Subjec ^ to Protective Order of 14 th Judicial District Court No. 91-1X45 2-40 Continued exposure to high concentrations of the tetrachloroethanes leads to local irritation of the eyes and nose. There may be sick stomach and vomiting, bur since tetrachloroethane is less volatile than other hydrocarbon solvents, it does not often have an anesthetic effect. Subacute tetrachloroethane poisoning is the form usually encountered. This develops gradually as a result of prolonged or repeated work in an atmosphere containing more than 5 parts of tetrachloroethane per million parts of air but under conditions where the amount absorbed causes no immediate reaction. Repeated exposure even to low concentrations seems to increase sensitivity, and may lead to subacute poisoning. For some time, workers with subacute poisoning may show only such signs and symptoms as unusual fatigue, loss of appetite and weight, con stipation and abdominal distress or pain. At any time they may develop more severe evidence of absorption such as vomiting, dizziness, tendernes and pain over the liver, and jaundice. Even if removed from further ex posure, the illness may persist and grow worse over a period of days, weeks or even months, and may finally even end in death. However, if after a few months there has been steady improvement, complete recovery is the rule. Some conditions under which subacute poisoning may occur in employees are as follows: (a) Where the ventilation is inadequate, resulting in high concentra tions of more than 5 parts of tetrachloroethane per million of air. (b) Where the vapor concentrations are high intermittently, due to faulty handling of the liquid. (c) Failure of the individual to observe precautionary measures. Tetrachloroethane is absorbed through the skin so that systemic poisoning can occur by this route with the same signs and symptoms as described above. Tetrachloroethane may cause dermatitis after repeated or prolonged contact with the skin, such as that which might occur in the handling of rags wet with the chemical product, dipping hands into the liquid, or wearing clothing saturated with it. Reddening, burning, and, rarely, blisters may follow such exposure. In certain rate cases, the dermatitis may be caused by hypersensitivity to tetrachloroethane. The skin becomes rou^i , red and dry due to the removal of skin oils. It cracks easily and is readily susceptible to infection. The skin has a chapped appear ance . SL 010005 CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 2-41 Tetrachloroethane may enter the eyes either as a vapor or as liquid (spray or splash). The resultant irritation produces lacrimation, burn ing and other symptoms of inflammation. It can cause serious eye damage if immediate care is neglected. The first symptoms after toxic amounts of tetrachloroethane are taken by mouth are those of irritation of stomach and bowels, such as sick stomach, vomiting, and diarrhea with bloody stools. It is absorbed very rapidly and even a small amount may go on to produce unconscious ness and a deep flushing of the skin. Death is apt to occur before such systemic changes as liver and kidney damage occur. TREATMENT: Most important in the case of any poisoning is quick removal from exposure. In the case of tetrachloroethane poisoning, this means first removing the patient from the contaminated atmosphere and, insofar as possible, removing the tetrachloroethane from the patient's skin, or gastrointestinal tract, if those areas are involved. The patient should be kept quiet and comfortably warm, but not hot, A physician should be called immediately. He should be told briefly and clearly what has happened and the exact location of the patient. A person showing symptoms of tetrachloroethane vapor poisoning should be removed promptly from the contaminated area. In case breathing has stopped, effective artificial respiration, such as that obtained by the prone pressure method or the Eve rocking method should be started immedi ately. If oxygen inhalation apparatus is available, oxygen should be administered, but only if one familiar with the operation of the apparatus is present to administer it. If the patient is conscious, hot tea or coffee may be given as a stimulant. A physician should be called at once. All contaminated clothing should be removed at once. Clothing, in cluding shoes, soaked in tetrachloroethane should be removed and not worn again until thoroughly free from tetrachloroethane. All affected areas should be washed thoroughly with warm water and soap. After this, an ointment containing lanolin should be applied in order to help in replacing the natural skin oils. For serious or persistent cases of skin trouble, and for signs and symptoms of generalized poisoning, a physician should be consulted. If liquid tetrachloroethane has entered the eyes, they should be washed promptly with copious quantities of water for at least 15 minutes. (It is advisable to irrigate the eyes gentle with water at room tempera ture in order to minimize additional pain or discomfort.) Medical attention should be obtained in all cases involving contact with the e ye s. 010006 St 2-42 If a person has swallowed tetrachloroethane he should be made to vomit, if conscious, by having him drink a glassful or more of lukewarm water in which a teaspoonful of salt to the glassful has been dissolved; a similar amount of warm soapy water may be used. If necessary, the patient should be encouraged to stick his finger down his throat to induce vomiting. When possible, vomiting should be induced at least three times. Following this a tablespoonful of Epsom Salt dissolved in a glass of water should be given. A physician should be called at once. COt^o orA1 C"' t SL 010007 2-43 NAME: Toluene (TLE) FORMULA: C6II5CH3 MOLECULAR WEIGHT: 92.13 ROILING POINT: 231F VAPOR PRESSURE: 28 mm (<* 25C FREEZING POINT: -139F LIQUID DENSITY: 7.27 #/gal RELATIVE VAPOR DENSITY: FLASH POINT: 39F EXPLOSIVE LIMITS: 1.27 - 6.75% MAXIMUM ALLOWABLE CONC: 200 ppm DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: TLE is a high fire hazard and as such should always be kept under a N2 pad. TREATMENT: Remove contaminated clothing. If splashed in eyes, flush for 15 minutes. For inhalation, remove patient from area; administer artificial respiration if required to restore breathing. Report to First Aid. SL 010008 2-44 NAME: Tertiary Amyl Alcohol (TAL) FORMULA: (CH3)2COHCH2CH3 MOLECULAR WEIGHT: 88.15 BOILING POINT; 215F VAPOR PRESSURE @ 75F: 15 mm FREEZING POINT: 11F LIQUID DENSITY Q 68F: 6.75 #/gal., 0.81 gm/ml RELATIVE VAPOR DENSITY: 3.04 (air = 1.0) FLASH POINT: 75F Open Cup, 74F Closed Cup EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Tertiary amyl alcohol is a flammable liquid and a dangerous fire hazard. It'is considered to be very toxic, although little is known of its action on the body. The liquid and vapors are dangerous to the eyes. TREATMENT: Remove and wash contaminated clothing. Wash exposed body surfaces thoroughly with soap and water. If eye contact is experienced flush with copious quantities of water for 15 minutes. Notify a physician immediately. SL 010009 2-45 NAME: Tertiary Butyl Alcohol (TBL) FORMULA: (CH3)3COH MOLECULAR WEIGHT: 74,12 BOILING POINT: 180F VAPOR PRESSURE @ 75F: 38 mm FREEZING POINT: 78F *" LIQUID DENSITY (d 81F: 6.50 #/gal., 0.7793 gm/ml RELATIVE VAPOR DENSITY: 2.56 (air =1.0) FLASH POINT: 60F Open Cup, 48F Closed Cup EXPLOSIVE LIMITS: 2.4 to 8.0% by volume MAXIMUM ALLOWABLE CONC: 100 ppm DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: Tertiary butyl alcohol is a flammable liquid and a dangerous fire hazard. Skin contact causes inflammation of the skin and is normally considered as an irritant. All bodily contact should be avoided as well as high vapor concentration. TREATMENT: Remove and wash contaminated clothing. Wash exposed body surfaces thoroughly with soap and water. If eye cpntact is experienced flush with copious quantities of water for 15 minutes. Notify a physician immediately. SL 010010 2-46 NAME: Tricresyl Phosphate (TCP) FORMULA: (C6H4 - CH3 - 0)3 - PO MOLECULAR WEIGHT: 368.4 BOILING POINT: 788F VAPOR PRESSURE: Unknown FREEZING POINT: Below -3,1F LIQUID DENSITY: 9.7 #/Gal. RELATIVE VAPOR DENSITY: ' FLASH POINT: 470F (Cleveland Open Cup) EXPLOSIVE LIMITS: Unknown MAXIMUM ALLOWABLE CONC: Unknown DETECTABLE ODOR CONC: Unknown HAZARDOUS PROPERTIES: TCP is a slight fire hazprd'when exposed to heat or flame. When heated to decomposition, it emits highly toxic fumes of oxides of phosphorous. Avoid contact with the skin or inhalation of its vapors. TREATMENT: Wash exposed areas thoroughly wil:^ soap and water. If TCP is splashed in the eyes, irrigate the eye thoroughly with water for 15 minutes. Report to First Aid. 2-47 NAME: Triphenyl Phosphite (TPP) FORMULA: (C^O^P MOLECULAR WEIGHT: 3X0.28 BOILING POINT: 680F VAPOR PRESSURE: FREEZING POINT: 72F LIQUID DENSITY: 9.81 to 9.86 at 86/60F RELATIVE VAPOR DENSITY: Normally a liquid FLASH POINT: EXPLOSIVE LIMITS: MAXIMUM ALLOWABLE CONC:, ( DETECTABLE ODOR CONC: HAZARDOUS PROPERTIES: TPP is considered only slightly toxic from the standpoint of oral ingestion. Prolonged contact with the skin should be avoided to prevent skin irritation. TPP may irritate eye tissues but should not cause permanent damage. TPP is hygroscopic apd must betkept dry. It forms phenol when reacted with water, TREATMENT: Wash contacted skin area thoroughly with soap and water. If splashed in the eyes, flush eyes thoroughly with water for a minimum of 15 minutes. SL 01001? 2-48 NAME: Vinylidene Chloride (VDC) FORMULA: CC12CH2 MOLECULAR WEIGHT: 96.95 BOILING POINT: 89F VAPOR PRESSURE @ 75F: 560 mm FREEZING POINT: -187.6F LIQUID DENSITY (3 68F: 10.15 #/gal., 1.218 gm/ml RELATIVE VAPOR DENSITY: 3.35 (air =1.0) FLASH POINT: 5F Open Cup, 55F Closed Cup EXPLOSIVE LIMITS: 7.3% to 16.0% by volume in air MAXIMUM ALLOWABLE CONC: 25 ppm DETECTABLE ODOR CONC: 500 to 1,000 ppm HAZARDOUS PROPERTIES: Vinylidene chloride is a flammable and toxic material. Vinylidene chloride is moderately irritating to the eyes and to the skin. The greatest danger from vinylidene chloride is inhalation. A single exposure for a few minutes to a high concentration of vinylidene chloride vapor rapidly produces a "drunkenness" which may progress to unconscious ness if exposure is continued. Even concentrations too low to cause an anesthetic effect, may produce organic injury to the liver and kidneys. A secondary danger from vinylidene chloride exists. Unstabilixed vinylidene chloride in contact with air will decompose and form explo sive peroxides. These peroxides are evident by the presence of a white solid. For this reason, all vinylidene chloride will be stabilized and all equipment will be padded with an inert gas such as nitrogen or methane. TREATMENT: When the skin is contacted by vinylidene chloride it should be thoroughly washed with soap and water and all contaminated clothing removed and washed. If the eyes become contaminated, they should be flushed with water for 15 minutes or more. If a person is affected or overcome from breathing vinylidene chloride vapors, he should be removed to fresh air at once. Medical attention should be obtained immediately. Artificial respiration should be administered if breathing stops. SL 010013 SPECIAL SAFETY HAZARDS Subject CrpIDaTI.. Of i4fch Judicial DrBt.J 0rtier No. ' i s fc r i r* 91-1145 Court 2-49 There are several materials handled in the Tri-Ethane Plant that present safety hazards that require special considerations. While the majority of the materials handled in the plant are toxic or hazardous to various degrees and should each be handled with its due respect, these deserve separate discussion. Phenol As discussed under "Safety Data" section, phenol is extremely toxic when either inhaled, ingested, or contacted with the skin. Whenever it is necessary to handle phenol where bodily contact is possible, extreme care should be taken. A full face shield, coated gloves, and a full sleeve apron should be worn in these cases. This equipment is provided for the operators in the Tri-Ethane area and should be worn when transferring the phenol from drums to the storage tank. Under any other conditions where concentrated phenol is to be handled, this protective equipment must also be worn. When the phenol handling is com plete, the gloves and apron should be washed thoroughly with water to remove any phenol that has been spilled on them. This precaution should be taken in order to avoid brushing the contaminated gloves or apron against skin or clothing after they are removed. Any spills on the slab or equipment should be washed to the sewer with copious quantities of water. All equipment that is used in handling phenol should be thoroughly washed, and any hoses or lines used in phenol service that could be unknowingly contacted during normal operation should be thoroughly flushed and washed. Never leave contaminated equipment or wearing apparel lying around where someone could inadvertantly contact the phenol. Wash everything thoroughly with water. There is a special suit available for use when handling phenol. This suit pro vides a complete seal of the body away from any splashes of phenol. The sleeves of the jackets are constructed such that gloves fit tightly over plastic rings connected to the sleeves and prevent any contaminant from reaching the hands or arms. Whenever handling phenol, this protective suit must be worn along with rubber boots and full face shield. After use, the suit should be thoroughly washed off and stored, VDC While VDC itself has certain toxic properties, the major hazard from this material is its tendency to form peroxides when it is unstabilizgd and contacts air. Two precautions are taken to avoid the peroxide formation in the plant. First, all vessels that contain VDC are padded with nitrogen to exclude the presence of air. In addition to this, all liquid VDC is stabilized with HQMME. The HQMME serves as an oxygen scavenger and prevents the peroxides from forming even when air is present. With this protective system, there should never be any peroxides in the plant; however, this material should be watched for and all precautions taken to avoid its forming. The peroxides are polymerization catalysts and cause VDC to polymerize when they are formed. If they are present, it will be indicated by a white solid in the VDC or the VDC system equipment. This solid is polymerized VDC and contains the SL 010014 2-50 peroxides. If these solids are isolated and dried, they will explode violently from either heat or mechanical shock. Other catalysts, such as light, water, or iron, will cause VDC to polymerize, so the presence of a white solid does not guarantee that peroxides have been formed; however, no chances should be taken if polymer is found. The most readily available peroxide destroyer is water, but the most effective material is caustic or cell liquor, which is also available in the plant. It is advisable to flush any equipment (that has contained VDC) with cell liquor, followed by a water wash, before any maintenance is done on it. This will insure against accumulated peroxides being trapped anywhere in the equipment or piping where they would be a maintenance hazard. It is necessary to handle small quantities of unstabilized VDC for control analyses during the normal operation of the plant. These samples should be handled with extreme care. Take the samples in the containers provided, analyze the material immediately, then dump it in the plant sewer where a good stream of water is flowing. Do not dump it into a stagnant sewer where it might remain for an extended period of time. DOE The same hazard exists with DOE (ethylene glycol dimethyl ether) as with VDC. This material will also form peroxides when in contact with air. This material is received in 5 gallon cans which will be kept sealed until needed. If the first usage does not consume the can contents, dump the unused DOE to the sewer and follow with plenty of water.. Put a water hose in the empty cans and flush them thoroughly with water to avoid leaving a quantity of DOE sitting around in a can. No DOE will ever be allowed to remain exposed to air for any length of time. If this should ever occur accidentally, flush the container with water before moving it. DOX Dox will also form peroxides when in contact with air. The precautions as to keep DOX drums under N2 pad are the same as for DOE. However, a drum of DOX can be resealed after partial use. Care must be taken to ensure that NO air comes into contact with the DOX when disconnecting the drum from the stabilizer suction manifold. After disconnecting, the drum should be thoroughly purged with N2 to preclude any air from entering the drum and then the drum should be quickly capped. NRE Do not use the Karl Fisher analysis procedure for determining moistures of NRE. It is possible that the Karl Fisher reagent may react with the NRE and the reaction products are unknown. Tf a moisture is to be run on NRE, it should be done by another technique. o\oo^ CONFIDENTIAL: 2-51 Activated Carbon Whenever filling a new or freshly reactivated carbon bed, care must be taken in order to prevent heat buildup in the bed. The heat of adsorption of activated carbon and MC is very great and if a carbon bed is filled too rapidly, extremely high temperatures will result. With the high temperatures, decomposition of the MC occurs. In addition, a burn hazard exists if the operator comes in contact with the vessel. When filling the carbon bod, fill as slowly as possible to minimize the heat buildup. Take as much time as needed. TPP Avoid mixing water with TPP as water will react with TPP to form phenol. Also do not come into contact with TPP as it will have some moisture associated with it and as such may have some phenol in it. Wash off TPP immediately if it comes in contact with your skin. See safety precautions on phenol for additional information. POL DOL will also form peroxides when in contact with air. It is normally received as a mixture of DOL and IBL. This mixture should never be contacted by air. MCA MCA will spontaneously ignite when exposed to air. MCA is diluted in VDC in our plant, but great care should be taken to prevent contacting streams contain ing MCA with air. CONFIDENTIAL? Subject to Protective Of 14 th 'i 1 Cl f! j I ' } fc . SL 010016 2-52 EMERGENCY HORNS. There are two distinct emergency horns in the area: the plant or Area "B" evacuation horn and the MC area evacuation siren. The Area "B" evacuation horn is the regular plant horn blown in short blasts. It may be activated from the EDC/MC control room or the guard house. The sounding of this horn will shut down all non-process equipment in Area "B" and will cause all non-essential personnel to leave the area. Area "B" include all the Organics Area--est of Columbia Southern Road and South of Parish Road. The Area "B" evacuation horn should be sounded in case of a major break or if there is some reason to expect a major break. Whenever the evacuation horn is sounded the guard should be notified of the nature of the emergency if at all possible. If it is desired to evacuate the whole plant, the guards will have to be notified and they will sound the plant evacuation. The guards are the only people able to sound the all-clear signal. The MC area evacuation siren is used to evacuate all non-essential personnel from the operating area and to have all arcing devices in the operating area shut down. This siren is controlled by a switch on the wall in the control room. The area siren should be used in case of a spill involving release of flammable vapors. AREA "B" ROAD WARNING LIGHTS. In the event there is a spill that could release flammable vapors across the Area "B" main road, the Area "B" warning lights should be activated. The lights are rotating red beacons located under the N-S piperacks north of the Per-Tri stabilizer building and south of the HC1 compressor building. These warning lights can be activated from every Area "B" control room and are designed to stop all vehicle traffic on the Area "B" main road. As soon as it is determined that flammable vapors could be released across the road the warning lights should be turned on. PARISH ROAD TRAFFIC GATES. There are two gates located at the East and West extremities of the Organics area on Parish Road. These are to be lowered when it is felt that there is a possibility that flammable vapors could be released across Parish Road and present a hazard to vehicles utilizing the road. The control switch for the gates is located in the EC-VC-HC1 Control Building. SL 010017 CONFibF^^;e or6er Sub3eC t to juaicidJ o lAtb No. ' Court 2-53 FIRE PROTECTION CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 The MC Plant is protected from fire by a water deluge system. It can be tripped several different ways: 1. Manual trip on the control board or at the sprinkler house west of the catalyst building; 2. Activation of one of the HAD's (head activated devices) located in the unit; 3. Release of flammable vapors near one of the flammable vapor detectors which are located in the area. The stabilizer storage and NRE storage north of the process area as well as the NRE storage northeast of the MC dock tanks are also protected by a water de luge system. Each of the systems can be tripped manually or by activation of one of the HAD's. A sudden rise in the HAD supervisory air pressure will cause the deluge valve to open and cover the area with a water spray. Do not be afraid to manually trip in any of the areas in case of a fire or spill in that area. Whenever any deluge valve is tripped, an alarm will sound in the guard house, but the fire truck will not come unless the guards are notified or they can see the fire or smoke- Anytime a deluge valve is tripped, the valve must be reset before automatic protection is available again. The valve is reset by closing one water valve upstream of the deluge valve, removing the cover of the deluge valve and resetting the weight. The HAD's are the heat sensing elements and are located at all strategic points in the process. The HAD's are empty shells connected to the release diaphragm of the Suprotex deluge valve by a manifold of 1/8" FVC coated copper tubing. The HAD's and the tubing manifold are pressurized with 24 oz. air pressure. An abnormal temperature rise in one of the HAD's, as would occur in the event of a fire, will create a pressure rise in the units and the tubing manifold. This pressure rise will cause a diaphragm operated release mechanism to release a suspended weight. This weight drops and disengages the latch holding the deluge valve closed, thereby starting the flow of water to the distribution system. The water is dispersed in the area by sprinkler heads, which are lo cated so as to provide a spray over all exchangers, surge tanks, pumps, and skirts of columns. The manual trip lever is the handle located on the Suprotex deluge valve. When pulled, this handle releases the weight. A change in environment temperature will not trip the system because the Suprotex valve has a compensating vent valve in the diaphragm. This valve is sized so that a slow pressure buildup in the supervisory air (HAD system) system will bleed through the valve to the other side of the diaphragm thereby equalizing the pressure. As may be seen from the description of the supervisory air system, an accidental break in the HAD's or tubing manifold will not trip the deluge valve. Anytime the system has a break in it, all automatic fire protection for this system is lost. Anytime the supervisory air pressure gets below 16 oz. an alarm will sound. Check the alarm out immediately as you are in danger of losing your protection. The alarm will sopnd if any single circuit of the supervisory air system develops a leak. When the alarm sounds, check the supply pressure and the overall supervisory air pressure. If both of these are normal then a SL 010018 2-54 particular circuit has a leak, but enough air is being bled into the system to maintain the required 24 oz. pressure. Automatic Sprinkler will have to be called to find and repair the leaking circuit. To silence the alarm, the electrical power to the valve house will have to be shut off, the horn dis connected and power put back to the valve house. This power will come from the emergency circuit. Fire protection exists until the supervisory air is about 6 oz. The sprinkler system in the Tri-Ethane and VDCM process area consists of two main water headers. Each header has a Suprotex Deluge Valve. Activation of one of the valves will cause subsequent activation of the other valve. This is accomplished by a tie in on the water pressure impulse line downstream of the valves. This is the impulse line which activates the alarm bell when the system trips. When pressure rises in the impulse line, a switch trips the other deluge valve. 2-55 FIRE EXTINGUISHERS There are 15 fire extinguishers in the MC Plant area, most of them being the dry chemical type. The dry chemical is most effective for organics fires while the CO2 extinguishers are good for small fires or small electrical fires. Anytime you are in doubt as to the type of extinguisher to use, use the dry chemical. It is good to avoid the use of the dry chemical on small electrical fires, as the chemical leaves a harmful residue. SAFETY INSPECTIONS Once per week an inspection of all safety equipment in the MC plant shall be made. This includes fire extinguishers, fire protection system, protective masks, safety showers, etc. A form has been provided for use as a check-off list. This has a two-fold purpose: 1. To ascertain that required equipment is in good operating condition; and 2. to familiarize Operations personnel with the location of safety equipment for quick use in an emergency. VAPOR DETECTOR SYSTEM The vapor detector system consists of detectors located around the process area. These detectors monitor the area continuously for flammable vapors and send a signal to an indicating board in the control room. The vapor detectors are located at: 1. VDC vaporizer recirculation pump 2. VDC DH still phase separator 3. VDC still reflux pump 4. VDC reactor bottom 5. VDC DH still product pump 6. VDC vaporizer feed pump 7. Southwest corner VDCM day tank dike 8. Northwest corner VDCM storage day tank dike 9. VDC storage tank dike 10. VDCM Reactor heatup pump 11. South end stabilizer storage dike 12. North end stabilizer storage dike 13. North end DOL/IBL storage dike 14. Southwest corner DOL/IBL storage dike 15. Sewer southwest of control room Vapor Detectors located at positions 1 through 10 will trip the process area sprinkler systems. Detectors located at positions 11 through 14 will trip the sprinkler system at the stabilizer storage area. Number 15 does not activate a sprinkler system. SL 010020 2-56 There is an amber warning light and bell which are energized at 20% of the lower explosive limit (L.E.L.) of ethyl chloride. At 40% L.E.L., a red light on the panel board is energized and the sprinkler system is tripped. The cabinet bell also rings in the event of filament failure at any of the remote detector points. The alarm, or warning, conditions are maintained until manually reset. Upon receiving a warning light and bell on the vapor detector board, the operator should ascertain where the problem is and correct it as soon as possible. In the event that the problem is in the detection system, it can be bypassed by a switch located on the control board. The "OFF" position on the switch prevents the sprinkler system from tripping when the 40% L.E.L. is reached. Unless there are problems with the detector system or a controlled spill is occurring (e.g. sampling VDC near a detector head), the bypass switch should be kept in the "ON" position. To insure proper operation for each detector unit, the following schedule should be followed: Weekly: Check zero reading on the 0-1.0 L.E.L. meter for each detector. This is done as follows: a. Check for presence of combustible gas at detector head with a portable combustible gas indicator to insure none is present. b. Turn zero adjuster to bring reading to "0". Monthly: Check operation of alarm signals and settings for each detector: a. Block off the water to the sprinkler system being tested. b. Insure that indicator is zeroed. c. Squirt a sample from an ethyl chloride bomb on the ground near the detector head being tested,. A second party should be watch ing the indicator for positive movement and that the alarms come on at the desired level. Feel or listen to the Solenoid valve behind the control board to be sure it is activated. This Solenoid trips the sprinkler system. d. Reset the deluge valves and unblock the water to the sprinkler system. Subie-0';: to of l4th * No- j 1V** order c'- SL 010021 EQUIPMENT IN THE MC AREA CONFIDENTIAL: 2-57 Subject to Protecfcive Order of 14th Judicial District Court No. 91-1145 Electrical Equipment The characteristics of some of the materials handled in the Tri-Ethane Plant are such that the plant is classified as a Group D, Class I installation by the National Electrical Code. The method and materials of installation are those recommended by Factory Insurance Association. In general, the in stallation is Class I, Group D, Division 2. Motors are TEFC (Totally Enclosed Fan pooled), lighting is vapor-tight, and all arcing devices are explosion-proof with seal-offs. Relamping and Receptacles Vapor-tight fixtures are used in the process area. The relamping procedure will be to first determine the lamps which need changing by turning on all lights. Then, turn off all lights and relamp. To simplify this procedure, circuit breakers for lights in the process area and control laboratory have been grouped in the lighting panels. Globes and guards must be replaced after relamping. Grounding Grounding in the Tri-Ethane Plant has been given special attention due to problems peculiar to the handling of hydrocarbons. Grounds for motors and other electrical devices are contained in the conduit supplying the device and connected to the device frame internally. Motor change-outs should be checked to see that the ground has been replaced. Due to the tendency for hydrocarbons to build up a static electricity charge as a result of movement or agitation, a system of jumpers for pipe flanges has been installed to provide metallic continuity of the piping system containing flammable materials. All vessels are grounded at two points. The result is a system of lines, tanks, and vessels operating at ground potential. This will not prevent the generation of static charges but should provide adequate leakage to ground to prevent the accumulation of dangerous charges. It is obviously important that the grounding system be maintained intact. This should be kept in mind when performing maintenance work on any equip ment in the Tri-Ethane area. Pumps and Equipment Any pump or piece of equipment that is removed from the Tri-Ethane process must be thoroughly cleaned and inspected at a provided location before it is permitted to leave the area for the main shop or other work areas. SL 010022 CONFIDENTIAL: Protective Order Subject to District Court of 14th Judicial Clearing of Tanks and Process Vessels Mo 2-58 The area supervisor and maintenance supervisor will see that all vessels or tanks are cleaned and checked with an explosion meter before declaring them suitable for maintenance. Clearing Procedure: a. The tank or vessel will be emptied and all valves will be closed and tagged. b. The vapor contents of the tank will be purged with an inert gas. c. Blinds will be inserted in all connecting lines. d. The equipment will be steam purged where possible to vaporize and remove all flammable materials. If steam cannot be utilized, an inert gas will be used. e. Purge the equipment with plenty of air. f. The equipment will then be checked with an explosion meter before work is begun. If entry into the vessel is required, the vessel must be also checked with an oxygen meter. g- Safety belts and safety lines will be required in top exit tanks. Safety Equipment 1. Stretchers....................1 a. One located inside the control room. .2 Full Face Masks....7 (all purpose cannister) a. Four in the control room. b. One by the HCl separator. c. Two at main entrance to Area B. d. Two at air compressor building. 3. Scott Air-Pnks...,.2 a. Two in the control room. 4. Emergency Lights...3 in the control room emergency light storage a. Two flashlights b. One hand lantern SL 010023 GAS MASKS CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 2-59 The standard chlorine escape mask will be carried in the Tri-Ethane area and is effective for emergency protection for most of the materials that will be encountered. However, there are three materials that personnel could be exposed to in this area for which these masks are not adequate. Methane and ethylene are not filtered out by these masks, so the masks offer no protection in the case of a major leak involving either of these two gases. Since neither of these two gases are toxic, the area exposed to these two materials can be evacuated before sufficient concentration is reached to suffocate any personnel. If it is necessary to enter an area where quantities of these gases are accumu lated, a self-contained breathing device, such as a Scott Air-Pak, must be worn. NRE also presents a special hazard for vapor protection. The heat of absorption of NRE on the activated charcoal contained in the cannister type escape mask is so high that the heat generated in the mask would be sufficient to ignite the NRE. Consequently, this type of mask should never be worn in an area where NRE vapors will be contacted. A self-contained breathing device must be used if it is necessary to enter an area containing quantities of NRE vapors. CONTROL BUILDING The control building is pressurized to prevent accumulation of any vapors inside. Since it is a pressurized building, non-explosion proof electrical equipment is used and smoking is permitted inside. The positive pressure is maintained by a fan which draws its intake air across an activated carbon filter. Should a major break occur, the filter would be unable to eliminate all contaminants, therefore, the fan should be shut down. To prevent any vapors from entering the building when the fan is off, instrument air bleeds should be opened. (Do not bleed the air system down by taking too much.) To prevent dust from accumulating in the control room, filter bags are in the suction of the air conditioner. For any problems with the air conditioner, notify the supervisor. LAB AND LAB HOOD FAN The laboratory has several nitrogen outlets. If this nitrogen were opened up and allowed to purge into the room, any person in the lab could be asphyxiated. Protection against this is given by the lab hood fan. This special hood has two fans, one discharging into the hood and one pulling out of the hood to the outside. The fan pulling out has a larger capacity, thus there is a net flow of air out of the lab, preventing concentration of fumes or nitrogen. St e,.. uC0KPIde^TIAL: Subject to Prot,of 14th`j'ud7ci;rn^V- *>' rdGr Cour-1 GENERAL PROCESS DESCRIPTION The Tri-Ethane and vinylidene chloride monomer (VDCM) plants are a closely related complex of four processing units and a stabilizing section. The general chemical reactions are (see compound abbreviations EDC + ci2 --------- - TCE + HCl + Heavies TCE + NaOH ---------- ^ VDC + Impurities VDC + HCl----- ----- MC MC + Stabilizers: Tri-Ethane VDC + Impurity (DCA) + Reactant (morpholine) ------* VDCM + Adduct TCE Section: The chlorination of EDC to product TCE, HCl and heavy chlorinated organics is carried out in a liquid phase TCE Reactor. A free radical initiator > AIBN, is added to aid in complete chlorination. The heat from the exothermic reaction is removed by a vertical condenser through which the HCl gas passes and by a thermosyphon cooler mounted on the side of the reactor. The TCE and heavies are drawn off the reactor as a liquid mixture. The liquid mixture is purified to give a high purity TCE product in the Lights Still and Heavies .Still. The function of the Lights Still is to separate un reacted EDC (a light component in comparison to TCE), in the liquid taken from the TCE Reactor, from the TCE and Heavies. This unreacted EDC is recycled back to the TCE Reactor. TCE and Heavies are the bottoms off the Lights Still and are fed to the Heavies Still where the TCE is separated from the heavy chlorinated organics. The product TCE (99+% TCE) is then pumped to TCE storage. The bottoms from the Heavies Still, containing the heavies and a small percentage of TCE,are trans I'erred to the Bottoms Plant for further processing. SL 010025 3-2 The HC1,after being partially cooled in the vertical TCE reactor condenser, still contains EDC and TCE as major impurities. This HCl gas is countercurrently contacted in the EDC absorber with a TCE rich stream to absorb most of the EDC. The HCl gas from the EDC absorber is then chilled to less than 50F to condense out all but trace quantities of TCE and EDC. This HCl can then go to the MC Section (where it reacts with VDC to form MC) or to the Area B HCl distribution system. VDC Section: TCE is dehydrochlorinated in the VDC Reactor by reacting with sodium hydroxide to form vinylidene chloride. The source of NaOH is cell liquor or press wash (a side stream in Caustic Department) or a mixture of the two. The VDC Reactor is a column containing 39 contacting trays. Cell liquor and TCE are mixed and then fed to the reactor. Steam is injected into the bottom of the reactor to boil up organics, while cooled steam condensate and VDC are fed at the top of the reactor to prohibit boiling unreacted TCE over head. The bottoms stream from the reactor contains water, NaCl and unreacted NaOH. The overhead reactor stream,consisting of VDC, H2O and impurities formed in the reactor, is fed as a vapor to the VDC still. The contents of the VDC Reactor and all other equipment in the VDC System are inhibited against peroxide formation by an oxygen scavenger (HQMME), The function of the VDC still is to remove the heavier impurities, primarily isomers of VDC, from the VDC. The VDC Still also uses live steam injection at the bottom as the heat source. The bottoms stream from the VDC still, containing the heavies dissolved in water, is pumped to the Per-Tri acid pit for recovery of the organics. CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 3-3 The wet VDC taken overhead from the VDC still is dried in the VDC Drying Still. The Drying Still utilizes the formation of an azeotrope between VDC and H2O to dry the VDC. The still is a packed column and has two forced circulation reboilers tp provide heat input. Water is taken overhead and con densed, then periodically drained to the sewer. The dried VDC from the bottom of the Drying Still is transferred to crude VDC storage. This VDC is sufficiently pure to be used to make methyl chloroform, but contains one impurity (DCA) which prohibits its use by polymer producers. MC Section: Methyl chloroform is formed by the reaction of VDC and HCl in a liquid phase MC Reactor. This reaction is carried out in the presence of ferric chloride catalyst, dissolved or suspended in the reactor liquor. The heat from the exothermic reaction is removed in two large forced circulation coolers. Tars formed in the MC Reactor and FeCl^ are removed from the liquid stream from the reactor in a Flasher and Dopp Kettle system. These kettles are steam jacketed, scraped walled vessels which make handling of the tars possible. The Flasher boils MC and unreacted VDC overhead where it is condensed as a clean liquid. The FeCl3 and tars flow from the bottom of the Flasher to the Dopp Kettle where they are further concentrated before dumping. The VDC in the clean MC-VDC liquid is removed in the MC Stripper to leave a VDC free MC. Methyl chloroform is heat sensitive and will revert back to VDC and HCl when heated unless properly heat stabilized. A heat stabilizer, TPP (triphenyl phosphite), is added to the MC Stripper to prohibit MC decomposi tion. This heat stabilizer is removed from the final MC product by a Topping Still which separates the MC overhead and leaves the heat stabilizer in the bottoms. The Topping Still Bottoms are pumped back to the Flasher where the TPP prevents MC decomposition in the Flasher and Dopp Kettle. SL 010027 3-4 The Topping Still product contains trace amounts of HCl which drops the pH below specified levels. The trace acidity is neutralized by reaction with a sodium carbonate-water mixture in a mixing and phase separating system. Mixing is accomplished in a pump, while further contacting takes place and the water phase is separated from the more dense MC in the neutralizer vessel. The neutralized MC is dried in dessicant driers before being transferred to the storage and stabilization area. Tri-Ethane Stabilization: Tri-Ethane is used in several solvent appli cations. Most of these applications can successfully use the standard grade of Tri-Ethane Type 324. This blend contains varying amounts of seven stabilizers. These stabilizers are added to the MC in Stabilizing Tanks and subsequently stored in Day and Shipping Tanks. Other applications require specially stabilized blends. Several of these specialties are produced and a small section of the tankage and equipment is allocated to this service. The major uses of Tri-Ethane include many industrial solvent and degreasing activities. Some of the uses of specialty grades are for Liquid Drano and as a carrier for latex. An important possible future use of TriEthane is in textile processing. Vinylidene Chloride Monomer Section: One of the impurities in the crude VDC material has been found to cause color formation in the VDC in storage. Polymer producers are unable to use this VDC due to the color formation. This impurity (DCA) is removed from the crude VDC by reaction with morpholine. This reaction is carried out batchwise in the VDCM Reactor. The crude VDC material is treated with the morpholine at 130F for 4 hours. The DCA-Morpholine reaction product and unreacted morpholine are removed from the VDC in the VDCM Sf'"'l. The monomer grade VDC is boiled overhead, condensed, dried and stabilized SL 010028 COLSFXDEllTlM*: Subject to of uth ^ Court 3-5 with HQMME on the way to storage. Some facilities are also available for stabilization with phenol. The reaction product and unreacted morpholine are purged from the system off the bottom of the VDCM Still and go back to the crude VDC reactor. If the levels of the DCA in the crude VDC remain below 100 ppm, the morpholine treatment step can be eliminated. The VDCM still is then used as a VDC purification still, removing Toluene, and cis-and transdichloroethylene. The VDCM reactor is then bypassed. VDCM has several uses, the most common being Saran which is a copolymer of VDCM and vinyl chloride. It is also used in the production of specialty fibers for clothing and carpets and as a barrier coating in packaging. CONFIDENTIALs subject to nf 14th Judicial District ot x ui-1145 SL 010029 Detailed Process and Equipment Description 4-1 TCE Section Chemical Reactions: The chlorination of EDC to TCE and heavier chlorinated organics are described by the following reactions. HI HI AIBN H-C-C-H + Cl2 Cl Cl Cl - 6 - A - H + HCl 6i cl EDC HH Cl - C - 6 - H + Cl2 Cl Cl 1,1,2 Trichloroethane (TCE) HH Cl - C - C - Cl + HCl Cl Cl TCE Sym. TeCE or Cl H Cl - d - C - Cl + HCl Cl H Unsym. TeCE HH Cl - C - Q - Cl + ci2 Cl Cl H Cl Cl - C - C - Cl + HCl Cl Cl TeCE PCE These reactions are carried out in the TCE reactor at conditions such that 16 to 40% of the reactor liquor is TCE. A free radical initiator - 2,2 azobisisobutyronitrile (AIBN) - is added to the reactor to aid in the chlorina tion reaction. The presence of iron in the TCE reactor will inhibit the com plete utilization of the chlorine and cause subsequent chlorine breakthrough into the HC1 and Lights Still systems. An examination of the chemical reactions reveals that a mole of HC1 is formed for each mole of TCE formed. Also, one mole of VDC is formed per mole SL 010030 CONFIDENTIAL: Subject of 14th Ju CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 4-2 of TCE reacted and one mole of HC1 is reacted with one mole of VDC to form MC. Thus any HC1 formed in addition to the HC1 formed by TCE formation represents an excess of HCl--not usable in the MC plant. Further observation reveals that for each mole of chlorine consumed in the chlorination to TCE and heavies, one mole of HC1 is produced. The formation of heavies in the TCE reactor is a direct function of the TCE concentration; that is, the greater the TCE concentration, the greater the formation of heavies. Although these heavies are not usable in the MC Plant, they do not represent a loss to the Company because they are good feedstock for the Per-Tri plant. EDC Feed System: A. Equipment 1. EDC Feed pumps (formerly used as EDC feed pumps to Per-Tri plant)SAC Nos. 55-796, 797. These pumps are Goulds Model 3196, size 1x28 and are constructed of ductile iron. The pump has a 8" semi-open impeller. The pumps are powered by 3500 rpm, 10 h.p. motors (SAC Nos. 50-3431, 3450). The pump uses a 1 3/4" John Crane Type 9 mechanical seal. 2. EDC Feed Drier (SAC 73-104). This vessel is all steel construc tion, 42" I.D. x 20`8" seam to seam. The design vessel pressure is 300 psig to full vacuum at 300F. The 9000 pound charge of flake calcium chloride is supported by a three piece steel grating with a 41 3/4" O.D. carbon steel wire cloth, 18 Gr. x 6 mesh. The drier has a fiberglass roll at the top which is supported by 1/2" rods and held down by a basket with an expanded metal grid. The drier is protected from overpressure by a 1 x 1 1/2" SRV set to relieve at 150 psig. 3. EDC Feed Filter (SAC 72-154). This is a cast iron/steel Commercial Ful-Flo filter Model WYFDS-10-2. The filter uses twelve 10 inch 25 micron fiberglass filter elements. Overpressure protection is provided by a 1 x 1 1/2" SRV, set to relieve at 150 psig. B. Operation The EDC for the TCE Reactor comes from storage tanks in No. 1 EDC Plant. This EDC must be dry and free of iron. Each tank is checked for moisture and iron content before pumping to the TCE Reactor. The drier serves as backup to to insure that only low moisture EDC is fed to the reactor. SL 010031 CONFIDENTIAL: Subject to Protective Oi:c3er of 14th Judicial District Court No. 91-1145 ., 4-J Metering of the EDC feed is critical for the carbon-chlorine balance and efficiency calculations in both TCE and EDC plants. This flow can be measured by tank difference, by a positive displacement Barton meter and by an orifice type flow meter. Chlorine Feed System: A. Equipment 1. Chlorine Vaporizer (SAC 70-66). This exchanger is an Armstrong Size "I" vaporizer. It has a 300 psig shell design pressure at 400F and 100 psig tubeside design pressure at 400F. The vaporizer originally has 200 one inch carbon steel tubes 4'6" long. Each tube has a 1/2" copper bayonet tube inside which extends up about 4'. Some of the tubes at the chlorine inlet were removed and replaced with a steel baffle plate to prevent impingement of the liquid feed on the tubes. The vaporizer is protected from overpressure by a 4" chlorine barge-type SRV, set to relieve at 300 psig. 2. Spare Chlorine Vaporizer (71-1315). This vaporizer is identical to the one described above with the exception that the baffle was replaced with a distribution belt. The belt extends around the vaporizer at the bottom and gives a large area to feed the liquid into, thus cutting velocity. 3. Chlorine Surge Drum (SAC 60-1014). This steel vessel is 4'6" O.D. by 12" tangent to tangent. It is rated at full vacuum to 300 psig at 300F design temperature. The drum is protected from overpressure by a 2" x 3" SRV set to relieve at 150 psig. This SRV is protected from chlorine attack by a 2" 150 psig TeflonMonel-Teflon rupture disc. 4. There are several safeguard systems built into the Cl feed system. These safeguard systems will be checked periodically for proper operation. a. One safeguard is an automatic shutdown system that closes the CI2 PCV to the surge drum and the CI2 FCV to the TCE reactor. This system is activated when the CI2 temperature into the CI2 surge drum ojc the CI2 surge drum bottom temperature drops below 110F. The control valves cannot be put back into service until the CI2 temperature at both these points is above 110F and a reset button is pushed behind the control board. Both these points have low temperature alarms set at 130F; both points are recorded on TRI (points TRI-1 and TRI-9). SL 010032 Subject *t.on protec ti.v-ej Order t Court judicial Distnc Of 14th NO. 91-U45 4-3a b. In order to keep TCE reactor liquor from backing up through the CI2 system to the Cl2 surge drum, there is an automatic shutoff valve located in the CI2 piping right at the entrance to the TCE reactor sparger ring. This valve is designed to shut off when the pressure difference between the TCE reactor and the CI2 surge drum drops below 3 psi. The impulses for the DP cell are taken from a tap on the sparger ring and a tap upstream of the orifice run. There is also a manual trip switch located by the CI2 FCV to enable the operator to close the valve. There are two positions on this trip switch--"auto" is the normal position which allows the valve to remain open; "manual" bleeds off the N2 impulse to the anti-backup valve and closes the valve. A second field mounted switch allows the anti-backup valve to be opened for startup. "Automatic" is the normal position for this switch. This position allows the shutdown system to operate. "Manual" bypasses the system and opens the anti-backup valve. This switch has been covered with a cover plate to prevent inadvertent operation. c. There is a nitrogen pad system set up to pressurize the CI2 piping between the CI2 FCV to the TCE reactor and the anti backup valve. This system contains 4 nitrogen bottles piped up to a common manifold which ties into the CI2 piping at the CI2 FCV. It is separated under normal operating conditions by a double block and bleed valving arrangement. The regu lators on the bottles are set to maintain 125 psig pressure on the CI2 piping when it is put in service. Three bottles are floating on the line with one bottle in the rack blocked off as a reserve. A safety relief valve set at 150 psig protects the N2 piping from rupturing in the event of a regulator failure. d. CI2 vaporizer outlet temperature is also monitored and alarmed. It is recorded on the Cl2 FRC as a second pen. Its low and high temperature alarms are set at 150F and 170F respectively. & Steam flow, temperature, and pressure are recorded with the steam flow having a low flow alarm. Note: Replacement SRV's for the CI2 Vaporizer are in the Storeroom. If the existing SRV needs to be changed, get rebuilt SRV from the Storeroom and return the used SRV to the Storeroom. This SRV will be rebuilt and put back in the Storeroom. B. Operation Liquid chlorine can be fed directly to the chlorine vaporizer in the TCE Section, or can be preheated in the chlorine vaporizer in the EDC plant. The preheating is accomplished by taking a liquid draw-off the EDC chlorine 4-4 vaporizer. This liquid draw-off will be free of oxygen, which can inhibit the TCE reaction if present in significant quantities. Preheating of the chlorine was used before the advent of AIBN. AIBN has proven capable of overriding the effects of oxygen in the chlorine when it is fed directly to the vaporizer in the TCE Section. Thus, preheating is not normally used now. i A brief sketch of the vaporizer is shown in Figure 1. SRV Figure 1* Sketch f CI2 Vaporizer Internals, showing two tubes. Of^r? CONFPJDr EEN'Vl j\ j th JiuHcip ot r X D I. Wo. Sj. - 4i. .4J. l S *- 45 *rn Order r^ct r> ourt 4-5 Liquid chlorine enters the bottom of the shell side of the vaporizer and is vaporized by steam condensing in the vertical tubes. The vaporized chlorine goes out near the top and goes to the pressure control system. The steam enters the chest at the bottom of the vaporizer. Any condensate entrained in the feed steam (for example--when using saturated steam) drops out in the chest and is removed via a small steam trap at the bottom. Steam flows from the chest up through the bayonet tubes into the main tube, where it is condensed on the tube surface and falls.down to the condensate chamber. This condensate is removed through parallel steam traps. The chlorine vaporizer operates under a variable heat transfer area principle. The vaporizer runs with a level of liquid chlorine in the shell side. The chlorine chest pressure is near the liquid line pressure, since pressure control valves are on the outlet vaporized chlorine. Steam chest pressure is maintained by a pressure control valve on the incoming steam. As chlorine throughput increases, more area is needed to transfer the additional heat; so, the liquid level builds up until enough additional tube area is covered to boil off the additional chlorine. Conversely, if chlorine through put drops, the chlorine level drops to decrease the chlorine boilup. The flow of the vaporized chlorine is split between the HC1 plant and the CI2 surge drum. Chlorine to HC1 goes through a pressure control valve (PCV) and then to a surge drum in the HC1 Plant. All the controls for this PCV are in HCl. Chlorine to the TCE Reactor passes through a PCV which reduces the vaporized chlorine pressure to 75 psig. This flow then goes to the chlorine Surge Drum and then off the top of the Surge drum to a flow control valve leading to the TCE Reactor. A small stream is taken off the top of the Surge Drum and goes to the vinyl chloride plant for chlorination of chloroprene in their recycle SL 010035 EDC Stream. CONFIDENTIAL: Subject to Protective Order of 14th Judicial bistrict Court No. 91-1145 ., The Surge Drum is equipped with a safety relief valve which opens if the pressure exceeds 150 psig. There is a TMT rupture disc under the SRV set at 150 psig. The temperature of the vaporized chlorine must be controlled so that no liquid is formed in the Surge Drum or downstream piping. Any liquid chlorine fed to the TCE Reactor could lead to greater than normal reaction rate, possibly so great that the normal cooling equipment would be inadequate to handle the increased heat removal load. This can lead to overpressuring of the reactor with subsequent blowing of the rupture disc. Large amounts of liquid chlorine feed could possibly lead to rupture of the reactor vessel. Liquid chlorine begins to condense at 63F when under 75 psig pressure. The temperature of the chlorine in the Surge Drum is controlled above 130F. This is done by adjusting the steam chest pressure controller. The steam chest pressure determines the condensing steam temperature, and the degree of super heat given to the vaporized chlorine by the tubes above the liquid chlorine level is determined by the temperature driving force between the steam and the chlorine. Thus, an increase of steam pressure results in more superheat. Ethylene System: Ethylene is used in the TCE Reactor only during startup. This ethylene comes off a 175 psig feed line in the EDC plant. It passes through an orifice meter in the TCE Section and is flow controlled to the TCE Reactor as needed. After the TCE Reactor has been started up and ethylene is no longer needed, the C2H4 FCV and bypass will be blocked, tagged, and sealed by the Lead r Operator. TCE Reactor System: 010036 A. Equipment 1. TCE Reactor (SAC 59-19). The reactor is 8'5" I.D. by 32*9" seam to seam. The vessel is constructed with 20% nickel clad steel. Design pressure is full vacuum to 75 psig at design temperature CONFIDENTIAL: Subject to Protective of 14Hi Judicial Hi. a trie No. 91-1145^' Order t Court 4-7 of 400F. The two chlorine spargers are located near the bottom. A short (1 foot) packed section is located about four feet above the chlorine spargers. This packed section covers the full cross section of the reactor. The packing is supported by a Stoneware nickel "Multi-Beam" support plate, and is held down by a nickel grid-type holddown plate. The packing is 1 1/2" nickel pall rings. The reactor is protected from overpressuring by an 8" 75 psig graphite rupture disc. 2. TCE Reactor Condenser (SAC 71-1197). This shell and tube exchanger is mounted vertically on top of the TCE reactor. It has 588 one-inch nickel 16 BWG tubes, 10' long. The tubeside has a design pressure of 75 psig with 300F design temperature, while the steel shell has 75 psig design pressure with 150F design temperature. Both tubesheets are nickel. The total heat transfer area is 1541 sq. ft. 3. TCE Reactor "Sidearm" Cooler (SAC 71-1217). This cooler is mounted on the side of the TCE reactor. It has 330 one-inch 16 BWG nickel tubes, 12' long. The tubeside has a design pres sure of 100 psig with 300F design temperature. The steel shell has 75 psig design pressure with 150F design tempera ture. Both tubesheets are nickel. The total heat transfer area is 1037 sq. ft. 4. TCE Reactor Circulating Pump (SAC-55-1553). This is an Ingersoll Rand Model 8 APL single stage elbow type, circulating pump. It is an axial flow pump with top suction and end discharge. The pump has a Monel case and impeller. It uses a John Crane Type 9 Code QP mechanical seal. It is powered by a 1750 rpm, 10 HP motor. 5. AIBN Storage Refrigeration. This is a Kolpack Industries Inc. insulated refrigerator (11' x 7'). It is cooled by a 4500 BTU refrigeration unit powered by an Americold Compressor Inc. refrigeration compressor. The unit uses Freon-12 as a refriger ant. The refrigerator is equipped with a liftable lid to relieve any pressure that could possibly develop in the event that the AIBN decomposed. The cold box is also equipped with an oxygen analyzer and temperature indication. B. Operation Chlorine is fed through the two spargers at the bottom of the reactor EDC (and ethylene, as required) also enters through a sparger at the bottom. The chlorine feed line forms a loop the height of the reactor, which prevents back-up of reactor liquid into the chlorine system on shutdown. As the reaction to TCE and heavies is carried out, heat is evolved. The heat of SL 010037 CONFIDENTIAL: Subject to Pr-otootivo Order of 14th Judirie. !. District Court No. 91-1145 4"8 reaction is removed by two means; the overhead partial condenser and the 1 sidearm cooler. The overhead partial condenser is mounted vertically on top of the reactor such that the HC1 formed in the reactor passes up through the tubes and is cooled by cooling tower water (CTW) on the shell side. Condensed EDC and TCE fall back down into the TCE reactor. The water piping is arranged so that CTW enters the condenser at the top, flows down and out through a loop which goes back up to the top of the condenser. A small drain line (1/2") takes a water purge to the sewer from the top of the condenser. This is to ensure that the full length of the tubes stays wetted to prevent corrosion from occurring due to the tubes being wet part of the time and then dry due to air pockets. The TCE reactor "sidearm" cooler is a thermosyphon type cooler mounted on the side of the TCE reactor. TCE reactor liquor circulates through the tube side of the cooler, while CTW is on the shell side. The reactor liquor circulation is created by the thermosyphon effect--this is, as cooling occurs in the tubes of the cooler the liquor becomes more dense and flows down. The cooled, dense liquid that flows down is replaced by the hot, less dense reactor liquid in the top of the tubes. Thus the flow is opposite to the normal flow encountered in a thermosyphon reboiler. A pump was originally supplied to provide circulation, but the success of the thermosyphon effect has so far eliminated the need for the pump. The TCE reactor temperature control is somewhat dependent upon pro duction rate. At rates up to about 150-170 TPD, the overhead partial con denser has adequately cooled the off-gas, without the sidearm cooler being in service. The TCE reactor temperature will be about 245 to 255F when SL 010038 Of Subject to Protective 14th `Judicial Dist rice rde r Court No. 91-1145 4-9 in this production rate range. At higher rates, however, the reactor temperature continues to go up, thus increasing the condensing and cooling load on the overhead condenser. The HC1 off-gas temperature from the reactor condenser increases above about 160F and overleads the downstream absorption and refrigeration equipment. The sidearm cooler is then put in service to lower the reactor temperature as required. The design reactor temperature at peak rate (245 TPD) is 212F. The reactor temperature is controlled with the sidearm cooler by throttling the bottom organic valve (top valve being fully open). CTW flow is set at such a rate that the outlet water temperature is below 130F. Thus, if more cooling is required, the bottom organic valve is opened more to allow more circulation and, hence, cooling. An automatic controller is provided to control reactor temperature by water flow, but is not used because of possibility of getting outlet water temperature above the point where plating out of silica and calcium may occur. Another important aspect of TCE reactor temperature is the concen tration and life of A1BN in the reactor. AIBN decomposes to a non-useful form very quickly at the TCE reactor temperature. Thus, the cooler the reactor temperature, the longer the life of AIBN and the lower the require ments for make-up AIBN. The half life of the AIBN increases ten fold by dropping the reactor temperature from 250F (half life is 0.6 minutes) to 212F (half life is 5.5 minutes). The TCE reactor level is controlled at 25'-26' by the make-up of EDC. The normal liquid take-off is located at 24', with another take-off located 2 feet below this. The reactor pressure is maintained at slightly above 45 psig by a pressure controller in the downstream HC1 system. SL 010039 CON FI \ r i,j . * of Subject to p totot. cive Order Uth Judici aJ- district No. 91-1145 Court 4-10 Reactor concentration is a function of production rate and/or requirement for heavy chlorinated organics, as well as the HCl require ments for Area B. If area requirements for heavies and HCl are high, the TCE strength is increased so as to make more of these two co-products. As mentioned previously, iron in the TCE reactor is detrimental to the reaction. Any water present can lead to corrosion in the associated equipment and result in iron in the reactor. The iron content normally runs less than 1 ppm, and water content ranges from 50-80 ppm (when run by GC method of moisture analysis). HCl Purification and Distribution: A. Equipment 1. EDC Absorber (SAC 67-73). The absorber is a steel vessel 24' O.D. by 21'10" seam to top flange. It is designed for 75 psig and full vacuum at 300F. The absorber is packed with one fifteen foot packed section (containing approxi mately 50 cu. ft.) of 1 1/2" chemical porcelain Intolox sad dles. The packing is supported by a three piece chemical porcelain U. S. Stoneware "Multi-Beam" type support plate. The liquid feed is sparged into the absorber at the top through a 1 1/2" pipe with one large hole in the bottom at the end. This feed is distributed over the packing by a Stoneware 'Weir-Riser" chemical porcelain distributor tray. The packing is held down by a carbon steel grid-type plate. The absorber is protected by a 3" Teflon-Monel-Teflon rup ture disc with 75 psig bursting pressure. 2. TCE Reactor Vent Condenser (SAC 71-1198). The vent condenser is a U-tube exchanger with a special shell design. The ex changer, has 266 - 3/4" steel 12 BWG U-tubes with 8'6" nominal bundle length. The tubeside design pressure is 150 psig with -10 to 200F design temperature. The shell has a design pressure of 120 psig over -30F to -20F range, and 300 psig over -20F to 200F. The inlet head is designed to give four tubeside passes. The shell consists of a horizontal 26" O.D. steel cylinder topped by 20" O.D. horizontal steel cylinder which serves as a vapor-liquid separation chamber. The upper cylinder is connected to the main shell by four 4" pipes. The vent condenser (shell side) is protected from overpressure by an SRV with 2" inlet which relieves at 275 psig. The heat transfer area is 850 sq. ft. SL 010040 e Order ict Court 4-11 3. Vent Gas Scrubber (SAC 67-71). This vessel is 4' diameter by 18' high. It is constructed of Haveg 41 composite. The design pressure is full of water at 200F. The scrubber has a 12 foot packed section (150 cu. ft. of packing) of 1 1/2" chemical porcelain Intalox saddles. The packing is supported by a 4 piece chemical porcelain Stoneware "Multi-Beam" support plate. A maximum water flow of 260 gpm is distributed over the packing by a chemical porcelain Stoneware "Weir-Trough" distributor. Water enters the scrubber through a 6" I.D. nozzle made of Haveg 41 with large opening (looking down) at the end. 4. HCl Surge Drum (SAC 60-869). This steel vessel is 6' l.D. by 6' tangent to tangent. It has 150 psig design rating at 200F design temperature. The vessel is protected from overpressur ing by a 2" x 3" SRV set at 65 psig with a rupture disc between the Surge Drum and SRV set at 100 psig. 5. TCE Vapor Separator (60-1015). This vessel is steel and is 30" I.D. by 5' seam to top flange. The design pressure is 50 psig to full vacuum at 300F design temperature. The top of the tank has a 6" Teflon demister. 6. Absorber Feed Cooler (71-661). This all steel exchanger has seventy-two 3/4" tubes. Both shell and tube side have 150 psig design pressure with 400F design temperature. The heat trans fer area is 170 sq. ft. B. Operation The HCl gas coming off the TCE reactor condenser contains sufficient EDC and TCE to contaminate products in the plants to which the HCl is ulti mately fed. These impurities are removed in an absorption and chilling operation. The major portion of the EDC in the HCl is removed in the EDC absorber. The HCl enters the absorber right below the packed section and is contacted with a TCE rich stream (Heavies still feed) as it passes up through the packing and out the top, EDC in the HCl is absorbed by the TCE, leaving a relatively EDC-free HCl gas. The absorber feed stream is cooled in the absorber feed cooler. Some cooling of the reactor off-gas also takes place in the absorber. SL 010041 4-12 Most of the remaining EDC and TCE are condensed out in the TCE reactor vent condenser. The HC1 stream passes through the tubeside of the condenser while liquid Freon 22 is evaporated on the shell side. The exit HC1 gas temperature is lowered to less than 50F, which leaves only trace quantities of organics in the product HC1. The Freon-22 system will be discussed in detail in a later section. The HCl and condensed organics flow from the vent condenser to the TCE vapor separator. The condensed organics are separated from the product HC1 in the vapor separator, and flow out the bottom of the separator to the corrosion products pot. This liquid stream will be further discussed in the "Absorber Bottoms System." The product HCl passes up through a demister in the vapor separator and out to the HCl surge drum. HCl to be fed to the MC reactor comes off the top of the surge drum, as does HCl which goes to the HCl distribution system. The flow rate of HCl to the MC reactor is flow controlled. The flow of HCl to HCl distribution is regulated to maintain the HCl surge drum pressure at 45 psig. This is the pressure control for the TCE reactor, EDC absorber and absorber bottoms system. This primary pressure control is backed up by a pressure control valve on the HCl to the vent scrubber. This controller is normally set to open to control the system pressure at 48 psig. Thus, any increase in system pressure above 48 psig will cause the HCl flow to be diverted to the vent scrubber. This over pressure could be caused by loss of HCl to HCl distribution, or primary HCl PCV malfunction. The vent scrubber is designed to take the entire HCl production at the peak 245 TPD rate. The HCl enters below the packed section and is . CONFIDENTIAL: Subject to Protective Order of 14th Judicial Lustrict Court No. 91-1145 CONFIDENTIAL* to Droto-t;vo Order Court 4-13 absorbed in water as it passes up through the packing. The water used is blowdown from No. 4 cooling tower, and is metered by a field-mounted orifice meter. This flow is normally regulated to control cooling water hardness concentration, but can be increased as necessary in emergencies. Maximum design water flow rate is 260 gpm. The HCl-water stream flows into the plant sewer system, and thus represents a direct chloride loss to the Company. Any unabsorbed gases are discharged out the top of the scrubber through a 4" Chemtite line which goes up the side of the VDC still. The top of the vent line is fitted with a small separator pot which traps any entrained liquid and drains it to the sewer through a 1" Chemtite line. Absorber Bottoms System: A. Equipment 1. Corrosion Products Trap (SAC 60-1016). This steel vessel is 18" O.D. by 3' seam to top flange. It is rated at full vacuum to 75 psig at a design temperature of 300F. 2. TCE Vent Condensate Drier (SAC 73-106). This steel drier is 2' Dia. by 6' flange to flange. It is protected by a 2" 100 psig graphite rupture disc. The desiccant charge is supported by a steel basket with two layers of fiberglass wool on the upper side. The desiccant consists of one foot of walnut-size calcium chloride topped off by enough flake calcium chloride to bring the total desiccant height to about 18" from the top flange. Carryover of calcium chloride is prevented by a tightly com pressed roll of fiberglass wool in the top of the drier. This dryer is available as a spare dryer. 3. Absorber Bottoms Pumps (SAC 55-1517, 1518). These pumps are ductile iron Goulds Model 3196, size 1 x 2-8. Each pump has an 8-inch semi open 316 SS impellor. The pump is powered by a 1750 rpm, 3 H.P. motor (SAC 50-2872, 73). The pump uses a John Crane type 9 seal. Each pump has an N2 purge line run to the seal flush line--this purge is used on the "spare" pump and has greatly increased seal life. 4. Absorber Bottoms Drier (SAC 73-100), also known originally as TCE Reactor Vent Condensate Drier. This is a steel drier, 20" O.D. by 6' flange to flange. The drier has a full vacuum to SL 010043 4-14 150 psig design pressure with 100F design temperature. The desiccant charge is supported by an expanded metal screen with two layers of fiberglass wool. The bottom one foot of desiccant is walnut sized calcium chloride, which is topped by flake calcium chloride up to 18'1 from the top flange. A tightly wound roll of fiberglass wool in the top prevents carryover of flake calcium chloride. 5. Absorber Bottoms Filter (SAC 72-237). Construction of this filter is iron and steel--its design pressure is 150 psig. It has a nine element charge of 75 micron 10" fiberglass filter elements. 6. Absorber Bottoms Heater (SAC 71-659). Steel is the material of construction of this shell and U-tube heater. It has twentysix 3/4" U-tubes, 16 BWG, 11'6" long. The design condition on both shell and tube sides are 150 psig at 400F. The tubeside is four pass. The heat transfer area is 121 sq. ft. 7. HC1 Separator (60-538). This vessel was the stripper reflux drum in the 75 TPD MC Plant. For this reason, it is nickel clad, 42" O.D. by 7'9" seam to seam. It has a 75 psig design pressure with 300F design temperature. B. Operation The condensed organic primarily TCE, from the TCE vapor separator contains the highest concentration of water in the TCE system. This is due to its low temperature (less than 50F). If this stream is returned to the absorber system, the water content will be caught up in an internal recycle; i.e., it will flash off in the hot absorber, go overhead, be recondensed in the vent condenser and continue to build up in the systan. The stream formerly went through the vent condensate dryer, but since it was not effective, the dryer has been bypassed and remains only as a spare dryer in the unit. Because of the moisture buildup, the vent condensate is purged from the system--it is sent to the Per-Tri recycle tank. The purge rate is automatically controlled so as to maintain a constant level in the corrosion products trap. Flow of this stream can be diverted into the absorber for short periods of time if the level in the TCE vapor separa tor gets out of control. SL 010044 COKFIDIHJTJAL: Subject to Protect:-"e Order of 14th Judicial itir.trict Court Mo. 91-1145 Of 14th :t t f-rc Jl lQ , r ' i () i /; j. too. 9]- ii<5 ict C'o ur t- 15 The bottoms stream from the absorber is saturated with HCl, and is primarily TCE. The suction line to the absorber bottoms pumps is water jacketed to subcool the liquid and prevent flashing of the HC1 in the pump. Absorber bottoms are pumped from the absorber through the absorber bottoms drier and filter to the absorber bottoms heater. The temperature of the absorber bottoms is raised from about 140 to 160F up to 220F in the tube- side of the heater. Steam flow to shell of the heater is controlled to maintain this temperature. The flowrate of the absorber bottoms is con trolled by a level control valve (LCV) downstream of the heater so as to maintain a constant level in the bottom of the absorber. The LCV dis charges into the HC1 separator. Gas is flashed overhead from the HCl separator and goes back to the vapor space of the TCE reactor. The absorber bottoms pump discharge pressure (about 85 psig) is dropped to the TCE reactor pressure across the LCV. This combination of heating and flashing removes most of the HCl from the absorber bottoms stream. The liquid flows off the bottom of the HCl separator to the lights still. The flowrate is controlled by a LCV to maintain a liquid level in the HCl separator. The lights still is a lower pressure vessel (normally about '5 psig at the point where the HCl separator liquid is fed) and for this reason flashing can occur across the LCV. Experience has shown that if the outlet temperature on the absorber bottoms heater exceeds 230F, excessive flashing does occur in the line downstream of the LCV. This gives excessive pressure drop and can cause a high level in the HCl separa tor. On the other hand, too low a temperature will give poor HCl separation and will increase the vapor load on the lights still. SL 010045 Lights Still System: CONFIDENTIAL: Sabject: to !- :roze t . vg Order of 14th Juciicia^ i Lslrict Court No. 91-1145 4-16 A. Equipment 1. Lights Still (SAC 67-66). The still is constructed of steel and is 84" X.D, by 98'6" seam to seam. The design conditions are full vacuum to 50 psig at 400F. It is protected from over pressure by 10" 50 psig graphite rupture disc. The column has 60 trays with 18" tray spacing. The trays are the Glitsch design with V-l ballast units. The primary feed points (TCE reactor liquor) are located at trays 35, 39, 43 and 47. The normal feed point is tray 47. The recycle feed points (for HCl separator liquid) are located at trays 17, 21, and 25. The normal feed point is tray 25, 2. Lights Still Feed Pump (SAC 55-808). The feed pump is a Goulds Model 3196, size 2 x 3-8, with an 8" impellor. The construction is ductile iron with a 316 S.S, semi-open impellor. It is powered by a 5 h.p. 1750 rpm motor. A John Crane Type 9 mechani cal seal is used. 3. Lights Still Reflux Pumps (SAC 55-1491, 92). No. 1 reflux pump serves as a spare for both the feed pump and No. 2 reflux pump. The reflux pumps are Goulds Model 3196, size 2 x 3-13. The pumps are constructed of ductile iron with a 13" semi-open Type 316 S.S. impellor. John Crane Type 9 mechanical seals are used. 4. AIBN Pumps (SAC 55-1791, 1792). These pumps are Crane Chem/ meter 200 series diaphram metering pumps. They are reciprocat ing plunger, positive displacement pumps utilizing a dual head on the pump to deliver a constant output flow. The pumping action is due to a diaphram in each head moving the fluid through a chamber having check valves on the suction and discharge. To change the flow the DC drive motor speed is varied by an adjust ment made in the control room on a manual potentiometer. Capacity of each pump is 20 gallons per hour steady flow. 5. Lights Still Condenser (SAC 71-1199). Steel is the construction for this condenser. It has 910 - 3/4" O.D. 16 BWG steel tubes, 12' long. The shellside design pressure is 150 psig and design temperature is 300F. The tubeside is rated at 150 psig at 12CtF design temperature. The exchanger is fitted with double tubesheets. The space between each set of tubesheets is under continuous air purge. Cooling tower water makes two passes on the tubeside. The heat transfer area is 2144 sq. ft. 6. Lights Still Reboilers (SAC 71-1200, 1220). The reboilers are identical and are constructed of steel. Each reboiler has 745 - 1" O.D. 12 BWG tubes, 12' long. The shellside has 150 psig SL 010046 CONPTDFN?l A' Subject to "; of 14th Jutir, -i i V r> rr ,, ,OrCr'fninr rV design pressure at ^0 F (^esjl^n temperature.' 4-17 The tubeside is rated at 150 psig at 400F. The heat transfer area is 2340 sq. ft. each. 7. Lights Still Secondary Condenser (SAC 71-522). This is an exchanger converted from a former thermosyhon reboiler service to a horizontal partial condenser. It has all steel construc tion with 31 - 3/4 O.D. 12 BWG tubes, 8' long. Heat transfer surface area is 48 sq. ft. Shellside design pressure is 150 psig at 400F, while tubeside is rated at 150 psig at 200F. The tubeside is single pass. 9. Heavies Still Feed Drum (SAC 60-1018). Steel is the construc tion for this 6' O.D. by 8'8" seam to seam tank. The vessel is designed for full vacuum to 50 psig at 300F design tempera ture. Protection from overpressure is provided by a 4" 50 psig rupture disc. Capacity of the drum is 2078 gallons, full. 10. No. 1 and 2 AIBN Mix Tanks (60-1190 and 1191). These are steel tanks 5*-0" l.D. by 3'6" tangent to tangent. Each tank has a capacity of 636 gallons and each is protected by a 2" 100-pound graphite rupture disc. Each tank is equipped with an 8" tube turn hinged lid recharging nozzle on top. Mixing of the AIBN and EDC is accomplished by a 316 S.S. Penberthy 3/4" circulat ing tank eductor installed in each tank and the AIBN mix tank recirculating pump. 11. AIBN Mix Tank Recirculating Pump (55-1793). This is a Goulds lxl 1/2-8 Centrifugal pump with a 6 1/4" impeller. It is powered by a 2 h.p. 1735 rpm motor. A John Crane Type 9 mechanical seal is used. Flow rate is gpm. B. Operation The function of the lights still is to remove the unreacted EDC from the TCE reactor liquor. The EDC is then recycled back to the TCE reactor. Any EDC which goes out the bottom of the lights still will react to give an undesirable impurity in the VDC section, or go unreacted into the MC section and end up in the MC product. The maximum allowable EDC content in the lights still bottoms is 0.03%. The EDC in the lights still feed and the recycle (HC1 separator liquid) feed are taken overhead and condensed in the lights still condenser. This condenser is a partial condenser in that the dissolved HC1 in the feeds is driven overhead from the still and is only partially reabsorbed SL 010047 C0NFIDFNT17\L* Subject to Protect^ Ordr 14th Judicial District Court No. 91-1145 4-18 in the condenser. The vent HCl stream then goes to the Lights Still Secondary condenser where it is chilled by chilled brine which is on the tube side. The source of this F chilled brine is in the HCl plant. The vent stream temperature from this condenser varies somewhat with lights still feed rate, but should be considerably under 100F. This vent stream goes to the lights still seal pot and then to the vent scrubber. The purpose of the seal pot is to provide a liquid seal such that moisture from the scrubber system cannot back up into the lights still system. The liquid streams from the lights still condenser and secondary condenser flow into the lights still reflux drum. This liquid, which is primarily EDC, is partially returned to the lights still via the reflux pump and a flow control valve (FCV). The flow is set to match the feed rate (a 1:1 reflux to feed ratio). The balance of the overhead stream is returned to the TCE reactor via a LCV which maintains a constant level in the reflux drum. This lights still recycle stream goes into the bottom of the TCE reactor right above the chlorine spargers. A1BN is pumped from the AIBN tanks into the recycle stream. Heat input to the lights still comes from the two vertical thermo syphon reboilers. Steam flow to the shell of these exchangers is controlled so as to maintain a specified temperature profile. The top pressure on the lights still normally runs about 2 to 5 psig, with about 10-13 psig bottom pressure. Under these conditions, the top temperature of the column should be maintained below about 200F in order to keep excessive amounts of TCE from going overhead. TCE in the overhead will be recycled back to SL 010048 CONFIDENTIALr Subject to rrot'f't i''" Order of 14 th Oudict.? v' ^ >-< i e J :"t Do. ?i-'l Subject of 14th J, No. J V0 t-* j i 91-1145 (') r- 4-19 the TCE reactor, and thus raise TCE concentration in the reactor. The bottom temperature should run about 290F. Experience to date has shown that about 222-225F at tray 26 with a top column pressure of 2-5 psig will give in-specification EDC content in the still bottoms and less than 0.5% TCE in the overhead with a 1:1 reflux to feed ratio. The TCE-heavies stream flows from the lights still to the heavies still feed drum via an overflow line. The overflow is located such that the liquid level in the still is about four feet above the top tubesheet of the reboiler. A separate line provides means of equalizing vapors between the feed drum and the lights still during level changes in the feed drum. The feed rate to the lights still from the TCE" reactor plays a major role in determining the TCE reactor concentration. Increasing the feed rate will take more TCE out of the reactor and thus lower the TCE concentration. Conversely, lowering the feed rate increases the TCE con tent. It should be noted that when the feed rate is raised, a decrease in TCE reactor level will occur. Normally, when TCE reactor level drops more EDC is added to maintain the level. In the case of a feed rate change, the change in level will be partially compensated for by changes in the EDC recycle flow from the lights still. This recycle flow will change because the amount of EDC being fed to the lights still is changed. The change in recycle flow will not be immediate because of surge time in the lights still and reflux drum. Thus, EDC feed changes should be made with the realization that more (or less) recycle will be coming back from the lights still. SL 010049 CONFIDENTIAL: Subject t O p f Q p -- ' of 141JJi JJuudriicu: L i: No. S1 -1 x n**Slaj- 4-20 In order to maintain a minimum amount of heavies and HC1 formation ' in the reactor, the lights still should be operated at full design rate. Experience has shown that the overhead condensing equipment is the limiting factor on the lights still system. Minimum ICE reactor concentration is obtained by feeding the lights still such that a recycle flow rate of 75 to 78 gpm is established. This loads the condensing equipment, but does not normally give excessive vent temperature from the secondary condenser. At low production rates (say 100 TPD), this will result in 16 to 18% TCE in the reactor. At peak 245 TPD rate, the design still feed rate is 109 gpm with a 66 gpm recycle rate. This will give about 36% TCE in the TCE reactor. Relation of TCE Reactor Chlorination with the Lights Still: AIBN flow to the Lights still recycle is regulated to keep free chlorine from coming out of the TCE reactor in the lights still feed stream. Chlorine breakthrough is checked for every hour by mixing a small sample of lights still feed or TCE reactor overhead HC1 with an orthotolidene - H2O solution. Presence of free chlorine is indicated by a yellow to red color; i.e., small amounts of free chlorine result in pale yellow color, while a major chlorine breakthrough is indicated by dark red color. This mixture should be clear at all times. If a color is developed, an increase in AIBN flow must be made. This is accomplished by increasing the setting on the AIBN pump or starting the spare pump, or even increasing the strength of AIBN in the feed tanks. SL 010050 CONFIDENT* orfler fn pro:--1; . Subject- to . < ; i 1 of I*th JU'io. 91 -11 cour1 cowry nr Subje 't 1-. I: , Of 14th Oucli r :; No . y \ T A L; '"'.-i'rv. Order ^tricL Cc^T?t A- If the chlorination cannot be controlled by either additional AIBN flow or by use of a higher concentration of A1BN in the AIBN feed, the TCE reactor must be shut down. Do not use ethylene to control chlorination in the TCE reactor. If the TCE reactor chlorinates badly all of a sudden, shut the TCE reactor down. Do not fight a sudden, bad chlorination with AIBN or ethylene. In either of the above cases, notify supervision immediately. Free chlorine analyzers on the TCE reactor vapor line and the reactor liquor give a continuous monitoring for presence of free chlorine in the system. Iron formed by corrosion in the lights still and absorber bottoms system will flow down the lights still and to the heavies still. This iron is very detrimental to reboiler life on both the lights and heavies stills reboilers. The iron will deposit out on the tube surface, and will also promote cracking. Tri-cresyl phosphate (TCP) is added to the pot of the lights still to tie up the iron. The TCP and iron form a com plex which does not easily deposit on the tube surface or promote cracking. Control of the TCP flow will be discussed under heavies still operation. Heavies Still System: A. Equipment 1. Heavies Still (SAC 67-13). This vessel is all steel construc tion, 5'3" I,D. by 97'6" tangent to tangent. The still was con verted from former lights still service in the 75 TPD plant. It is designed for full vacuum to 50 psig with 400F design temperature. The column is fitted with 60 trays*with 18" spac ing between each tray. The trays use Glitsch Type V-4 ballast units. All the feed points used when in lights still service were tied together by a common feed header, so that feed may be introduced at trays 18, 22, 26, 40, 44, 48, and 52. Currently, feed is going to tray number 18. The column is protected from overpressure by a 6" 50 psig graphite rupture disc. SL 010051 CONTI DITTI AN: Subject to Protective Order of 14th Judicial rostrict Court No. y1-1145 4-22 2. Heavies Still Reboiler (SAC 71-1245). The reboiler is con structed from steel. It has a shell side design pressure of 120 psig at 630F (150 psig at 400F), while the tubeside has 150 psig design pressure with 400 F design temperature. The reboiler has 745 1" tubes, 12 BWG, 12 long, which give a total heat transfer area of 2340 sq. ft. This reboiler is spared by an identical one (71-1438) which is stored in the plant area. 3. Heavies Still Condenser (SAC 71-648). The condenser is all steel and has 506 - 3/4" 0.0., 16 EWG, by 12' long tubes. Both shell and tube sides are rated at 150 psig with 400F design temperature. The total heat transfer area is 1192 sq. ft. 4. TCE Product Cooler (SAC 71-1201), This shell and tube exchanger is all steel construction with 92 - 3/4" tubes, 16 BWG, 12' long. The shellside has 150 psig design pressure with 300F design temperature, while the tubeside has 150 psig design pressure with 150F design temperature. The total heat trans fer area is 216 sq. ft. The tubeside is four pass. 5. Heavies Still Reflux Drum (SAC 60-553). This horizontal steel tank is 6' O.D. by 8'8" seam to seam. It has a capacity of 2078 gallons. The tank is designed for full vacuum to 50 psig at 300F. It is protected from overpressure by a 6" 50 psig graphite rupture disc. 6. TCE Storage Tank (SAC 60-1020). The storage tank is a vertical steel tank 18' O.D. by 22' high. It has a design pressure of -3 ounces to 1.4 psig at ambient temperature. The total capacity is 41,600 gallons (full) with each foot of level holding 1,890 gallons. The tank is fitted with a 4" Chemtite vent line which goes to a small Haveg seal pot. This seal pot is designed to hold a water level of a few inches over the vent line. Thus any increase in pressure (due to filling the tank) will over come the liquid head of the water and allow venting of the tank vapors through the water seal. Conversely, any drop in tank pressure is compensated for by a nitrogen makeup pressure con trol valve. Further protection against forming a vacuum is given in the design of the water seal pot. The seal has a short leg, filled with Perchlor which will be pulled into the seal pot and provide a breathing opening if a vacuum should develop. 7. Heavies Still Seal Rot (SAC 60-1105). This steel tank is 18" O.D. by 3' tangent to tangent. It has a 2" *50 psig graphite rupture disc. 8. Heavies Still Feed Pumps (SAC 55-1493, 94). These pumps are Goulds Model 3196, size 1 1/2 x 3-13. They are constructed of ductile iron with 316 S.S. semi-open impellers (10 1/2"). The pumps are powered by 10 horsepower, 1750 rpm motors (SAC 50-2848, 49). The pump uses a John Crane Type 9 mechanical seal. SL 010052 Let Court o 4-23 9. Heavies Still Reflux Pumps (SAC 55-806, 807). The pumps are Goulds Model 3196, size 2x3- 13 with 12 1/2" semi-open impellor. The construction is ductile iron with a 316 S.S, impellor. A John Crane Type 9 mechanical seal is used. The motors are rated 20 h.p., 1750 rpm (SAC 50-1541, 42). 10. Heavies Still Bottoms Pump (SAC 55-1495, 96). The pumps are Goulds Model 3196, size 1x2-6. It is constructed of ductile iron with 5 7/8" 316 S.S. semi-open impellor. The motors (SAC 50-2850, 51) are rated at 1 h.p., 1750 rpm. 11. Heavies Still Bottoms Drier (SAC 73-101). This steel vessel is 18" O.D. by 6* flange to flange. It was fabricated by PPG and has a 2" 100 psig graphite rupture disc. The desiccant charge is supported by an expanded metal screen with 2 layers of fiberglass foam. Flake calcium chloride (250 pounds) is the dessicant. Carryover of the flake is prevented by a tightly wound roll of fiberglass wool at the top of the vessel. 12. Heavies Still Bottoms Filter (SAC 72-248). 13. Heavies Still Bottoms Booster Pump (55-642). This pump is an Ingersoll-Rand 1 CRVN pump with a 5 1/2" impeller. It is powered by a 3 hp 1750 rpm motor. It is used in series with the Heavies still bottoms pump to give sufficient head to send the bottoms directly to the Per-Tri recycle tank. This pump is located in the No. 1 EDC plant. B. Operation The function of the heavies still system is to separate the heavier chlorinated organics from the TCE, leaving a high purity TCE product. The concentration of heavies in the feed stream varies with TCE reactor con centration; the designed maximum content is 12% tetrachloroethanes at full design rate. The liquid in the heavies still feed drum is pumped from the drum through a FCV to the heavies still. This flow rate is regulated to maintain the desired level in the feed drum. The heavies are concentrated by distillation in the bottom of the heavies still. Heat input is supplied by the vertical thermosyphon reboiler which has steam condensing on the shell side. TCE is boiler overhead from the still, condensed in the horizontal SL 010053 Subject tr 1 of 14th Juciic.. ....... NO- 91-1 vs Order t ric t Court 4-24 heavies Still condenser and flows by gravity into the heavies still reflux . drum. Part of this condensed stream is pumped back to the heavies still as reflux. The balance, which is the TCE product, is pumped from the reflux drum through the TCE product cooler to the TCE storage tank. The flow rate of the TCE product is automatically regulated to maintain a constant reflux drum level. Any inerts in the heavies still are vented off the condenser into the heavies still seal pot. The vent line goes down into the seal pot under a liquid (heavies still bottoms) level. The inerts then pass out of the seal pot into the vent header going to the vent scrubber. Any decrease in heavies still pressure is compensated for by a nitfogen makeup PCV. The bottoms from the heavies still are pumped to TCE bottoms storage tanks in the EDC plant via a LCV which maintains a constant level in the pot of the still. When the iron content is low in the bottoms, they are pumped directly to the Per-Tri recycle tank via a booster pump located in the EDC plant. The bottoms pumps also discharge into the heavies still bottoms drier and filter. The effluent from the filter goes back into the pot of the heavies still. This recirculation system through the drier- filter has proven to effectively remove most of the solids which contribute to fouling of the heavies still reboiler. The name "drier" is actually a misnomer in that any moisture in the heavies still will azeotrope overhead and thus the drier will not actually remove moisture. The large surface area provided by the flake calcium chloride "desiccant" provides area on which iron and contaminants deposit. The recirculation flow rate is manually regulated at a rate which just gives enough pump discharge pressure to flow through the LCV to storage. SL 010054 cr ' . ci: Court 4-25 The operating conditions for the heavies still are fairly straight forward. The design reflux ratio is 2 to 1 (reflux to product flows). Currently a 2 to 1 reflux to feed ratio is being used satisfactorily. The column top pressure normally runs about 1/2 to 1 psig. Bottom pressure is dependent upon rate; however, experience has shown 8 psig to be normal bottom pressure at 150 TPD. Under these pressure conditions, a bottom (pot) temperature of 285F has proven to give the desired concentration of TCE in the bottoms stream. Currently the steam flew to the reboiler is automatically controlled to give 262F at tray 4, when the bottom pressure is about 8 psig. This will meet the 285F pot temperature requirement, yet provides good control. In order to make pure enough TCE feedstock for VDCM grade VDC crude. the heavies still bottoms temperature is dropped to 280F. This increases the blowdown off of the bottom but it enables the heavies still product to remain at the 99.997. purity up to a rate of approximately 220 tons per day production rate of TCE. With this pure TCE, VDC crude containing less than 100 ppm DCA is normally produced. At this level the morpholine treat ment step in the VDCM plant can be bypassed and the VDC crude is further purified by redistillation in the VDCM still. With a bottom temperature of 285F TCE concentration in the heavies still bottoms stream runs about 2570, which is normally sufficient to purge contaminants (which are capable of fouling the reboiler) from the still. However, at the 280F bottom temperature, the TCE concentration approaches 507o. This TCE is not lost as it is fed to the Per-Tri recycle tank. The iron content in heavies still bottoms ranges from 50 to 250 ppm. The calcium chloride charge in the bottoms recirculation system should be renewed if the iron content exceeds this. 010055 C0NFIDENTJA Tri-cresyl phosphate (TCP) is normally fed to the heavies still in ,, the heavies still feed. TCP is necessary to complex the iron and prohibit it from catalyzing the cracking of tetrachloroethane in the heavies still reboiler by the following reaction. HH Cl - Cl - Ci - Cl Cl Cl Sym. TeCE (or Unsym TeCE) + Iron and Heat Cl Cl - 9 = C - H Cl + HC1 Trichloroethylene The trichloroethylene formed in the reboiler is carried overhead with the TCE product, since Trichlor is more volatile than TCE. The flowrate of TCP to the lights still is regulated so that the concentration of trichloroethylene in the heavies still overhead is less than 0.02%. Any trichlor fed to the VDC system leads to the formation of the color producing impurity (DCA), and thus control of this is important. During startup or upset conditions (possibly TCE reactor chlorination), TCP can be added directly to the heavies still pot. The TCP is mixed with TCE (a 50-50 mixture) in the TCP addition tank. The tank is operated at full line nitrogen pressure (90 psig) and the TCP is metered to the stills by a small purge rotometer. The TCE is added to TCP because TCP is very viscous the 50-50 mixture is much easier to meter than straight TCP. Toxicity of Heavies Still Bottoms; The bottoms stream off the heavies still contains the tetrachloro- ethane in a concentrated form. Tetras are very toxic (see Safety section for details). Great care should be taken to prevent inhalation or splash ing on body of this stream. Gloves and respirator should always be worn when sampling or working with the bottoms equipment. sL 010056 TCE Rework Line: 4-27 Rework of TCE from TCE storage back to the lights and heavies still is possible via a 2" rework line. The line originates at the TCE to VDC header and ties into the suction of the lights still feed pumps and to the discharge of the heavies still feed pumps. The TCE to the TCP tank is a side stream off the rework line. TCE to the Per-Tri plant also takes off the rework line. Off specification TCE may be reworked back to the stills as required. The line is also very convenient for recycling the TCE section still train to and from TCE storage. C 0 F 7 D F, N T -t A LU Subject to Pf.-ctcct'- vc Order Of 14th Judicial D'i sLi oict Court No. 91-1145 SL 010057 C* kj J -Of 14 th tilO. VDC SECTION ^ Ui L4-28 Chemical Reactions: The dehydrochlorination of TCE to form VDC, and associated reactions are described by the following reactions. HH Cl H Cl-C-C-H + NaOH --* Cl - C = C - H + NaCl + H20 Cl Cl TCE VDC The NaCl formed in this reaction is not recoverable. Thus, there is a built-in theoretical loss of one-third of the chloride fed to the VDC system (this amounts to one-fourth the chloride involved in the overall Tri-Ethane plant). The reaction also yields small amounts of the cis and trans isomers of VDC. HH Cl - C = - H Cl Cl Cis-1,2,dichlorethylene Cl H C=C-H Cl Trans-1,2-dichloroethylene Heavies such as tetrachloroethane, either symmetrical or unsymmetrical, can also be dehydrochlorinated as follows to form trichloroethylene: Cl H Cl-C-C-H + NaOH --------- Cl - C = C - H + NaCl + H20 Cl Cl Cl Cl Unsym-TeCE Trichloroethylene Trichlor is further dehydrochlorinated ("caustic cracked") to form the color producing impurity dichloroacetylene (DCA). Cl - C = C - H + NaOH -------- Cl - C = C - Cl + NaCl + H20 Cl Cl Trichlor DCA A small amount of VDC is also further "caustic cracked" to form monochlorace tylene (MCA). Cl H Cl - C = C - H + NaOH -------- Cl - C s C - H + NaCl + H20 VDC SL 010058 MCA CONFIDENTIAL: Subject to Protec'Jv? Order Of 14th Judicial D^trict Court Mo - 91-1*4 5 4-29 VDC is a relatively unstable material in that when it is in contact with air it will form peroxides. These peroxides are extremely hazardous. In the dry from, they will explode violently from heat or shock; consequently their formation is to be avoided. This is accomplished by two methods. First, oxygen is prevented from contacting VDC by padding the entire VDC system with nitrogen, thereby eliminating the possibility for the reaction to occur. A second precaution is that all VDC in the liquid phase is stabilized with hydroquinone monomethyether (HQMME). HQMME is an oxygen and free radical scavenger. Vinylidene chloride is commercially polymerized to make several types of plastics. This polymerization must be reduced to a minimum in the VDC section in order to keep lines and equipment in workable condition. Polymerization of VDC can be initiated by the presence of iron, oxygen, free radical initiators, and sunlight. All equipment which contacts VDC in the crude VDC system is constructed of stainless steel or nickel cladded to eliminate iron as a polymer initiator. As described above, the liquid VDC is stabilized with HQMME to scavenge any oxygen or free radicals which might be present. The effects of sunlight are diminished by using amber glass on all sight glasses. The triple bond impurities, MCA and DCA, are very unstable. The exact role they play in polymerization is not known. The reactivity of MCA is demonstrated by the fact that it will spontaneously ignite when it comes in contact with air. They are normally diluted enough in the VDC streams to be no problem; however, any abnormal cone---tration of these impurities must be prohibited. 5V. rONFlDENTlM'1 -c order rict court 4-30 VDC Reactor and Still System: A. Equipment 1. VDC Reactor (SAC 59-20). This column is 4'6" I.D. by 54' seam seam. The reactor is constructed of Type 316 stainless steel. The design pressure is full vacuum to 50 psig at 350F. Over pressure protection is provided by a 8n 50 psig graphite rupture disc. The steam inlet at the bottom consists of an Inconel sparger pipe with an ell directing steam flow down. The end of the ell discharges into an Inconel pan which redirects steam flow outward and up. The reactor has 39 trays. They are Glitsch ballast trays with Type V-l and V-IX on trays 1 and 25 through 39. Trays 2 through 24 has Type V-4 and V-4X ballast units. The trays and ballast units are Type 316 stainless steel. They are mounted with 12" tray spacing except at the feed points. The bottom feed point, tray 20, has a 24" tray spacing. At feed trays 24 and 28, the tray spacing is 18". Feed is introduced into the column at each point by a sparger with holes drilled in the bottom. The reactor pot has been lined with Inconel. 2. VDC Still (SAC 67-67). The still is constructed of Type 316 stainless steel and is 5'3" I.D. by 76' seam to seam. The design pressure is full vacuum to 50 psig at 350F. It is protected from overpressure by an 8" 50 psig graphite rupture disc. Steam enters the bottom through a 10" stainless line into a tee mounted so that the steam is discharged to the side out each end of the open tee. The still has 57 Glitsch ballast trays with combinations of the V-l and V-IX ballast units. Construction of the trays and ballast units is Type 316 stainless steel. The tray spacing is 12" except for the feed trays (27, 31, and 36). The bottom three trays have the free moving ballast units removed, and thus are acting as "dual flow trays". 3. TCE Product Pumps (SAC 55-804, 805). These are Goulds Model 3196, size 1x2-8. They are constructed of ductile iron with 316 S.S. semi-open impellors. The impellor size is 6 1/2". The motors for the pumps (SAC 50-1539, 1540) are 10 h.p., 3600 rpm. A John Crane Type 9 mechanical seal is used. 4. Cell Liquor Pumps (SAC 55-759, 760). These pumps are Goulds Model 3.196, size 1x2-8. They are constructed of ductile iron with 8" cast iron semi-open impellors. The pumps are powered by 20 h.p., 3600 rpm, motors (SAC 50-1475, 1476). Sealing is provided by a packing gland. These pumps are located in the Caustic area. 5. Retention Tank Pump (SAC 55-1497). This pump is a Goulds Model 3196, size 4x6- 10. It is constructed of Type 316 S.S., with 9 1/2" 316 S.S. semi-open impellor. It is driven by a 30 h.p., 1800 rpm motor (SAC 50-2852). It uses a packing gland with a cooled condensate water flush stream. SL 010060 CONFIDENTIAL: Subject H Of 14th j of. Court 4-31 6'. VDC Still Reflux Pumps (SAC 55-1498, 1499). The reflux pumps are Goulds Model 3196, size 1 1/2 x 3 - 13, They are constructed of Type 316 S.S. with 11 1/2" S.S. semi-open impellor. They are driven by 15 h.p., 1750 rpm motors (SAC 50-2853, 2854). A John Crane Type 9 mechanical seal is used. 7. HQMME Addition Pumps a. No. 1 HQMME Pump (SAC 55-1149). This pump is a Lapp Pulsafeeder type CPS-3. It has a rated capacity of 4.25 gpm. The head is stainless steel and the diaphram is Teflon. It is powered by a 1 hp 1730 rpm motor (SAC 50-2301). (See Auxiliary Equipment Section for detailed operating description.) b. No. 2 HQMME Pump (SAC 55-562). This pump is a Lapp Pulsafeeder CPS-2 with a remote operating head. It is stainless steel with Teflon diaphragm. The pump is driven by a 1/2 h.p., 1750 rpm motor (SAC 50-1211). 8. VDC Still Bottoms Pumps (SAC 55-1515, 1516). These pumps are Gounds Model 3196, size 1 1/2 x 3 - 10. They are constructed of Type 316 S.S. with 8 3/8" S.S. semi-open impellors. The pumps are driven by 3 h.p., 1750 rpm motors (SAC 50-2870, 2871). 9. VDC Retention Tank (SAC 60-1021). This vertical tank is 4' OD by 10' tangent to tangent. It is constructed of Type 316 S.S. The design pressure is full vacuum to 75 psig at 300F. It has a capacity of 1018 gallons. Overpressure protection is provided by a 3" 75 psig Teflon-Monel-Teflon rupture disc with a 3" x 4" SRV (65 psig relief pressure) mounted over the disc. 10. VDC Still Phase Separator (SAC 60-1022). This horizontal tank is 6' O.D. by 14'8" seam to seam. The construction is 316 S.S. The design pressure is full vacuum to 50 psig at 300F. The capacity is 3390 gallons. The tank has a 4" 50 psig graphite rupture disc. A phase-off line is located at the 2.5" level. 11. HQMME Tank (SAC 60-416). This horizontal steel tank is 36" O.D. by 6'. It is rated at atmospheric pressure at 300F. The capacity of the tank is 317 gallons. A hairpin heater coil is mounted internally at the bottom--the coil is 1/2" diameter schedule 80 pipe. 12. HQMME Tank Agitator (SAC 61-64). This is a Lightnin Model N33G200, top entering mixer. It is driven by a 2 h.p., 1750 rpm motor. It has an 8" propellor type agitator which rotates at 350 rpm. 13. Cell Liquor Heater (SAC 71-1202). This shell and tube exchanger is all steel, with 76 - 3/4" O.D., 16 EWG by 12' long tubes. It has a shellside design pressure of 150 psig at 400F, or 120 psig at 650F; tubeside design pressure is 150 psig at 360F. The exchanger is two pass on the tubeside. The heat transfer area is 179 sq. ft. confids&tial to Protects SL tDObCA 4-32 14. Condensate Cooler (71-1203). This exchanger is all steel. It has 110 - 3/4" O.D. , 16 BWG tubes, 12' long. The shellside design pressure is 150 psig at 400F, while the tubeside is rated at 150 psig at 150F. The heat transfer area is 259 sq. ft. The tubeside is two pass. 15. VDC Still Condenser (SAC 71-1204). The heads and tubeside of this condenser are Type 316 S.S. It has 1068 - 1", 16 BWG tubes, 12' long. The shellside (made of steel) has a design pressure of 75 psig at 150F, while the tubeside is designed for 75 psig at 300F. It has a heat transfer area of 3355 sq. ft. B. Operation The function of the VDC reactor system is to bring TCE and sodium hydroxide in intimate contact under the temperature conditions necessary to form VDC. The source of sodium hydroxide is either cell liquor and/or "press wash" from the Caustic area. Cell liquor normally contains about 10% NaOH, whereas press wash NaOH concentration varies, but will normally be higher than cell liquor. Cell liquor contains about 17.5% NaCl; this salt is lost when fed to the VDC Reactor. Press wash is used whenever available because it is much lower in NaCl content, thus giving a lower salt loss to the Company when it is fed to the reactor. This lower feed NaCl content also tends to aid the VDC reaction. Cell liquor/press wash (hereafter referred to as cell liquor) is pumped from storage tanks in the Caustic area and is flow controlled to the VDC Reactor system. The cell liquor pumps are provided with a recir culation line from the discharge back to the tanks; thus, any shutdown of cell liquor in our area does not cause deadheading of these pumps in the Caustic area. Any major changes in cell liquor flow, however, should be communicated to the Caustic area lead operator. The temperature of the cell liquor is adjusted to 145F in the cell liquor heater. Steam to the shell of this exchanger is regulated to give the desired temperature. The exchanger is also piped up to use well water to cool the stream, which is often necessary in summer months. An automatic controller SL 010061 CONFIDENTIAL: Subject tc Protective Order of 14th Judicial District Court No. 9]-J!4 5 4-33 is available which will control the combined TCE-cell liquor feed stream temperature. This controller adjusts steam flow to the cell liquor heater as required. TCE is flow controlled into the line carrying the cell liquor. This combined stream is two phase, the liquid TCE and the aqueous cell liquor. The stream then goes into the retention tank where it is recir culated at a rate of about 800 gpm by the retention tank recirculation pump. The mixed feed discharges from the top out to the feed line to the reactor. In years past the salt buildup in the retention tank (due to reac tion) was great enough to restrict the feed piping and result in bursting of the retention tank rupture disc and relieving of the SRV. However, the rupture disc piping was also subject to plugging which could result in a possible overpressuring of the retention tank itself. To eliminate this plugging problem due to the salting out, enough condensate is added to the retention tank to keep the salt in solution. 15 gpm cooled condensate to the tank is added through the SRV nozzle (to ensure that the nozzle is kept flushed clear). The condensate flow is metered and alarmed to be sure that sufficient flow is maintained going to the retention tank. The low flow alarm is set at 12 gpm. Retention tank pressure is monitored at the SRV nozzle. If the pressure on the retention tank reaches 45 psig a high pressure alarm sounds. At 60 psig the system is automatically shut down by solenoid valves bleeding the instrument air pressure off of the TCE and cell liquor flow control valves, thus shutting off the feeds. SL 010062 CONFIDENTIAL! Of S1u4btjhecJt utdoicPiarlotDecistitvreictOrCdeorurt No. 91-1145 4-34 To put the retention tank back in service, the system pressure must drop below 60 psig; in addition a reset button located on the control board must be pressed before the feed FCV's will operate. This prevents an inadvertent readdition of feeds to the retention tank before the system has been checked out. A valve is located on the condensate line at the retention tank SRV nozzle so that the shutdown system can be checked while the VDC sec tion is running. The condensate flow is throttled, thus raising the sensed pressure to the alarm and shutdown points. Of course, the feed FCV's must be bypassed to prevent a serious upset of the system. As in the CI2 vpaorizer shutdown system, the bypass valves on the TCE and cell liquor FCV's are shut and sealed. The seals carry the .same significance as a lead operator's tag. Detailed procedures on checking the shutdown system are located in the MC plant Standard Operating Procedures Manual. The VDC section can run at about 22 gpm TCE feed without the retention tank being in service; so, if problems develop with the reten tion tank, it can be bypassed without shutting down the VDC section. The mixed cell liquor-TCE feed is normally fed to the VDC reactor at tray 24. The function of the reactor is to provide intimate contact between TCE and cell liquor and to separate the VDC produced from the react ing mixture. Heat is introduced to the bottom of the reactor via live steam injection. The steam flow is regulated to maintain the temperature at the bottom of the reactor high enough to keep TCE from being lost out the bottom of the reactor. The top of the reactor must be cooled so that rectification of the VDC product mixture (including water, cis, trans, Trichlor, MCA, and DCA) SL 010063 CONFIDENTIAL: su b jec: t t , !' 1 ->t ne r i v Order 14th Judicial District Court No. 91-1.14 5 4-35 from TCE will occur in the top of the reactor. If this separation is not accomplished, TCE could go overhead and be lost to the VDC reactor system. Cooling is provided by a VDC reflux flow and by a cooled condensate flow. The condensate comes from the Tri-Ethane condensate collection tank and is pumped through the condensate cooler before being flow controlled to the top tray of the VDC reactor. The cooling tower water flow to the condensate cooler is regulated to maintain the condensate temperature at about 110F to 120F. Both the VDC reflux and the condensate flows to the reactor have dual purposes. In addition to providing reflux, the VDC stream carries HQMME to the reactor for stabilization of the reactor. The condensate stream provides additional water for dilution of the NaCl formed in the TCE to VDC reaction. If this dilution is not accomplished, NaCl content will build up above its saturation point, deposit out in the reactor and create plugging problems. Salt fed to and formed in the reactor is washed down through the trays and flows out the bottom to the sewer. This aqueous stream also contains a small amount of unreacted NaOH, some dissolved TCE, VDC, and heavies and any HQMME that is refluxed to the reactor. The flow rate of this stream is automatically regulated to give a constant level in the bottom of the reactor. This aqueous stream is above its boiling point when it leaves the reactor; for this reason it goes to a flash pot where the dissolved organics and some water boil off. This flashing is quenched by well water which is sprayed into the top of the flash pot. This well water is the effluent water from a Freon condenser in the MC section. An additional well water line is also provided. SL 010064 CONFIDENTIAL: to protective Subject Order ;t court of 14th judicial Mo. 91'H4j 4-36 The bottoms stream from the VDCM still (to be discussed in detail in the VDCM Section) also is fed to the VDC reactor. This stream enters the reactor at tray 25. It is composed primarily of VDC, but has appreciable dissolved and entrained solids. It also has an appreciable concentration of morpholine. The morpholine and solids are washed out the bottom of the VDC reactor in the aqueous stream. The flow rate of the VDCM still bottoms will vary, but will normally be from 0.5 to 1.5 gallons per minute. VDC Reactor Control: The flow rate of TCE to the VDC reactor is flow con trolled to give the desired VDC production rate. Cell liquor flow rate is flow controlled to give an excess of 10 to 15 grams per liter of NaOH in the VDC reactor bottoms. The condensate flow rate is designed to be about half the TCE feed flow rate--it is currently being controlled at about the same flow rate as the TCE feed. VDC reflux flow is designed to be one-third the TCE flow rate--currently it is about two-thirds of the TCE feed rate. The VDC reactor pressure is controlled by the pressure on the VDC still, since the reactor overhead is fed as a vapor to the still. With a 15 psig top pressure on the still, reactor bottom pressure currently is about 20 psig at 150 TPD, but will increase as production rate goes up. Under this pressure condition, the bottom reactor temperature should run about 240 to 250F. Top temperature should be under 130F to prevent TCE from being carried overhead. Several outside factors influence the internal temperature profile in the reactor. The cell liquor temperature greatly affects the reactor temperature and should be closely maintained at 145F. Introduction of the VDCM still bottoms stream tends to drop the temperature in the upper section of the VDC reactor. CONFIDENTIAL: Subject to Protective Order SL 010065 of 14th Judieiai District Court No. 91-1145 4-37 VDC Still; The overhead from the VDC reactor is fed as vapor to tray 31 of the VDC still. Heat is supplied to this distillation column by live steam injection at the bottom. The VDC is boiled overhead, condensed in the VDC still condenser and collected in the VDC still phase separator. Water is also carried overhead with the VDC, condenses and phases out on top of the more dense VDC in the phase separator. This water phase is periodically drained off. VDC is pumped from the Phase separator to the VDC reactor (this is the source of reflux to the reactor), to the still as reflux and as product forward to the VDC drying section. HQMME is pumped to the phase separator from the HQMME tank. In addition the HQMME recycle stream from the VDC vaporizer (to be discussed in the MC Section writeup) is returned to the phase separator. The VDC still condenser is vented to a vent PCV and then to the outlet line from the vent scrubber. Another PCV on a nitrogen makeup line works in conjunction with the vent PCV to maintain the still top pressure at the desired level. The vent PCV setting is normally set so that the valve is always closed, thus insuring against loss of VDC under normal con ditions. The set point on the N2 makeup PCV is set 2 to 3 psig below the vent PCV to insure against loss of pressure on the system. To prevent unnecessary losses of VDC through the vent system, the VDC still top pres sure alarm is tied to the vent PCV signal so that the alarm sounds when the PCV opens up. The function of the VDC still is to separate the heavier impurities from the VDC. The isomers of VDC, cis and trans, are separated and go out the bottom of the VDC still. Each of these components will run about 0.27o in SL 010066 CONFIDENTIALi Subject to Protective Order of 14th Judicial District Court No. 91-1145 4-38 the still feed. Cis-dichloroethylene is almost completely removed from VDC, while the trans is dropped to 0.04% or less in the VDC product. Trichlor which is formed or fed to the VDC reactor, and which is not reacted to form DCA, also is separated out the bottom of the VDC still. Any unreacted TCE coming overhead from the reactor goes out the bottom of the still. DCA has essentially the same boiling point as VDC and therefore goes overhead with the VDC. MCA has a lower boiling point than VDC, goes overhead in the still and goes into solution in the VDC as it condenses. Most of the toluene (which is introduced via the HQMME system) goes out the bottom of the VDC still. HQMME in the feeds to the still are purged out the bottom. The bottoms stream from the still is primarily water with dissolved TCE, Tri, cis, and trans. Under normal operating conditions there is no separate organic phase. This bottoms stream flows out of the still, through the still bottoms cooler and then is pumped to the acid pit at the Per-Tri plant. The flow rate of bottoms is controlled by a LCV to maintain a con stant level in the bottom of the VDC still. The bottoms stream is carried by stainless steel piping through the cooler, which is stainless steel on the tube side, and through stainless piping up through the LCV. The line from this point to the Per-Tri acid pit is steel. The stream has been found to be corrosive to the steel piping, particularly when not properly cooled. This cooler is normally operated with maximum cooling tower water flow, however, plugging in the cooler can give excessive outlet temperatures, so close attention must be given to the outlet temperature. This temperature should be below 130F. SL 010067 CONFIDENTIAL: subject to fotcctive of Order t 'court 4-39 Dumping of the VDC still can create serious problems in the Per- Tri area. Any flow of organics, particularly VDC, in the bottoms stream should be communicated to the Per-Tri lead operator immediately. I HQMME System: HQMME is purchased as a powder or flake in 100-pound con tainers. This is then dissolved in toluene (TLE) in the HQMME tank to allow pumping it to the VDC system. The tank is equipped with an agitator to aid in dissolving the HQMME. The HQMME-TLE mixture is specified in the MC Plant Standard Operating Procedures Manual. The mixture is pumped through rotometers to the drying still phase separator and to the VDC still phase separator. The HQMME tank is vented through an open line to the sewer. A slight N2 pad is maintained on the tank by a N2 makeup regulator. The HQMME-TLE mixture is maintained at about 165F by steam con densing in the hairpin heating coil in the tank. The steam flow is auto matically controlled to maintain this temperature. All the piping carrying the HQMME-TLE mixture is steam traced and insulated. VDC Still Operating Conditions; The top pressure of the VDC still is normally set at about 15 psig. This has proven adequate to prevent vent ing of VDC on hot summer days. The pressure will go down as ambient tem perature decreases. The N2 make-up valve is normally set to maintain the system pressure no lower than 12 psig. The design reflux flow to the still is 2.2 times the product flow. This flow is most easily estimated by multiplying the TCE feed (which is roughly equal to VDC product flow) by 2.2. Under these conditions, the top temperature is maintained at SL 010068 < confidentialr Subject- tn I rnroctive Order of 14th Judiciaj C: ?;i: circ Court No. 91-1145 4-40 about 125-130F, and with the temperature at tray number 8 at 145-150F. This temperature profile has proven to give the desired product purity with the desired dissolved organics in the bottoms stream. The HQMME flow to the still phase separator should be regulated to give 200-250 ppm HQMME in the reflux flow. VDC Drying System: A. Equipment 1. VDC Drying Still (SAC 67-75). This vessel is constructed of Type 316 stainless steel. It is 1*10" I.D. by 53'6" flange to seam. It is designed for full vacuum to 100 psig at a 300F design temperature. Overpressure protection is provided by a 4" 75 psig graphite rupture disc. The column has four packed sections. Each packed section is supported by a 2-piece Stoneware 316 S.S. support plate. The packing in each section is held down by a 316 S.S. grid-type holddown plate. The feed and reflux is distributed over the top packed section by a 3-piece 316 S.S. Stoneware orifice-type distributor tray. Each packed section has about 15 feet of 1 1/2" chemical porce lain Intalox Saddles (total volume of saddles is 110 cu. ft.). 2. Drying Still Product Pumps (SAC 55-1519, 1520). These pumps are Goulds Model 3196, size 2 x 3 - 10. They are constructed of Type 316 S.S. with a 9 3/4" 316 S.S. semi-open impellor. They are driven by 10 h.p. 1750 rpm motors (SAC 50-2874, 2875). A John Crane Type 9 mechanical seal is used. 3. VDC Drying Still Reflux Pumps (SAC 55-614-622). These pumps are Ingersoll-Rand 3/4" type CORV. They are constructed of Type 316 S.S. with 4 3/4" S.S, open impellor. They are driven by 2 h.p. 3450 rpm motors (SAC 50-1296, 2545). They use John Crane Type 9 seals. 4. VDC Drying Still Phase Separator (SAC 60-571). This vertical tank is 36" I.D, by 7'9" seam to seam. It is constructed with 20% nickel cladding on interior surface. It is rated at full vacuum to 50 psig at 300F design temperature. Overpressure protection is provided by a 3" 50 psig graphite rupture disc. 5. No. 1 VDC Storage Tank (SAC 60-91). This horizontal tank is 4' O.D. by 14' seam to seam. Overpressure protection is provided by a 4" 50 psig graphite rupture disc. Tank capacity is 1335 gallons. The vessel has a 10% nickel cladding. SL 010069 CONF.T PE NT I AL : Subject t.o Protective Order of 14th Judicial District Court No. 91-iJ 45 4-41 6. No. 2 VDC Storage Tank (SAC 60-536). This horizontal tank is 10' O.D. by 29*9" seam to seam. It has 10% nickel cladding on the interior surface. The design pressure is full vacuum to 50 psig at 200F design temperature. The tank has an 8" 50 psig graphite rupture disc. The capacity of the tank is 18,640 gallons. 7. Nos. 1 and 2 Drying Still Reboilers (SAC 71-1219, 1222). These horizontal exchangers are constructed of 316 S.S. on the tubeside with steel shell. Each has 74 - 1" O.D., 12 EWG, 12' long tubes. The shellside design pressure is 120 psig at 650F or full vacuum to 150 psig at 500F. The tubeside design conditions are 150 psig at 200 F. The tubeside is two pass. Each exchanger has 232 sq. ft. of heat transfer area. 8. Drying Still Condenser (SAC 71-649). This horizontal condenser is constructed of all Type 316 S.S. The shellside design pressure is 150 psig at 300F design temperature, while tubeside is rated at 150 psig at 150F. It has 180 - 3/4", 16 BWG, 12' long tubes. The tubeside is four pass. It has 424 sq. ft. of heat transfer area. 9. VDCM Driers - to be described in VDCM Section. B. Operation ' The VDC product stream from the VDC still phase separator is saturated with water. This water must be removed before the VDC can be used in the MC section. Water and VDC form a minimum boiling azeotrope. The azeotrope composition is 99,54% VDC at 129F at 15 psig. This azeotrope is used in the VDC drying still to dry the wet VDC. Feed from the VDC still phase separator is flow controlled at a rate sufficient to maintain the desired level in the phase separator. This flow is a sidestream off the discharge of the VDC still reflux pumps and goes to the top of the VDC drying still. The feed flows onto the distri butor tray above the top packed section. VDC flows down through the packing and to the VDC product pumps. The VDC is pumped from the drying still into the drying still reboiler where SL 010070 CONFIDENT I Alii of Subject 11' 14th Judicial t; wCt i VO M. n!r i c Order t Court No. 9i -1145 4-42 it is partially vaporized by steam condensing in the shell of the reboilers. Each reboiler is sized for full load. The other reboiler serves as a spare. The partially vaporized VDC returns to the drying still below the bottom packed section (yet above the liquid level in the bottom of the still). The vaporized VDC goes up through packing stripping off the water. The VDC and water go overhead from the still, where they are condensed and collected in the drying still phase separator. The water phases out and is periodically drained to the sewer. The condensed VDC is pumped back to the top tray on the drying still as reflux. The flowrate of reflux is automatically controlled to maintain a constant total (water plus VDC) level in the phase separator. Dried VDC product is taken as a side stream off the discharge of the VDC product pumps. The product flow rate is automatically controlled to maintain a constant level in the bottom of the drying still. The product flows directly to either of the two VDC storage tanks. The drying still condenser has a vent system very similar to that of the VDC still. Vent from the condenser goes through a PCV to a vent heater going to the vent line off the vent scrubber. A N2 make-up PCV maintains the pressure at the desired lower limit. In addition, the vent line off the condenser is provided with a continuous nitrogen purge which is metered by a rotometer. An additional point is that the vent PCV and N2 make-up valve fail in the closed position in the event of loss of instrument air. Thus, pres surizing of the drying still by the continuous N2 purge up to N2 line pressure (45 psig) will occur on instrument air failure. CONFIDENTIAL: Subject to erotoctive Order of 14tii Judicial District Court No. 91-1145 SL 010071 4-43 Any monochloroacetylene in the drying still feed goes overhead in the drying still and is partially absorbed in the VDC taken overhead. Not all of the MCA is absorbed, however, and this is an important con tinuous vent off the drying still condenser. The purpose of the continuous nitrogen sweep described above is to carry the vented MCA out of the dry ing still system. Insufficient purging of the MCA could lead to buildup of MCA to dangerous levels. The nitrogen purge must be left on at all times. Currently a minimum flow of 1000 SCFH is being maintained. The drying still top pressure is maintained at 15 psig, with the nitrogen makeup PCV set to open at 12 psig. The steam flow to the reboiler is maintained at a rate to boil overhead enough reflux to keep the reflux pumps near their capacity of 15 to 18 gpm. With this method of steam control, a large increase in feed rate can be easily absorbed without changing steam rate. The VDC product off the bottom of the still will normally be less than 20 ppm H2O. Another operating point that must be considered is the discharge flow rate from the VDC product pumps. As noted above, this stream is divided between the flow to the reboilers and flow to the product LCV to storage. If the pumps are allowed to pump wide open, the discharge pres sure will not be high enough to provide flow through the product LCV, since the path of least resistance is back to the still via the reboiler. In addition, the pressure drop in the suction line increases with flow rate and the available net positive suction head (NPSH.) will become less \ SL 010072 Subject Of 14th Ji c 13 i L) i s t No. 91-1145 4-44 than required suction head (NPSH^), causing the pump to cavitate. For these reasons, the inlet valve to the reboiler is normally throttled to give about 50 to 55 psig discharge pressure on the pumps (with 15 psig top still pressure). This will give a circulation rate through the reboilers of 167 gpm. The flow rate of HQMME to the drying still phase separator is con trolled to give a minimum of 200-250 ppm in the reflux to the drying still. This will give the VDC product an HQMME level in the range of 250-300 ppm due to the additive effect of HQMME in the feed and in the reflux. The VDC drying still can be bypassed (for maintenance or other reason) at production rates of 80 TFD or less. This is accomplished by diverting the product flow from the VDC still phase separator to the VDCM driers. These driers were used to dry VDC in the 75 TPD plant before the advent of the drying still. Three driers are available, each with a dessicant charge of 450 pounds of activated alumina. The effluent mois ture content from the driers is cyclic, but operation by a strict time schedule minimizes this effect. Detailed operating and reactivation procedures are discussed in the VDCM Section. The VDC storage tanks are provided with vent pressure control valves and nitrogen PCV's in the same way as the VDC still and drying still. The VDC product from the bottom of the drying still is at its boiling point. Thus, the storage tank pressures are maintained above 15 psig in order to keep VDC from flashing off in the tanks and being vented. Any vent from is a direct loss to the Company, since this vent goes to the vent line from 4-45 the vent scrubber. The N2 make-up valve opens up at about 12 psig. It is important that this make-up set point be enough lower than the vent PCV set point to keep both valves closed. Leak through of either PCV will result in loss of VDC and excessive usage of nitrogen. Two alarms monitor the vent system of the two VDC storage tanks. The first alarm will alert the operator if either vent valve opens up, thus indicating a lossof VDC to the scrubber vent stack. The second alarm also takes its impulse from the instrument air to the vent PCV but is set at a higher pressure to indicate the valve opening up a lot as in the case of the tank building pressure rapidly. It is important to investigate these alarms quickly as,both storage tanks are tied to the same two alarms--either tank can be building pressure. Off-specification product in VDC storage can be reworked to the VDC still or the VDC still phase separator. If it is out of specification on an organic impurity, the material is pumped to tray 33 on the VDC still. If it is high on moisture, the rework VDC is pumped to the still phase separator, where it can then be fed to the drying still. The rework material is pumped from the storage tanks by the VDC vaporizer feed pumps (to be described later) into a rework header. The piping around the pumps is arranged so that either tank can be reworked with one pump while the other tank is being fed to the VDC vaporizer. SL 010074 SubjPcl CNFlKNTl/it; of h ut^tive Wo/7j tricar Jl'U4 5 1 curfc MC SECTION 4-46 Chemical Reactions: The formation of methyl chloroform (1,1,1-trichloroethane) proceeds by the following exothermic reaction. FeCl3 Cl H Cl - C = C - H + HC1 Cl - C - C - H Cl H Cl H VDC MC The reaction is reversible, that is the MC will decompose to form VDC and HC1, in the unstabilized form in the presence of iron and/or heat. Tri-phenyl phosphite (TPP) is used in the process equipment as a stabilizer to prevent the decomposition of MC. TPP is added to MC wherever the MC is in contact with a heated surface, such as a reboiler. TPP is purchased in 55 gallon drums. This material freezes at 72F and must be kept in a warm place in cool months. Ferric chloride catalyst must be present in order for the MC reaction to proceed. This catalyst comes in-135 pound drums in powdered form. The powder should be silver black and shiny in appearance. Any reddish or brown colored material indicates the catalyst has become damp. Water reacts with the ferric chloride in such a way that the ferric (trivalent) ion is converted to the ferrous (bivalent) ion. The ferrous ion is not effective as a catalytic agent in the MC reaction. The reaction of water and ferric chloride also results in a very tarry substance which present real fouling problems in the piping and equipment. One of the side reactions of TPP is worthy of.special attention. Water will react with TPP to form phenol, the acute toxicity of which is discussed in the Safety Section. The most obvious danger is the toxicity of the phenol which is formed. Another danger is the heat evolved in this reaction, particularly in concentrated form when in a closed vessel. One incident has occurred in the CONFIDENTIALi CONFIDENTIAL* J Protect iO ve Order 1 Court 4-47 plant in which an aqueous solution of sodium carbonate (soda ash) was intro duced into the TPP storage tank. The formation of phenol and the subsequent reaction of phenol and sodium carbonate (a simple acid-base reaction) was violent enough to boil part of the contents out of the tank. Much splashing and spurting of the liquid contents on surrounding equipment occurred. Carry-over of TPP into the MC Reactor will be detrimental to the reaction, possibly killing it if present in sufficient quantities. Any trace quantities of water in the system will react with TPP to form phenol, which also will kill the MC reaction. Additional experience has shown that phenol in the system with ferric chloride will form tars which are very difficult to handle. The presence of either phenol or water in the MC Section must be prohibited. The VDC present in the MC Section must be handled in a manner similar to that in the VDC Section. All vessels containing VDC are kept free of oxygen. All liquid streams are stabilized with HQMME and all sight glasses on equipment with concentrated VDC use amber sight glasses. HQMME is detrimental to the MC reaction, but not to the extent of phenol. The HQMME cannot be fed to the MC Reactor for extended lengths of time, however, so it is removed in the feed system. The VDC is diluted with MC in all downstream equipment. The con centration of VDC in the overhead of the Stripper does become high enough to result in polymerization if unprotected. TPP has proven to serve a dual purpose here in that it serves as a stabilizer for the VDC as well as a heat stabilizer for MC in the top of the stripper. Chlorine breakthrough in the TCE Section will give chlorine in the HC1 fed to the MC Section. This chlorine reacts to give unsym-tetrachloroethane as follows: C1-C=C-H + Cl Cl H Ci l Ci l Cl - C - C - H Cl H VDC Unsym-tetrachloroethane SL 010076 CONFIDENTIAL: Subject to Protective Order 4-48 of 14th Judicial ^ \ r--No. This, heavy will be partially separated in the Flasher and Dopp Kettle; however, this is a two ideal plate separation at best and will not give com plete separation. MC Reactor System: A. Equipment 1. VDC Vaporizer Feed pumps (SAC 55-626,627). These pumps are Ingersoll-Rand 1*' CORV pumps. They are constructed of stainless steel with 4 1/4" closed impellors. They are driven by 3 h.p., 3450 rpm motors (SAC 50-1327, 3004). A John Crane Type 9 mechanical seal is used. 2. VDC Vaporizer Recirculation pump (SAC 55-1500). This pump is a Goulds Model 3196, size 3x4-8. It is constructed of 316 S.S. with a 6 3/4" semi-open impellor. It is driven by a 7 1/2 h.p., 1750 rpm motor. It uses a Chesterton 770 mechanical seal and has a rotometer on the seal flush. 3. MC Reactor Recirculating pumps (SAC 55-1501, 1502, 1503). These pumps are Goulds Model 3196, size 8 x 10 - 13. The pumps are constructed of ductile iron with 11 1/4" 316 S.S. semi-open impellors. Each pump uses a Chesterton 500C mechanical seal. The motors are 40 h.p., 1180 rpm (SAC 50-2856, 2857, 2858). A side stream off Stripper feed is used as seal flush. Also, nitrogen is piped to each seal flush line for purging the pumps while not in service. 4. VDC Vaporizer Rectifying Section (SAC 67-68). This vessel con sists of a tank 3' O.D. by 13'6" flange to flange, mounted in tegrally on top. The construction is 316 S.S. The design pressure is full vacuum to 100 psig at 300F. The bottom tank section is protected from overpressure by 2" Monel 100 psig rupture disc with a 2" x 3" 65 psig SRV mounted over the disc. The 10' packed section (1 1/2" chemical porcelain Intalox saddles) is supported by a Stoneware 316 S.S. metal support plate and is held down by a 316 S.S. heavy duty hold-down plate. A 316 S.S. 'Veir-Riser" distributor is provided at the top of the packed section. 5. MC Reactor (SAC 59-21). This reactor is a vertical tank 9' O.D, by 37' tangent to tangent. It is constructed of steel and has a design pressure of full vacuum to 50 psig at 200F. The suction line to the recirculation pumps comes off 30' above the ^ bottom tangent line. The recirculation stream re-enters the \ MC reactor at the bottom through a 16" line which tees into the 10" ells. The ells are arranged so that the entering liquid has a counterclockwise (looking down) swirling action. The reactor is protected from overpressure by a 10" 50 psig graphite rupture disc. The capacity of the reactor at the 32' level is 15,400 gallons. The feeds are introduced through four spargers which have several 1" holes drilled in bottom side. 4-49 6. VDC Vaporizer Reboiler (SAC 71-1206). This horizontal forced circulation reboiler is constructed of 316 S.S. on the tubeside, with a steel shell. The shell side design pressure is full vacuum to 150 psig at 500F or full vacuum to 120 psig at 650F. Tubeside design pressure is 150 psig at 200F. The exchanger has 146 - 1" O.D. tubes, 12 BWG, 12' long. The tubeside is two pass. The exchanger has a heat transfer area of 459 sq. ft. 7. MC Reactor Coolers (SAC 71-1208, 1209). These horizontal shell and tube exchangers are all steel construction. Both shell and tube sides are designed at 75 psig at 150F. There are 936 - 1" O.D., 12 BWG tubes, 16' long. The tubeside is four pass. Each exchanger has 3929 sq. ft. heat transfer area. 8. MC Vent Condenser (SAC 71-656). This horizontal shell and tube partial condenser is all steel and has 120 - 3/4" O.D., 16 BWG U-tubes, 8' straight length. The shellside design pressure is 300 psig over -20 to 100F range. The tubeside is rated at 150 psig over the -20 to 100F range. The shellside is specially constructed in that it has a 22" O.D, shell around the tubes, but has an additional 20" O.D. shell (actually a liquid-vapor separating and surge area) above the 22" shell. The top shell is connected to the bottom shell by four 6" nozzles. The tubeside is two pass. The heat transfer area is 402 sq. ft. The shellside is protected from overpressure by an SRV set at 225 psig. 9. MC Reactor Catalyst Addition Chamber (SAC 60-1035). This small tank is 1'6" O.D. by 10" seam to seam with a quick opening hatch mounted at the top. The construction is steel. Design pressure is full vacuum to 150 psig at 200F. The quick opening hatch is fitted with a 8 1/2" O.D. by 1/4" Viton O-ring gasket. 10. MC Vapor Separator (SAC 60-1025). This small vertical steel tank is 1'4" O.D. by 3' seam to top flange. The design pressure is full vacuum to 50 psig at 300F. The top of the vapor separator has a 4" thick polypropylene demister. 11. MC Vent Catch Dot (SAC 60-626). This is a salvaged vertical 304 S.S. tank, 2' diameter by 4' tangent to tangent. Original design information is not available, but PPG calculations show it to be good at 50 psig at ambient temperatures. Overpressure protection is provided by a 2" 50 psig graphite rupture disc. 12. VDC Vaporizer Feed Filter (SAC 72-229). This is a Commercial Model WY3055-10-1 1/2F. It is constructed of 316 S.S. and has a design pressure of 150 psig at 200F. The filter uses 6-25 micron fiberglass filter elements. SL 010078 COMFlbF^Tl^*^ QCSer Subiect to rrotfe--- f ar 14th JucHt-UMo. 91 -1145 c Cou rt 4-50 13. VDC Vaporizer Bottoms Filter. This is a Ronningen-Petter Model SS-1118-STD single quick coupling filter with 316 S.S. castings and body. The filter element is a reusable 316 S.S. wire mesh equivalent to a 60 micron filter. Element size is 2" x 18". Inlet and outlet are 1" quick disconnect couplers. This filter is interchangeable with the VDCM still bottoms filter. B. Operation VDC Vaporizer System: The purpose of the VDC vaporizer system is to remove the HQMME from the feed VDC liquid. This is accomplished by vaporizing the VDC off the much less volatile HQMME. The liquid VDC is flow controlled to the bottom section of the VDC vaporizer rectification section. The vaporizer recirculation pump takes the liquid from the bottom section of the vaporizer and circulates it through the vaporizer reboiler tubes. Steam condensing on the shell side vaporizes part of the VDC. The partially vaporized stream is fed back into the rectification section right below the packed section. The unvaporized liquid is recirculated through the pump The vaporized VDC passes up through the packed section and out the top where it goes to the MC reactor. Some of the VDC condenses in the packed section giving internal reflux. The separation action in the packed sec tion assures that no HQMME is carried overhead. The HQMME is purged off the discharge of the pump and goes back to the VDC still phase separator. The steam rate to the VDC vaporizer is automatically controlled to maintain a specified level in the VDC vaporizer. As the level increases, the steam rate increases to boil off more VDC. The purge rate of the HQMME stream off the bottom is manually regulated to maintain about 1000 ppm HQMME in the bottom of the vaporizer. Too high concentration of HQMME can lead to fouling of the vaporizer reboiler. SL 010079 CONFIDENTIAL: Ord@I* ur 4-51 The design recirculation rate for the vaporizer pump is 295 gpm. Operation of the pump with the discharge valve fully open with a clean vaporizer reboiler will result in flows considerably above the design rate. At these high flows, the required net positive suction head (NPSH) becomes greater than the available NPSH. This will cause cavitation of the pump and surging flow. Control of the vaporizer steam is very difficult under these conditions. Throttling the discharge valve to give about 45-50 psig discharge pressure will give approximately the design recirculation rate (based on about 25 psig bottom vaporizer pressure). MC Reactor System: The HC1 off the HCl surge drum is flow controlled into a pipe loop which extends up to the top of the MC reactor. The VDC from the VDC vaporizer is combined with the HCl at the top of the loop. The combined feeds then flow down the back side of the loop and are introduced into the MC reactor via four spargers. The purpose of the pipe loop is to prevent backing up of reactor liquid into the feed lines and systems on shutdown. The reaction to form MC is carried out in the liquid phase in the MC reactor. The VDC and HCl are absorbed in the MC reactor liquor. Any excess HCl passes through the reactor unabsorbed and goes to the vent system. Some VDC and MC will also be carried out with any HCl vented, due to their vapor pressures. The heat of reaction and absorption is removed in the MC reactor coolers. MC reactor liquor is pumped from the 30' level of the reactor by the MC reactor recirculation pumps to the tube side of the MC reactor SL 010080 CONFIDENTIAL: ,,., L prolp.ctjve order Subiec, ^ - , . . cc .court No. 4-52 coolers. The pumps and cooler piping is designed so that normally No. 1 pumps discharges to No. 1 cooler and No. 3 pump discharges to No. 2 cooler. No. 2 pump can be used for either cooler. During periods in which only one cooler is used, any pump can be used for any cooler. The cooled liquid flows from the coolers into the bottom of the MC reactor. The recirculation line in the bottom of the reactor gives the reactor liquor a swirling action to keep the catalyst and tars suspended. Each pump has a capacity of 1930 gpm, thus at full design rate with both coolers the total recirculation rate is 3860 gpm. The cooling is provided by well water on the shell side of the coolers. Catalyst is added batchwise into the system via the catalyst addition chamber. The catalyst is carried into the reactor by a cir culating stream of reactor liquor. The circulating stream comes off the discharge of the reactor pumps and goes back into the piping downstream of the cooler. The piping is arranged so that the catalyst chamber can be lined up from piping to either cooler. The inlet and outlet pipes from the catalyst chamber each have an air operated valve which may be closed from the control room in case of a major leak on the catalyst chamber. These valves can also be operated at the catalyst chamber when adding FeC^. The liquid product stream from the MC reactor to the flasher comes off the discharge of the reactor pumps at the same point as the inlet to the catalyst chamber. The vent stream from the reactor goes into a 6" uninsulated line which goes down to the bottom pipe rack level and then back up to the MC vent condenser. The vent off the flasher condenser (discussed in detail later) also ties into the vent line as it comes down off the MC reactor. The SL 010081 0 O N FID E N TIA fi f S! 11 > '] ' C* ! j'i ' * r ^ V' O 0 IT d O t Of 14th Oud.'.Licii Pi strict Court No. 91 -1i4 5 4-53 reactor temperature normally runs above ambient temperature; therefore, soom cooling and condensing occurs in the vent line- The vent line will fill up and form a positive liquid seal if not drained. This is done by continuously draining the condensed liquid into the MC vent catch pot. The accumulated MC-VDC is periodically pressurized through a 1" line to the flasher accumulator. The vent stream is chilled in the MC vent condenser and then passes to the MC vapor separator. Condensed liquid drops out and flows by gravity back to the flasher accumulator. The HCl goes up through a demister in the vapor separator, through an orifice metering run and out to a pressure control valve, then to the vent header leading to the vent scrubber. The vent stream is cooled in the tube side of the vent condenser by the evaporation of liquid Freon 22 on the shell side of the exchanger. The detailed writeup of the MC refrigeration system is in the Auxiliary Equipment Section. The vent temperature from this condenser will normally be less than 50F. During periods of good MC reactor operation, the vent HCl flow is so small that the flow at the thermocouple on the outlet of the condenser is stagnant, thus giving an erroneously high (greater than 50F) vent temperature. MC Reactor Operating Conditions: The MC reactor level is maintained at 32' by a LCV on the feed flow to the flasher. The MC system pressure (including the flasher and Dopp kettle system) is maintained at 3 psig at the vent condenser. The actual reactor top pressure will be slightly higher due to pressure drop in the line. SL 010082 COMF1 DFKTTAr.: Sub j ect to Protectjvp Order of 14th JudicjaJ Dis'lrict Court No. 91-1145 4-54 The reactor operating temperature is maintained at 95-100F by manually throttling the well water flow to the MC reactor coolers. Higher reactor temperature will result in lower solubility of HCl and VDC and possibly a slower reaction. Also, the MC and VDC vapor pressures will be higher and give a higher condensing load on the vent condenser, as well as more liquid condensation in the vent line itself. Appreciably lower temperatures could also lead to a slower reaction rate. Well water rather than CIW must be used in the reactor coolers because of the high CTW temperature during summer months. The well water flow is throttled on the inlet to the coolers: this is done so that the pressure on the water side is less than the pressure on the process side, in case of a tube leak. The outlet water should be visually checked for organics twice/shift to insure against a loss of MC to the sewer due to a tube leak. The well water out of the MC reactor coolers is reclaimed in the well water recovery tank and is used for cooling tower makeup. See section in Auxiliary Equipment concerning the wellwater recovery system. The reactor operates with unreacted VDC in the reactor liquor. The design VDC content is 3.7%. Experience has shown that a VDC concentration range of 3 to 5% will result in good complete reaction with a minimum of catalyst. Control of the HCl-VDC feed ratios is very important. Currently, the practice is to set the HCl feed rate at a specified flow (this feed rate is determined by the desired MC production rate); then the VDC is adjusted as necessary to stay in the above mentioned VDC concentration range. It should be remembered that the VDC flow rate overhead from the VDC SL 010083 CONFIDENTIAL' Sub j ech to Protective Order Of 14th JudiciaJ District Court No. 91-1145 4-55 vaporizer will be less than the VDC feed rate to the vaporizer by the amount of purge off the bottom of the vaporizer. Catalyst addition to the MC reactor is a very important phase of reactor operation. Insufficient catalyst addition will result in incom plete reaction and subsequent venting of HCl. The addition of too much catalyst presents perhaps as many difficulties as too little catalyst. Some of the pitfalls of too much catalyst includes: (1) the dropping out of excess catalyst in the reactor, coolers, and piping; (2) increasing the solids removal load of the flasher and Dopp kettle; (3) the increased catalyst cost, and (4) the possible ignoring of reactor feed imbalance. The important point to remember is that FeCl3 is sparingly soluble in MC reactor liquor; thus, a requirement for much greater than normal catalyst consumption is an indication of other problems. One possible problem is the killing of the ferric chloride catalyst by water in the system. The feed VDC may be the source of water, but a leak in the stripper reboiler is another possibility. The need for catalyst addition is indicated by the following: 1. An increase in the vent flow flow (which currently runs zero under normal conditions). 2. A decrease in the MC reactor temperature indicating a loss of reaction (which should also result in a vent flow). 3. Necessity for the MC reactor LCV to run in a more closed position than normal (which should again be indicated by 1 and 2). Due to the low solubility of FeCl3 in MC reactor liquor, no more than 20 pounds of catalyst should be added at one time. If more catalyst SL 010084 CONFIDENT] A17' Subject p/'t ; vc Order of 14th Judicjni Dj.'.tj u;t' Court No. 91-1145 4-56 is needed (such as on startup), the frequency can be increased to every 10 to 15 minutes. Normal frequency at 125 TPD is about every two hours, but will probably increase to every hour at full design rate. Liquid VDC can be fed directly to the MC reactor for 6 to 8 hours during periods when the VDC vaporizer system is out of service for maintenance. This liquid feed normally requires a higher catalyst addi tion rate and results in a more tarry flasher and Dopp kettle system. Flasher-Dopp Kettles System: A. Equipment 1. Flasher (SAC 70-67). The flasher is an agitated, scraped wall steam jacketed vessel. It is constructed of carbon steel and is 10' I.D. by 13' on straight side. The shell and jacket have a design pressure of full vacuum to 50 psig at 300F. The approximate liquid volume is 8600 gallons. The shell is protected from overpressure by a 6" 30 psig graphite rupture disc. The jacket is protected by the SRV on the 45 psig steam supply header--set to relieve at 51 psig. The agitator has cross bars which are angled to give a mixing action to the liquid. The crossbars are tied together by a steel bar which is shaped to roughly match the interior contour of the shell. The walls are scraped by scrapers attached to this contour bar. The scrapers are mounted on a simple sleeve bearing surface so that the inertial action of the rotating agitator swings the scrapers out against the wall. The packing uses 5/8" Pure Braided Teflon. 2. Flasher Agitator Drive (SAC 61-143). This is a Patterson V-88W vertical agitator drive with an output speed of 16.6 rpm. It is driven by a 20 h.p., 1150 rpm motor (SAC 50-3113). 3. No. 1 Dopp Kettle (SAC 70-68). This is a small agitated, scraped wall steam jacketed vessel, similar to the flasher. It is constructed of carbon steel, 36" diameter by 36" straight side. The shell is designed for full vacuum to 50 psig at 300F, while the jacket is rated at 25 psig at 300F. The shell is protected from overpressure by a 4" 30 psig graphite rupture disc. The jacket is protected by a 1 1/2" x 3" SRV on the inlet steam line set to relieve at 30 psig. The scraper blade and agitator assembly is similar to the one described in the flasher writeup. The bottom of the kettle is fitted with a Strahman ram type drain valve. The packing uses 1/2" Pure Braided Teflon. CONFIDENTIALt SL 010085 Subject t ) pi otective Order of 14th Jud r i a ! trich Coui fc NO. ;? X o 4-57 4. No. 1 Dopp Kettle Agitator Drive (SAC 61-78). This is a Patterson PF-21 right angle drive unit with an output speed of 37 rpm. It is driven by a 5 h.p., 1750 rpm motor (SAC 50-2883). 5. No. 2 Dopp Kettle (SAC 70-56). This agitated, scraped wall steam jacketed vessel is again similar to the flasher and No. 1 Dopp Kettle. This vessel was the flasher in the 75 TPD plant. It is constructed of carbon steel and is 78" diameter by 87" tangent to tangent. The shell design pressure is full vacuum to 50 psig at 300F. The jacket design pressure is 50 psig with atmospheric pressure in the shell, or 35 psig with full vacuum in the shell. The shell is protected from overpressure by a 4" 30 psig graphite rupture disc. The jacket is protected by the 45 psig steam header SRV, set to relieve at 51 psig. The scraper blade and agitator are similar to the assembly described in the flasher writeup. The bottom nozzle is fitted with a Strahman ram type drain valve. This vessel is not in service. 6. No. 2 Dopp Kettle Agitator Drive (SAC 61-84). This is a Patterson PF-51 right angle drive with an output speed of 20 rpm. It is driven by a 15 h.p., 1150 rpm motor (SAC 50-1560). 7. Flasher Entrainment Separator (SAC 60-1034). This vertical steel tank is 3' O.D, by 6' tangent to top flange. The design pressure is full vacuum to 50 psig at 300F. Overpressure protection is provided by a 6" 50 psig graphite rupture disc. A 4" thick Teflon demister is mounted near the top of the separator. 8. Flasher Condenser (SAC 71-1210). This horizontal all steel exchanger condenser has 415 sq. ft. of heat transfer area. It has 176 - 3/4" O.D., 16 BUG tubes, 12* long. The shellside design pressure is 150 psig at 300F, while the tubeside design pressure is 150 psig at 150F. The tubeside is four pass. 9. Flasher Accumulator (SAC 60-1024). This horizontal steel tank is 6' O.D. by 12' tangent to tangent. The design pressure is full vacuum to 50 psig at 300F. The tank is protected from overpressure by a 6" 50 psig graphite rupture disc. Full tank capacity is 2740 gallons. B. Operation The MC reactor liquid contains primarily MC with 3 to 5% VDC, and has both dissolved and suspended iron and tars. The purpose of the Flasher-Dopp SL 010086 Subject C"NFT>nBWTAt,: Of i4th o j: < Ko. Order ` i. c t- '-ourt 4-58 kettle system is to remove the iron and tars from the liquid stream. The feed rate to the flasher from the MC reactor is automatically controlled so as to maintain a constant level in the reactor. The feed enters the top of the flasher. The organics are boiled overhead by steam condensing in the flasher jacket--the steam Tate is regulated to maintain a constant level in the flasher. The organics flow through the flasher entrainment separator where any entrained liquid or tars are dropped out and returned to the flasher. The vaporized MC-VDC stream goes up through the demister in the separator and then down to the flasher condenser. The MC-VDC stream is condensed out here and flows by gravity into the flasher accumulator. The MC must be stabilized in the flasher to prevent decomposition. This is done by the introduction of a TPP-rich MC stream (Topping Still Bottoms) into the top of the flasher. TPP may also be pumped directly to the. flasher when needed. Ferric chloride and tars are concentrated in the flasher. This concentrated stream is then fed to the MC Dopp kettles (either one or both) by gravity flow. The Dopp kettle boils off more MC and further concentrates the FeCl3 and tars. The vapor goes up through a vertical vapor line, then across to the side of the flasher entrainment separator. The concen trated stream is then periodically dumped from the bottom of the kettle to a waste dumpster box. The MC is heat stabilized by the TPP in the Dopp kettle feed. Any TPP fed to the MC system also goes out in this dump stream due to the high boiling point (680^) of TPP. The steam rate to the Dopp kettle is regulated to maintain a constant steam chest pressure. Feed rate and dumping rate are coordinated to maintain a constant level. SL 010087 CONFIDENTIAL: Subject to protective Order1 of 14th Judicial, District Court No. 91-1145 4-59 The feed line to the Dopp kettle is susceptible to plugging and is steam traced to minimize this. In order to combat a plugged condition, a clean MOVDC stream (stripper feed) and 90 psig nitrogen are piped into the line right below the flasher. These lines are equipped with double block and bleeds and are used to flush out the line when it plugs. A side stream may also be taken off the feed line at the kettle and directed to the dumpster box if extra heavy tars exist in the feed line. The concentrated FeCl3 and tars make instrumentation on the flasher and Dopp kettle somewhat difficult. Special procedures and instrument techniques are employed. In the case of the flasher, the level is sensed by a float chamber type level transmitter. Tars can cause the float to stick, thus indicating a false level. For this reason, the float chamber is pro vided with a clean MC flush stream (stripper feed) which can be directed through the chamber and into the flasher through both the top and bottom nozzles. The float chamber and both nozzles must be flushed each operator round. The flushing can all be accomplished from one position, with the aid of one remote valve operator. Instrumentation on the Dopp kettle is very important and should be thoroughly studied by each operator. The pot temperature of the kettle is measured by a special thermocouple which extends through the steam jacket and contacts the internal scraped wall. This temperature is recorded on a temperature recorder which activates a high temperature alarm when any temperature exceeds 245F. The pressure and level on the Dopp kettle are sensed by pressure switch and differential pressure transmitter which take SL 010088 No. . Cou i-f- 4-60 their impulse off a nitrogen purge stream going into the kettle. See Figure 2 for the schematic. Vapor Figure 2. Dopp Kettle Instrumentation The nitrogen purge rate is set at a specified rate on the purge rotometer. The nitrogen flows down into the Dopp kettle via a 1/2" dip tube which extends down to a few inches above the top agitator crossbar. The pressure of the nitrogen will be very slightly greater than the pressure in the kettle when the end of the dip tube is not submerged. This pressure is indicated in the field by a pressure gauge and is indicated on the control board by a high/normal/low pressure alarm. The pressure alarm is activated by a pressure switch mounted at the kettle. SL 010089 confidentialSubject to Protect.! ve Order of Htli Judicial District Court No. 91-1145 4-61 The pressure in the nitrogen purge line will exceed the pressure in the Dopp kettle when the liquid level increases up over the end of the dip tube. This pressure differential, between the nitrogen purge line and the actual vapor space of the Dopp kettle, is sensed by a differential pressure transmitter. The transmitter gets its high side pressure from the nitrogen line and the low side (Dopp kettle pressure) from an impulse taken off the vapor line of the Dopp kettle. The vapor line pressure should be very slightly lower than the actual kettle pressure if no plugging exists. Thus the differential pressure transmitter senses an increase in level. This output goes to a high/normal/low level alarm on the control board. The end of the dip tube is slashed with the opening pointing away from the direction of agitator rotation. This prevents splashing from causing intermittent activation of the alarm. The vapor line from the Dopp kettle is equipped with a RonningenPetter pressure sensing device. This device consists of a Teflon tube the same diameter as the vapor line. This Teflon tube is fitted into a flanged chamber which is integrally flanged into the vapor line. The chamber consists of another cylinder larger than the Teflon cylinder which creates a void space between the Teflon cylinder and the outer steel cylinder. This space is filled with a thin oil. Any increase of pressure in the vapor line will expand the Teflon diaphragm, thus creating more pressure on the oil. This pressure is indicated by a pressure gauge on the oil chamber. This Ronningen-Petter device is capable of sensing line pressure regardless of plugging or deposits which may form in the line. SL 010090 Subject of 14th d 4-62 Flasher-Dopp Kettle Operating Conditions: The flasher top pressure runs essentially the same as the MG reactor pressure, since the flasher con denser vents into the MC reactor vent line. This pressure normally runs about 3.5 psig and in conjunction with the concentration determines the overhead vapor temperature. This vapor temperature normally runs between 170 and 175F at this pressure. The steam flow to the flasher is manually controlled to maintain the desired level. Automatic control is not used because of cycling which could occur during upsets. Rapid cycles in the steam flow could result in excessive carryover of liquid and possible iron carryover into the flasher accumulator. The pressure on the Dopp kettle is a direct function of pressure drop in the kettle vapor line. This pressure drop is also a direct func tion of the load on the kettle. The load is indicated by the steam flow rate. Experience with No. 1 Dopp kettle indicates that the kettle will operate with about 400 Ibs/hour steam rate, with 11 psig steam chest pressure. This operation will result with a Dopp kettle pressure of 8 to 10 psig, and a pot temperature of 241 to 242F. At the present time, we have no experience with No. 2 kettle. Dopp kettle temperatures are very important indicators of the kettle operation. The 240 to 243F pot temperature has proven to be a good operating temperature, in that higher temperatures can result in excessive concentration of the tars. The dump material produced at 243F is still fluid and easily handled. The Dopp kettle vapor line CONFIDENTIAL: SV. 4-63 temperature is in the range of 175-180F for a kettle pressure of 8 to 10 psig. A gradual decrease of this temperature over several hours time could be an indication of buildup in the vapor line around the thermowell. Plugging in this line can not be tolerated and must be watched closely. The feed line temperature is normally about 175F; again, any fouling in this line is indicated by a gradual drop in the feed line temperature. The feed and vapor line temperature are very quick indications of loss of feed flow to the Dopp kettle. If feed flow is reduced, possibly due to plugging, the vapor and feed line temperatures will both notice ably drop off. This is an area which must constantly be watched. The general philosophy of operating the Dopp kettles centers around two main points. 1. Under no conditions should the Dopp kettle liquid be allowed to concentrate more than normal. If vapor or feed lines plug, the steam flow must immediately be shut off. A remote trip, located behind the control board, is available to close the steam valve in emergencies. 2. The feed rate to the Dopp kettle should be maintained at a maximum at all times. By doing this, tars and FeCl are being removed from the system at the maximum rate at all times. Thus, the flasher liquor is relatively clean and will result in a minimum of fouling in the flasher, Dopp kettle feed line, Dopp kettle and dump line. MC Stripper System:. A. Equipment 1. MC Stripper (SAC 67-19). This steel column is 36" I.D. x 45' seam to seam. The design pressure is full vacuum to 75 psig at 400F. Overpressure protection is provided by a 4" 75 psig graphite rupture disc. Feed is introduced through spargers to trays 23, 28, and 32. The still has 35 trays. These trays were constructed by Glitsch and use the Glitsch-Vl ballast units. The tray floor is steel with type 410 S.S. ballast units. SL 010092 4-64 2. Stripper Condenser (71-1211). The condenser is a vertical exchanger. The tubeside is 316 S.S. and has a design pres sure of 75 psig at 300F. The steel shell has a 75 psig design pressure atl50F. The exchanger has 446 - 1" O.D. , 16 BWG tubes, 6' long. The total heat transfer area is 701 sq. ft. Water flow inlet is at the top on the shell side, with outlet at the bottom through a pipe loop which goes back up to the top of the condenser to insure a liquid full shell. In addition a continuous water purge is taken off a special tube which extends up into the exchanger against the top tube sheet. This purge prevents the formation of a stagnant area. Flow is indicated on a manometer connected to orifice taps in the inlet water line. 3. Stripper Reboiler (SAC 71-1212). This vertical steel thermo syphon reboiler has 187 - 1" O.D., 12 BWG tubes, 12' long. The shellside and tubeside design pressure is 150 psig at 400F. The heat transfer area is 588 sq. ft. 4. Stripper Feed Pumps (SAC 55-764, 769). This is a Goulds Model 3196, size 1x2-8. The construction is ductile iron with a 6 1/2" semi-open 316 S.S. impellor. The pumps are driven by 10 h.p., 3550 rpm motors (SAC 50-1480, 1967). 5. Stripper Feed Driers (SAC 73-107 and 73-108). These steel vessels are PPG fabricated and are constructed of a 12-inch steel pipe with 150 psig blind flanges for heads. They are protected from overpressure by a 2" Teflon-Monel-Teflon 150 psig rupture discs. The 100-pound flake calcium chloride dessicant is supported by an expanded metal basket with two layers of fiberglass wool. A tightly wound roll of fiber glass wool is placed in the top to prevent carryover of flake calcium chloride. 6. Stripper Feed Drier Filter (SAC 72-254). This filter is Filterite Corp. model 18 CMS 3-2. It has 6 - 36" filter elements. The filter is made of carbon steel. 7. CTW Booster Pumps (SAC 55-1504, 1505). These pumps are Goulds Model 3196, size 1 1/2 x 3 - 6. They are constructed of ductile iron with 5" steel impellor. The pumps use packing glands. They are powered by 7 1/2 h.p., 3500 rpm motors (SAC 50-2859, 2860). 8. TPP Pumps (55-811, 812). The positive displacement pumps are Lapp Pulsafeeder Model CPS-1. The reagent head is constructed of 316 S.S, with a Teflon diaphragm. The maximum'design flow is 25,080 cc/hr. A detailed operating principle descrip tion is given in the Auxiliary Equipment section. CONFIDEKTIAL: Subjec! S/. of 14 til , 4-65 9. TPP Tank (60-641). The TPP tank, formerly used in the Pensacola plant, is made of 304 S.S, It is 3'6" O.D. by 8' tangent to tangent. The design pressure is 90 psig at 250F. The tank is vented through a 3" vent line which is always open. A slew N2 sweep keeps out atmospheric air. The tank has four 1/2" sparger pipes which extend down to about 4" off the bottom. The capacity full is 675 gallons. 10. TPP Tank Recirculation Pump (SAC 55-641). This is a steel Ingersoll-Rand 1" type CRVN with a 4 1/2" open impeller. The pump has packing installed in it. This pump is also used to unload TPP drums into the TPP tank. The motor is a 1 h.p., 1750 rpm (SAC 50-1314). B. Operation The liquid stream from the flasher system contains 3 to 5% VDC, the balance being primarily MC. The purpose of the MC stripper system is to separate the VDC from the MC. Feed to the stripper is flow controlled onto the top tray. The feed rate is regulated to maintain the desired level in the flasher accumu lator. MC flows down through the stripper to the stripper reboiler. The reboiler vaporizes part of the MC which then flows back up the column, stripping VDC out of solution on the way. The steam flow to the reboiler is automatically controlled to maintain a specified temperature in the stripper. The MC-VDC vapor stream pass up through the tubeside of the verti cal stripper condenser, where part of the stream is condensed and falls back into the stripper to act as reflux. The uncondensed stream, rich in VDC, is returned to the MC reactor via a pressure control valve which main tains a specified pressure on the stripper. This recycle stream enters the MC reactor at the 6-foot level. The MC must be heat stabilized in the stripper reboiler and the VDC rich liquid at the top of the stripper must be inhibited against polymer formation. TPP is added at the top tray of the stripper to accomplish both SL 010094 CONFIDENTIAL: Subject to Protective Order of 14th Judicial Di.Dcrict Court No. S-1-114 5 4-66 of these purposes. This TPP flows down through the stripper. The MC-TPP stream flows off the bottom at a rate automatically controlled to main tain a set-point level in stripper pot. The MC stripper system is all steel with the exception of the stripper condenser which is type 316 Stainless Steel. All the streams contain HCl (due to HCl dissolved in the feed) and therefore are corrosive if water is present. The feed to the stripper is continuously dried by the stripper feed drier to insure against the possibility of water buildup. The stripper condenser is located at the top of the stripper, and normal CTW pressure will not boost the CTW high high. CTW booster pumps are provided to raise the CTW pressure sufficiently to get up to the top of the stripper. The flow of CTW is controlled by a control valve on the inlet water to the condenser to maintain a specified temperature in the top of the stripper. The throttling is down on the inlet to the condenser so that the CTW pressure in the shell of the condenser is essentially atmospheric, or, more important, is less than the process side pressure. Thus, any tube leaks will result in flow from the process to the water side. Stripper Operating Conditions: The stripper is operated in such a manner to keep the VDC content in the bottoms stream less than 0.05%. Normally, this content is 0.01% or less. The TPP addition rate is regulated to main tain 0.15 to 0.25% TPP in the stripper bottoms. Operation of the MC Section with inadequate TPP will result in cracking of MC-^-this normally occurs first in the flasher and Dopp kettle system and is indicated by an excess vent flow through the vent line to the scrubber. SL 010095 CONFIDENTIAL: Subject to Protective ordfer of 14th Judicial i.'.i: r......... No. 91-1145 4-67 The pressure on the stripper is maintained at 20 psig by the PCV. Operation at this pressure with No. 29 tray temperature at 215F will give good control and no appreciable VDC in the stripper bottoms. The bottom temperature will be about 230F at this pressure. The CTW flow to the stripper condenser is regulated with a remote operated control valve to maintain 180 to 185F in the top of the stripper. Operation of the stripper at high temperatures will give excessive recycling of MC back to the MC reactor. This loads up the flasher and stripper systems unnecessarily. The stripper can be operated with no CTW flow to the condenser. With this type of operation, a great deal of MC is recycled and condensed in the MC reactor. Operation for short periods of time without CTW flow may be brought about by a leak in the stripper condenser tubes. The stripper pressure is raised to 30 psig under these conditions and the con trol temperature becomes 228F on tray 34. Topping Still System: A. Equipment 1. Topping Still (SAC 67-70). This steel column is 42" l.D. by 20' tangent to tangent. The design pressure is full vacuum to 50 psig at 300F, Overpressure protection is pro vided by a 4" 50 psig graphite rupture disc. The still has eight trays. Feed is introduced on No. 2. The still has GlitschV-4 ballast trays with steel floors and type 410 S.S. ballast units. 2. Topping Still Condenser (SAC 71-1214). This horizontal con denser is all steel. It has a shellside design pressure of 150 psig at 300F and a tubeside design of 150 psig at 150F. The exchanger has 176 - 3/4", 16 EWG tubes, 12' long. The tubeside is four pass. The heat transfer area is 415 sq. ft. SL 010096 Subject to Provo:;-: of 14th .hit < ci<-. 1 b'- ` 1 tu>. bi-i l1'0 order , '.'.v.rr t 4-68 3. Topping Still Reboiler (SAC 71-1213). This vertical steel thermosyphon reboiler has 235 - 1" O.D., 12 BWG tubes, 12' long. Both shell and tube sides are designed for 150 psig at 400F. The heat transfer area is 738 sq. ft. 4. Topping Still Accumulator (60-1026). This is a vertical steel tank, 3' O.D. by 8* tangent to tangent. The design pressure is full vacuum to 50 psig at 300F. Protection from overpressure is provided by a 3" 50 psig graphite rup ture disc. Full tank capacity is 420 gallons. 5. Neutralizer Feed Pumps (SAC 55-1398, 1509). These pumps are Goulds Model 3196, size 1 1/2 by 3 - 10. They are constructed of ductile iron with 9 1/4" semi-open impellors. They are driven by 7 1/2 h.p., 1750 rpm motors (SAC 50-2864, 2604). 6. Neutralizer Feed Cooler (SAC 71-1215). This horizontal all steel exchanger has 64 - 3/4", 16 BWG tubes, 12' long. The shellside design pressure is 150 psig at 300F, while the tubeside is designed for 150 psig at 150F. The tubeside is four pass. The cooler has 161 sq. ft. of heat transfer area. 7. Topping Still Bottoms Pumps (SAC 55-766, 767). These positive displacement pumps are Lapp Pulsafeeder Model CPS-2. The head is made of 316 S.S. with Teflon diaphragm. A detailed operating principle -description is given in the Auxiliary Equipment Section. B. Operation The function of the Topping Still is to remove the heat stabilizer, TPP, from the MC. The stripper bottoms stream is level controlled into the topping still at tray 2. MC is vaporized in the reboiler and passes up through the column and out to the topp still condenser. The condensed MC flows by gravity into the topping still accumulator. Some of this condensed MC is pumped to the still as reflux. The balance is pumped forward to the neutralizer at a rate automatically regulated to maintain the set point level in the accumulator. SL 010097 CONFIDENTIAL Subject to Protectj- vc Order of 14th Judicial D)st rict Court No. 9l~H4 5 4-69 The TPP rich stream is pumped from the bottom of the still by the topping still bottoms pumps. The flowrate is controlled so as to give about 1 to 27 TP? in the bottoms stream. The flowrate is controlled by adjusting the stroke length on the positive displacement pumps. Steam flow to the topping still reboiler is automatically regulated to maintain a set point level in the still bottom. Reflux to the still is regulated to give a reflux flow to product flow ratio of 0.5:1. This reflux ratio can be raised during upsets when heavy impurities, such as TCE, are present. Higher reflux rates will give better separation of MC from the heavies in the topping still. This is temporary, however, since the bottoms are recycled back to the flasher, a single separation stage. Continued high heavy impurity introduction into the MC section will eventually result in buildup of heavies in the MC system and high heavies content in the topping still product. The topping still condenser is not normally vented, since almost all of the inerts are stripped out in the stripper. An air pad pressure control valve is available to maintain a positive pressure on the column. The top pressure normally runs about 0.5 psig. A bleed valve is available to purge inerts on startup. The pot temperature on the topping still is about 170F at normal operating pressure. A specific temperature profile is not maintained because experience has shown that a reflux ratio of 0.5 will result in no TPP in the topping still product. SL 010098 JV Order Court 4-70 Neutralizer - MC Drier System: A. Equipment 1. MC Neutralizer (SAC 67-72). This vertical 10% nickel clad vessel consists of a bottom tank section 4'5 1/2" I.D. by 4' 10 1/2" seam to seam, topped by a packed column 3'6" l.D. by 10' tangent to top flange. The design pressure is full vacuum to 50 psig at 400F. The top flange has a 3" open vent nozzle. The 1 1/2" Intalox chemical porcelain packing is supported by a Stoneware chemical porcelain "Multi-Beam" support plant. The top is provided with a liquid-liquid distributor tray made of 304 S.S. by Stoneware. 2. Homogenizer Pump (SAC 55-1449). This is a Durcon 6 Mark II, size 1 1/2 x 1 1/2 p-74 with 7 1/2" impellor. The pump is fitted with a 1 7/8" John Crane Type 20 mechanical seal. The pump is driven by a 3 hp, 1750 rpm motor (SAC 50-1694). 3. Ash Liquor Pump (SAC 55-1034). This is a 1 1/2 x 2 9 1/2 type HHD1R090 pump with a 7" open impeller. The pump uses Garphite 100 packing. It is powered by an 1150 rpm 1 h.p. motor (SAC 50-1222). 4. MC Product Pumps (SAC 55-802, 803). These pumps are Goulds Model 3196, size 1x2-8 with 8" impellors. They are con structed of type 316 S.S., and use John Crane type 9 mechani cal seals. 5. Ash Liquor Tank (SAC 60-1027). This vertical steel tank is 5* O.D. by 4*6" top to bottom. It has an atmospheric design pressure at 200F. Part of the top is hinged for easy addi tion of soda ash. 6. MC Product Driers (SAC 73-95, 95). These vertical driers are constructed of 304 S.S., and measure 2*6" O.D. by 8' flange to flange. The design pressure is full vacuum to 150 psig at 400 F. Overpressure protection for each drier is provided by a 1" x 1 1/2" SRV set to relieve at 150 psig. The dessicant charge is supported by a Neva-Clog screen at the bottom. The charge consists of 30 cu. ft. of Dowex 50 SX-8 dessicant resin per drier. Carryover of dessicant from the drier is prevented by a cone-screen arrangement over the top (outlet) nozzle. The cone-screen assembly consists of two perforated nickel cones with a fine screen sandwiched between the cones. Each drier is jacketed with a Dean Panelcoil 401 Type SP-20 heat transfer panel. The SRV nozzle is located inside the cone to prevent plugging by the dessicant. SL 010099 COMF1 D FNT r m , of .f1 ucirj {tDliis-criie0t rder No. 91-ii4S Court 4-71 7. MC Carbon Bed (SAC 72-231), This vertical steel vessel is 2'6" O.D. by 8' flange to flange. The design pressure is full vacuum to 150 psig at 300 F. The vessel is protected by a 1" x 1 1/2" SRV set to relieve at 150 psig. The bed of acti vated carbon is supported by a Neva-Clog screen. About 30 cu. ft. of activated carbon are required in the vessel. 8. MC Carbon Bed Filter (SAC 72-262). This is a Commercial Fulflo filter, Model WY 3 TS-10-21. It is made of cast iron and steel. It uses 6 10" 25 micron fiberglass filter elements. Overpressure protection is provided for by a 1" x 1 1/2" SRV, set at 150 psig, mounted on the outlet liquid line. 9. Nitrogen Heater (SAC 71-1216). This exchanger is all steel with 20 - 3/4", 16 BWG, U-tubes, 12' nominal length. The shellside design pressure is 150 psig at 400F with tubeside design at 150 psig at 400F or 120 psig at 650F. The tubeside is 2 pass. The exchanger has 92 sq. ft. of heat transfer area. 10. MC Rework Pump (SAC 55-613). This is an Ingersoll-Rand 1" CRVN steel pump. It uses a John Crane Type 9 mechanical seal. The impeller diameter is 5". The pump is driven by a 3 h.p., 3500 rpm motor (SAC 50-1283). B. Operation Topping still product contains trace quantities of HC1 which lower the pH of the stream to 3,0 to 4.0. This acidity is neutralized by reaction with an aqueous solution (ash liquor) of soda ash (sodium carbonate) in the MC neutralizer system. The topping still product is level controlled from the accumulator to the suction of the homogenizer pump. Ash liquor is also pumped from the ash liquor tank by the ash liquor pump to the suction of the homogenizer pump. The sodium carbonate strength is maintained at 35-45 gpl Na2CC>3. These two streams are thoroughly mixed as they pass through the homogenizer pump. The pump discharges into the top of the neutralizer where the more dense MC phase settles to the bottom. The MC and soda ash solution are further contacted in the packing of the neutralizer. The SL 010100 EubjectC0NP^.. Of I4til J~ ll.T.+- Cl r.J. .....f.- 1 ' J U A V4i.? tio, - j j Order - Court 4-72 aqueous ash liquor solution phases off the top of the neutralizer and overflows back to the ash liquor tank where it is again recirculated to the homogenizer pump. The neutralizer is acting primarily as a phase separator. To keep the soda ash solution inside the neutralizer changed out (being the lighter phase it overflows from the top of the neutralizer) a continuous draw off from the MC soda ash interface area is taken back to the ash liquor tank. Otherwise the soda ash would be stagnant and eventually have a detrimental effect on the MC product pH. The MC phase off the bottom of the neutralizer should be nearly neutral and will be saturated with water (200-300 ppm). This MC stream is pumped to the MC driers. The flowrate to the driers is regulated by a LCV to maintain a constant MC level in the neutralizer. The level of the MC is sensed by an interface level transmitter (float chamber). The wet MC phase is pumped into the bottom of the MC driers, flows up through the driers, and on to the MC carbon bed. The effluent water content is normally less than 40 ppm. This dried MC then flows from top to bottom in the MC carbon bed, then through the carbon bed filter to catch any carryover activated carbon. This MC product then goes to storage. The MC carbon bed will absorb any traces of acidity or heavy trace impurities which may be present in the MC product. Note: On initial startup of any activated carbon bed, the bed should be very slowly filled so as to minimize heat buildup. This heat buildup could result in cracking of MC or even a fire if not carefully controlled. SL 010101 Of Sub 3ect t:fo;/i tic l* t? f) i-ist '--l '* J> ^L 4-73 The MC driers are set up on a fixed cycle. The desiccant must be properly reactivated in order to achieve satisfactory drying performance. The following cycle is used: 1. Change driers at 8 p.m. each evening. The MC in the drier being taken out of service is transferred over to the new drier by padding the used drier with air until all the MC is out. The flow in the new drier should be from bottom to top. 2. Put the used drier on hot nitrogen reactivation at the time of drier switching. The hot nitrogen comes from the nitrogen heater in which 90 psig nitrogen is heated to about 305F by 125 psig steam condensing in the shell. The design nitrogen flow rate is 8000 SCFH. The outlet nitrogen flow should be throttled to hold about 20 psig on the drier. This gives good distribution and heat transfer. The steam heating panels around the drier must be put in service when the hot nitrogen flow is started. 3. At 9 a.m. the following morning, open the outlet valve and release the pressure on the drier. This will lower the water boiling point and give assurance of the final traces of water being removed. Adjust the nitrogen flow at the desired rate. 4. At 4 p.m., stop hot N2 flow, cut off the steam heating panels and start cooling the drier with air. 5. When the drier is cool (about 8 p.m.), switch driers as described in Step 1. The temperature should be less than 100F before switching. The minimum temperature required for good reactivation of the Dowex resin is 225F. Normally, the outlet nitrogen temperature will be around 250F. The pressure drop across the MC driers should noted each operator round. Plugging occasionally occurs in the driers. An early indication of plugging is given by an increase in the pressure drop across the drier. Experience at 125 TPD indicates a normal pressure drop of 3 psig. When plugging does occur in the MC driers, the restriction can be removed by SL 010102 CONFIDENTIAL: Subject to Pro:e:: c i v? Order Of 14th Judicial DisorrcL Court No. 91-1145 4-74 backflushing. The restriction may be caused by fines plugging the openings ' in the bottom or top screens. Backflashing is accomplished by pressurizing the drier contents backwards out the inlet line (the MC product pump should be shut down and the bypass opened around the LCV). Under no circumstances should backflashing be done by changing the flow so that the inlet wet MC goes to the top of the driers. This will wet the resin on the outlet of the drier and give wet MC product when the flow is returned to the normal direction. The effectiveness of the neutralizer system has proven to be important in the M3 drier operation. If neutralization is good (e.g., above 6.4 pH on neutralizer bottoms), MC drier feed moisture will be in the range of 200-300 ppm. If neutralization is incomplete, the MC dryer feed moisture will be up to 700 ppm. This results in low product pH and also greatly shortens the life of the MC driers. Drier plugging often results also thus thorough mixing is required to give the desired results. "Good mixing" (and thus good neutralization) can be observed when a sample taken from the MC homogenizer pump discharge phases out slowly with the MC being in tiny droplets. The MC phase is then very clear. "Poor mixing" is when the MC phases out in large droplets and appears cloudy. Ways to improve mixing include throttling the homogenizer pump discharge valve to present cavitation, increase of ash liquor flow or a fresh charge of Soda Ash in the ash liquor tank. MC Rework System: During startups or upset conditions, off-specification MC is sometimes made. A rework pump and piping are available for the rework SL 010103 C0NFIM";TTAL: Subject to Protective Order of 14th Judicial 10 nlnct Court No. 91-1145 4-75 of the MC back into the system. The rework pump can take suction from any one of the stabilizing tanks and day tanks. The rework line is connected to the following points in the MC Section: 1. The recirculation line going to the MC reactor. 2. The flasher feed line. 3. The suction and discharge of the stripper feed pumps. 4. The feed line to the topping still. 5. The feed line to the homogenizer pump or neutralizer. The rework line tie-in to the homogenizer pump or neutralizer has a double block and bleed which must be used (bleed open) when not in service. If not used, water from the neutralizer system could back flow into the rework line and subsequently be pumped into the MC Section. Another line is also available which puts topping still product into the rework line. The rework pump can be blocked off, and the MC Section can be put on total internal recycle (no feeds to the reactor) with the stills in service. This is accomplished by putting topping still pro duct back to the rework line and opening up the rework line to either the MC reactor or flasher feed. In this way, a reactor outage can be taken without shutting down other equipment. The MC section can also be put on recycle by putting the MC product forward to a tank as usual, then rework ing from the tank back to the reactor or flasher. The moisture content of the tank material must be dry and be carefully monitored. In addition, no stabilizers can be allowed back into the MC Section. Stabilizers may be capable of undesirable reactions in the system. SL 010104 CONFIDENTIAL: Subject to I ' r'n. n^rlnr of 1 iti: Judjoi.-i TRI-ETHANE STABILIZATION AND STORAGE SECTION 4-76 A. Equipment 1. No. 1 Stabilizer (DOL-IBL and BLM) pump (SAC 55-646). This is an Ingersoll-Rand 1" CRVN steel pump with a 5 1/4" closed impeller. The pump uses a John Crane Type 9 mechanical seal and is driven by a 3 hp 3500 rpm motor (SAC 50-1319). 2. No. 2 Stabilizer (BTE and TLE) Pump (SAC 55-617). This steel Ingersoll-Rand 1" CRVN pump has a 5 1/2" closed impeller. It uses a John Crane Type 9 seal and is driven by a 2 hp 3500 rpm motor (SAC 50-1290). 3. NRE Pump (SAC 55-618). This steel Ingersoll-Rand 1" CRVN pump has a 4" closed impeller. The pump is driven by a 2 hp 3500 rpm motor (SAC 50-1291). It uses a John Crane Type 9 mechanical seal. 4. NRE/D0X Addition Pump (SAC 55-1841). This is a Goulds Model 3196, lx 2-10 pump with an 8 1/4" impeller. Its design capacity is 50 gpm. It is powered by a 5 hp 1800 rpm motor (SAC 50-3443). This pump is equipped with a John Crane Type 9 mechanical seal. 5. Specialty Stabilizer. Pump (SAC 55-636). This is also an Ingersoll-Rane 1" CRVN pump and has a 3 1/2" closed impeller. The pump is driven by a 1 hp 1750 rpm motor (SAC 50-2596). It has a John Crane type 9 mechanical seal. 6. Stabilizer Unloading Pump (SAC 55-1576). This pump is a Goulds Model 3196, size 1x2-8. It is made of ductile iron and has a 7 5/8" semi-open impeller. It is driven by a 5 hp, 1750 rpm motor (SAC 50-2958). 7. NRE/DOX Unloading Pump (SAC 55-1843). This is a Goulds model 3196, 1 1/2 x 3 - 8 pump with a 7 3/4" impeller. Its design capacity is 70 gpm. It is powered by a 5 hp 1800 rpm motor (SAC 50-3441). The pump is equipped with a John Crane Type 9 mechanical seal. 8. 324 Pump (SAC 55-550). This is a Durco Series DCI-HDI-090. It is steel and has a 9" impeller. The pump has a John Crane Type 9 seal and is driven by a 10 hp 1750 rpm motor (SAC 50-1195). 9. 321 Pump (SAC 55-637). The pump is an Ingersoll-Rand 1" CRVNL, steel. It has a 6" closed impeller. The pump has a John Crane Type 9 seal and is driven by a 7 1/2 hp 3500 rpm motor (SAC 50-1310). SL 010105 CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 4-77 10. Shipping Tank Pump (SAC 55-1510). This is a Goulds Model 3196, size 1 1/2 x 3 -6. It is made of ductile iron and has a John Crane Type 9 seal and is driven by a 7 1/2 hp, 3500 rpm motor (SAC 50-2865). 11. Tri-Ethane Barge Loading Pump (SAC 55-650). This is an Ingersoll Rand 4" CRVL steel pump with a 9" impeller. It is driven by a 25 hp 1750 rpm motor (SAC 50-1323). It uses a John Crane Type 9 seal. 12. Nos. 1 and 2 Stabilizing Tanks and Nos. 1-3 Day Tanks (SAC 60-396 through 400). These steel vertical tanks are 120" O.D. by 12' tangent to tangent. The design pres sure is 40 psig at 300F. Each tank is vented and is pro tected from overpressure by a 8" BS & B tank vent. The full capacity of each tank is 6500 gallons. 13. Nos. 5 and 6 Stabilizing Tanks and Nos. 8 and 9 Day Tanks (SAC 60-1028, 1029, 1031, and 1168). The vertical steel tanks are 18' O.D. by 22' high. The design pressure is 3 ounces external, 1.4 psig internal at ambient temperatures. The full capacity of each is 41,500 gallons. Each tank is vented by a 8" BS & B tank vent. 14. No. 7 Stabilizing Tank (SAC 60-1030). This is the old Day Tank No. 6 which has been converted into the 339 stabilizer tank. It is a vertical steel tank 18' O.D. by 22' high. The design pressure is 3 ounces external, 1.4 psig internal at ambient temperatures. The full capacity is 41,500 gallons. It is vented by a 8" BS & B tank vent. Instead of an agitator, this tank is mixed by an eductor mixer. The mixer is a 10 1/2" diameter pipe approximately 20 feet high. Liquid is drawn through holes spaced along the pipe and ejected at the bottom. The tank is mixed in approximately 30 minutes. 15. 339 Stabilizer Tank Transfer Pump (SAC 55-1842). This is a Goulds Type 3196, 1 1/2 x 3 - 13 pump with a 10 1/2" impeller. Its capacity is 150 gpm. It is powered by a 15 hp 1800 rpm motor (SAC 50-3442). This pump is used to mix the material in No. 7 stabilizing tank as well as transfer 339 to Shipping through the 3" 321 transfer line to Shipping. SL 010106 CONFIDENTIAL: '*" ive Order* strict Court 4-78 17. No. 2 ELM Tank (SAC 60-403). The tank is vertical, steel and is 96" O.D. by 10' tangent to tangent. The design pressure is 50 psig at 300F. The tank is vented by a 6" BS & B tank vent. The full capacity is 4422 gallons. 18. No. 1 TIE Tank (SAC 60-406). This vertical steel tank is 120" O.D. by 10" high. The design pressure is 6 ounces internal by 3 ounces at 100F. The tank is vented by 12" BS and B tank vent. The full capacity is 5816 gallons. 19. No. 2 TLE Tank (SAC 60-408). Description is same as for No. 1 TLE. .20 DQL-IBL Tank (SAC 60-1032). This vertical steel tank is 121 O.D. by 18' high. The design pressure is 3 ounces external and 1.84 psig internal at ambient temperature. The full capacity is 15,000 gallons. The tank is vented by a 16" BS & B tank vent. .21 BTE Tank (SAC 60-401). This is a steel vertical tank 120" O.D. bg 12' tangent to tangent. The design pressure is 40 psig at 300 F. This is the old Day tank No. 4. It is protected from overpressure by a 8" BS & B tank vent. The full capacity of the tank is 6,500 gallons. .22 Bulk DOX Storage Tank (SAC 60-541). This is a vertical steel tank 14r O.D. by 14'. tangent to tangent. The design pres sure is 40 psig internal pressure and 4 psig vacuum at 300F. It is protected by an 8" 25 psig carbon rupture disc. The tank is equipped with a 316 S.S. 1 1/2" Penberthy eductor mixer an the bottom head for mixing the DOX and MC. Complete turnover of tank material is 88 minutes using the NRE/DOX addition pump (50 gpm). The full capacity of the tank is 17,600 gallons. This tank is the old Day tank No. 6. 23. Bulk NEE Storage Tank (SAC 60-542). This tank is the same as the Bulk DOX tank except that it does not have an eductor mixer in it. This tank is the old Day tank No. 7. 24. Tri-Ethane Shipping Tank (SAC 60-1033). The tank is vertical, steel and 12r Q.D. by 30' high. The design pressure is 3 ounces external and 1.84 psig internal at ambient tempera ture. A 8" BS & B vent lid is used. Full capacity is 25,000 gallons. 25. No. 1 Tri-Ethane Dock Storage Tank (SAC 60-530). This steel tank is 48r diameter by 32* high (straight side). The design pressure is 3 ounces external and 3 ounces internal at ambient tenperature. A 16" BS & B tank vent is used. The full capacity is 430,000 gallons. rr;'r;T Sub iect to f I4t'h Jl'.Ji No ' ?r,der Lot. Court r 4-79 26. No. 2 Tri-Ethane Dock Storage Tank (SAC 60-413). This verti cal steel tank is 42' diameter by 32' high, straight side. The design pressure is 3 ounces, both internal and external, at ambient temperature. A 16" BS & B tank vent is used. The full capacity is 330,000 gallons. 27. Tri-Ethane Transfer Filter (SAC 72-59). This is a steel Com mercial Fulflo Model WB18D-10-3F. The design pressure is 150 psig at ambient temperature. The filter uses 36-25 micron fiberglass filter elements. 28. Specialty Carbon Bed Filter (SAC 72-103). This is a Filterite Model 18 MC 35-2, and is made of stainless steel. It uses 625 micron fiberglass filter elements. 29. Specialty Drier Filter (SAC 72- ). Same as 25. 30. 324 Decolorizer (SAC 73-24). This vertical steel vessel is 24" diameter by 8' 8 3/4" seam to top flange. The design pres sure is 150 psig at 300F. A 15 cubic feet charge of activated carbon (12 x 40 mesh) is supported by a Neva-Clog screen. Carry over of carbon is prohibited by a tightly wound roll of fiber glass wool in the top. The Decolorizer is protected by a 1" 125 psig Monel rupture disc. 31. Specialty Carbon Bed (SAC 73- ). 32. Rework Drier (SAC 73-41). This vertical vessel is 18" O.D. by 7' flange to flange and is made of stainless steel. The design pressure is full vacuum to 150 psig at 100F. The dessicant charge is supported by a fine wire mesh screen. The dessicant charge consists of 9 cu, ft. of Dowex 50 WX-8 resin. The drier is protected by a 1" 150 psig Monel rupture disc. 33. Specialty Drier (SAC 73- ). B. Operation The MC Product goes to the Stabilizing Tanks for blending in of stabilizers. The basic unstabilized MC is known as Type 321. The normal stabilized blend is Type 324. This material is normally blended and sampled in the Stabilizing tanks, moved to the Day tanks until cleared by analysis from the laboratory and then moved to the Tri-Ethane Shipping tank or the sv- 4-80 Dock Storage Tanks. Specialty blends are made from Type 321 in the Stabilizing tanks and are loaded directly into tank cars, trucks, or drums from these. The daily MC production is metered by the increase in tank level in the Stabilizing tank. The tank level must be gauged (by dropping a plumb bob with a measuring tape through the tank vent lid) each time production is switched into or out of the tank. The production line header is located on top of the tanks and MC enters each tank through a standleg going to the bottom of the tank. The tanks are tied together on the bottom by a common header (stabilizer tank suction header) which goes to the 324 or 321 pumps. The valves leading to this header from each tank must be closed except when transferring a tank. Type 324 Stabilization System: Type 324 Tri-Ethane^ consists of the following stabilizers along with percentages: DOL BLM BTE TLE IBL NRE ADH 0.9-1.3% 0.3-0.4% 0.7-0.9% 0.6-0.9% 0.7-0.91 1.9-2.3% 50 ppm Amounts of stabilizers for the various grades of methyl chloroform are specified in the tank transfer book as the orders are received. Each of the stabilizers is metered or measured as it is put into the Stabilizing tank. All of the stabilizers except ADH, BTE, and TLE are pumped through individual lines to a manifold at the top of the No. 1 Stabilizing tank. The stabilizers go through a single line to Stabilizing SL 010109 Subject Of 14th J cf.ive Order istrict t'^yrfe 4-81 tanks Nos. 3, 4, 5, and 6. BTE and TLE are pumped through a single line from the pump to Nos. 3, 4, 5, and 6 Stabilizing tanks. DOL-IBL (purchased as a 60-40 mixture) is pumped to the manifold by No. 1 Stabilizer pump through a Smith positive displacement meter. The desired number of gallons is set on the counter before starting the pump and the meter automatically shuts off flow when the counter reaches zero. BLM is also pumped by this pump and meter. BTE and TLE are pumped by No. 2 Stabilizer pump through another automatic shut-off Smith meter. NEE is pumped from the bulk NRE storage tank by the NRE/DOX addition pump through another Smith meter. NEE can also be pumped from drums. ADH is added directly to the tank from a measuring can via a pot which is pressurized to push the ADH into the tank. Note: Always turn off the agitators when the tank is thoroughly mixed. Operation of the agitator while the tank is being pumped down can result in serious damage to the equipment. All of the stabilizer lines should be blown clear of stabilizers and left under nitrogen pad when not in service. Nitrogen lines to each of the stabilizer lines are provided for this purpose. Each of the lines should be blown out and blocked at the manifold before blowing out another line. If each line is not blocked at the manifold as it is purged, the blowing of another line may back stabilizers into the first line. The stabilized 324 is agitated for about two hours, sampled, and then pumped by the 324 pump to the Transfer Filter and then into the Day tank via the Day tank inlet heater which goes to the bottom of each Day SL 010110 S,ub , 3ect CtOoNFlppm'1AL; of 14 Judicial^ t:] '/r- Order Ho. 9 1-; . 1 ' c!- Court -- *4 J 4-82 tank. The cleared 324 is pumped from the Day tanks through the Day tank suction header to the Shipping or Dock tanks by the 324 pump. A 3" line off the discharge of the 324 pump goes to these tanks. Type 339 is the second largest amount of Methylchloroform that is produced. Since it is a specialty grade, cross-contamination should be avoided. To do this and to have material available on a regular basis for shipments, the old Day tank No. 8 was converted to a 339 tank (S-7). Production can be routed to this tank and stabilizers can be added once the tank is filled with unstabilized methyl chloroform. There is a separate line for the DOX and NRE to be added from the bulk stabilizer storage facilities. The BLM is added from the 324 BLM' addition system. The 339 is then mixed with an eductor mixer and transferred directly to Shipping through the 3" 321 line. Piping around S-7 is separate from the 324 system in order to prevent cross-contamination. Occasionally, stabilized 324 product is made which is wetter than the specification (100 ppm) or has become discolored. A 324 Rework Decolorizer and Drier are available to solve these problems. The offspecification material can be pumped from the Stabilizing or Day tanks to the decolorizer or drier or both. The reworked 324 then goes through the Transfer Filter to the Day tank inlet header. The Rework Decolorizer, charged with activated carbon, can be reactivated by water washing if it becomes badly contaminated. In some cases, steam reactivation is necessary. The bed should be purged thoroughly with nitrogen before putting in service. This reactivation normally leaves residual water in the carbon, thus requiring use of the Rework SL 0101D CONFIDENT! Subject to Protect- i of I4ib -ludicitil i-. No. 91-114b n -t 4-83 drier downstream. Please refer to MC Carbon Bed startup procedures for startup precautions. The Rework Drier is reactivated by hot nitrogen flow. Normally, about 8,000 SCFH of nitrogen for an eight-hour period will thoroughly reactivate the Dowex resin. The steam heating panels around the Drier must be used during this period. As in the case of the MC Driers, the important point is that the resin should reach 225F. Specialty Stabilization System: A small percentage of total 321 produced is blended to give specialty stabilized products. These specialty blends are many and varied and are not described in detail here. See the Standard Operating Procedures Manual for specifications and procedures. These Specialty blends must be free of contamination of Type 324 stabilizers and thus must be handled in separate tankage when possible. They often must be free of cross contamination with other specialty blends also. This requires flushing of tanks with 321 before making each blend. The specialty Stabilizer system consists of Stabilizing tanks 1 and 2 and Day tanks 1 and 2. Occasionally Nos. 3 and 4 Stabilizing tanks can be used for Specialty blends. Some of the blends use some 324 stabilizers and the 324 stabilizer pumps and lines are used. A line with a double block and bleed connects the 324 stabilizer manifold to Nos. 1 and 2 stabilizing tanks. Extra precautions must be taken when using this manifold to insure that no unwanted 324 stabilizers are pumped to Nos. 1 and 2 tanks. A Specialty Stabilizer pump is available to pump special stabilizers from drums into a separate line which leads to Stabilizing SL 010112 Subject 14th j Order rfc 4-84 tanks Nos. 1 and 2. This Specialty pump and line can be flushed with the blend from the tank--this is done by pumping with the Rework pump from the tank into a 1" line which goes to the suction of the specialty stabilizer pump. A Specialty Drier and Decolorizer are provided to remove water or color producing impurities from the special blends. The Rework pump can pull from all four specialty tanks and pump to the decolorizer, drier, or both and then discharge back into S-l, S-2, and D-2. A rotometer is provided to aid in monitoring the flow rate. The reactivation procedures for these vessels are the same as for the Rework Decolorizer and Drier. Please refer to MC Carbon Bed startup procedure for startup precautions. The specialty blends are normally loaded directly from the stabilizing tanks after appropriate laboratory clearance. The stabilizing tank suction header must be cleared of any traces of 324 stabilizers before starting to pump the special blends. This is normally done by pumping from the current production tank or another tank of 321 through the suction header by the 321 pump (324 pump in some cases) and back to the production or 321 tank via an overhead recirculation line. The blends are pumped to Shipping via a 3" 321 line or a 1 1/2" special drum loading line. These headers are normally cleared of trace stabilizers (from previous blends) by blowing with nitrogen into flush tanks at Shipping. Some grades of Methyl Chloroform are stabilized directly in the lined tank car since contact of the stabilizers with the steel tanks and lines results in high color product. When this is done, 321 is pumped to the tank car and the stabilizers are poured into the tank car. Subject of 14th 3 e Order ict Court 4-85 Stabilizer Storage: The stabilizers stored in tanks are received by PPG in tank trucks. These stabilizers are pumped by the stabilizer unload ing pump into lines leading to the storage tanks. One line is used for BLM and DOL-IBL, while another line is available for BTE and TLE. Each of these lines must be blown out with nitrogen after use. The hookup from the trucks to the unloading pump is done with flexible 3" hoses supplied by the trucker. Due to the flammability of these components, the truck motor should always be shut off before hooking up to the pump. Any leakage in the hose connections must be corrected by the truck driver before unloading. In order to save time and possible demurrage cost to PPG, the following procedure should be followed on notification of truck arrival by the Storeroom: 1. Have Storeroom send truck to the Guard Gate. 2. Sample the truck and submit sample to Lab for clearance. 3. While the Lab is analyzing the sample, have the truck move to the Tri-Ethane area and hook up to the unloading pump. 4. Unload when cleared by Lab. NRE and DOX are both stored in bulk, thereby eliminating the hazards and problems associated with the handling of them in drum quantities. They are each stored as 50:50 mixtures with Methyl Chloroform. Specific handling procedures (i.e., unloading, transfer, etc.) are outlined in the Standard Operations Procedure book. Drums of NRE are still stored in a bunkered area near the dock storage tanks in the event that bulk CONFIDENTIAL: Subject to ProtectJ of 14th Judicial i.; i ol r Ko. 91-1145 Order - our t 4-86 NRE is not available. They are moved from the storage building to the drum storage building at the Tri-Ethane^ plant as needed. The bunkered storage area is the responsibility of the Tri-Ethanearea and dock rounds should include this storage. Tri-Ethane Dock Storage: The Tri-Ethane dock tanks have a total capacity of 4,095 tons, 2,330 tons on No. 1 and 1,765 tons in No. 2. Each tank is equipped with a pad regulator which is fed from a nitrogen system. The regulators maintain a positive pressure of a few inches of water. Dry air coming from a set of dryers in the dock area used to be used but due to continued problems with the dryers, the pad system was changed to low pressure N2- The BS & B vent lids and pad regulators must be properly maintained so that excessive ^ flow is not used. Excessive N flow can lead to excessive expenses since we purchase the SubjechCtNPlD"-"J;^ of Uth Jj udici ' i' No. i i -1 Ordor :L curt4_87 VDCM SECTION The function of the VDCM System is to remove the color producing impurity (DCA) from the crude VDC to give a monomer grade product. The impurity has a boiling point almost the same as VDC and thus can not be removed by distillation. The conversion to a removable component by chemical reaction is necessary. The VDCM plant was designed as a batch process; that is, the reactor was filled, reacted, and then the reacted crude VDC was distilled. The plant has no spare pumps since in a batchwise process there will be periods when each section will not be in use. Operation of the VDCM plant has been revised; for specific information other than in this book, refer to the Standard Operating Procedures Book, The hazards associated with VDC are present in this plant as they are in the crude VDC section. All air must be excluded from the system and all liquid streams must be stabilized with HQMME. The processing equipment is stainless steel or nickel clad up to the point where the DCA has been removed. Steel equipment is then used for the product VDCM. VDCM Reactor System: A. Equipment 1. VDCM Reactor Feed Pump (SAC 55-1506). This pump is a Goulds Model 3196, size 2x3 - 8, with a 7 3/4" impeller. It is made of 316 stainless steel. It is driven by a 5 hp, 1750 rpm motor (SAC 50-3023). The pump uses a John Crane Type 9 mechanical seal. 2. MPN Addition Pump (SAC 55-746). This pump is an Eco Gearchem, Model T700. It is a positive displacement 316 stainless steel pump with Teflon gears. The full rated capacity is 3 gpm. The shaft seal is provided by Teflon/asbestos packing rings. Addi tional sealing is given by lubricant which is injected through SL 010116 4-88 a grease fitting into the packing gland. The pump is driven through a variable speed reducer by a 1 hp 1750 rpm motor (SAC 50-1394). Overpressuring of the pump and packing gland is prevented by a 1" 100 psig SRV on the discharge which vents back to the suction of the pump. 3. VDCM Reactor Heatup Pump (SAC 55-1507). This pump is a Goulds Model 3196, size 2x3- 13 with a 10" impeller. It is made of 316 S.S. and has a Chesterton 770 mechanical seal. The pump is driven by a 5 hp, 1750 rpm motor (SAC 50-3024). Seal flush to the pump seal is available from VDC vaporizer feed line or from the VDCM still reflux pump. 4. MFN Tank (SAC 60-507). This 3' O.D. x 3' tangent to tangent vessel is made of 316 S.S. The design pressure is 20 psig at 120F, Protection is provided by a 2" 25 psig graphite rupture disc. Full capacity is 172 gallons. 5. VDCM Reactor (SAC 60-381). The VDCM reactor is the TCE reactor from the 75 TPD plant which has been converted to VDCM service. The vessel is 5'6" l.D. by 28' seam to seam and is constructed with a 207= nickel cladding on the internal surface. The reactor has a capacity of 4,429 gallons at the 24' level (top of the sight glass). The design pressure is full vacuum to 75 psig at 400F. Overpressure protection is provided by a 75 psig graphite rupture disc. The MPN line enters at the 12' level and the heater outlet enters at the 15' level. 6. VDCM Reactor Heater (SAC 71-1266). This exchanger is horizontal with a steel shell and 316 stainless steel tubes and tubesheets. It has 74 - 1", 12 BWG tubes, 12' long. The shellside design pressure is full vacuum to 150 psig at 200 F. The tubeside is 2 pass. The heat transfer area is 232 sq. ft. B. Operation In 1973, a change in specifications on allowable dichloroacetylene concentration in VDCM eliminated the need for the VDCM reactor. As long as DCA's remain below 100 ppm the reactor is bypassed and only the VDCM still is used to remove the trans-dichloroethylene and toluene in the VDC crude. There are several modes of operation of the VDCM plant when the morpholine reaction is required. One method is a batch-wise reaction SL 010117 CONFIDENTIAL: Subject to Protective Order Of 14th Judicial D.strict Court No. i.! 4-89 and distillation of the VDCM. The dichloroacetylene in the crude VDC is reacted with morpholine in the VDCM reactor to give a heavy reaction product known as adduct. DCA + MFN ---------------- * Adduct This adduct has severe fouling properties throughout the system, so if at all possible MPN's use should be avoided. Detailed procedures on the batchwise operation of VDCM are available in the unit's standard operating procedures. A second method of operation of VDCM with MPN is the "semi-batch" method. After initial reaction with MPN, the VDCM is fed at a continuous rate (generally up to 5 gpm) to the VDCM still while morpholine is added to the reactor on regularly spaced intervals (e.g. every 4 hours). This method is successful up to the range of about 500-600 ppm DCA in the VDC crude. However, the fouling properties of the adduct are still present in the system, perhaps not the same magnitude as with the batch operations. Details of this procedure are also outlined in the S.O.P. manual. As long as the TCE product purity remains above 99.98% TCE (generally <.02% unsym TeCE or <.01% Trichloroethylene), the VDC crude product will contain less than 100 ppm DCA. This level of DCA does not affect the quality of the VDCM, so the VDCM reactor is bypassed and the VDCM still is used as a "polishing" still, removing trans-dichloroethylene and toluene. VDCM Still System: A. Equipment CONFIDENTIAL: Subject to Protective Order ox 14th Judicial District Court No. 91-1145 1. VDCM Still Feed Pump (SAC 55-745). This pump is a Goulds Model 3196, size 1x2-6. It is made of 316 S.S. and has a 5 1/4" impeller. The pump is driven by a 5 hp 3500 rpm motor (SAC 50- ). The pump uses a Chesterton 770 seal. Seal flush comes from VDCM still reflux pump. SL 010118 4-90 2. VDCM Still Reboiler Pump (SAC 55-1614). The reboiler pump is a Goulds Model 3196, size 3x4- 10, It is made of 316 S.S. with 8 7/8" impeller. The pump has a Chesterton 770 seal. It is driven by a 10 hp, 1750 rpm motor (SAC 50-3027). The seal flush stream comes from the VDCM still reflux pump. 3. VDCM Still Reflux Pump (SAC 55-1612), This is a Goulds Model 3196, size 1 1/2 x 3 - 13, made of 316 S.S. with a 11 1/2" impeller. The pump is driven by a 10 hp, 1750 rpm motor (SAC 50-3025), and uses a Chesterton 770 seal, 4. Stabilizer Addition Pump (SAC 55-1616). This is a Gearchem Model 706W, 3/8". It is made of 316 S.S. with Hastelloy C gears. The shaft seal is provided by Teflon/asbestos packing. Additional sealing is given by lubricant which is injected through a grease fitting into the packing gland. The pump is driven through a variable speed drive by a 1 hp, 1750 rpm motor (SAC 50-3022). Overpressure protection is provided by a 1" 100 psig SRV which vents from the discharge back to the suction. 5. VDCM Still (SAC 59-4). This still is 30" I.D. by 49*9" seam to seam. It is constructed with 20% internal nickel cladding. The design pressure is full vacuum to .50 psig at 35CPf. Overpressure protection is given by a 4" 40 psig praphite rupture disc. The still has 37 trays. The bottom 22 trays have Glitsch type V-4 ballast units, while the top 15 have V-l ballast units. The feed point is at tray 7. (Note: The original bottom 3 trays have been removed from this still. The original feed point was tray 10.) 6. VDCM Still Reflux Drum (SAC 60-1037). This vertical tank is 36" O.D. by 10' tangent to tangent. The design pressure is full vacuum to 75 psig at 200F. It is protected by a 2" 75 psig graphite rupture disc. The tank has a 107o 316 S.S, internal cladding. The full capacity is 513 gallons. 7. No, 1 HQMME Storage Tank (SAC 60-1085). This vertical 316 S.S. tank is 4' O.D. by 5' tangent to tangent. It has a design pressure of full vacuum to 75 psig at 200F. Overpressure is prevented by a 2" 50 psig graphite rupture disc. The full tank capacity is 489 gallons. 8. No, 1 HQMME Tank Agitator (SAC 61-73). The agitator is a Lightnin Model N33GDS-150. The 8.9" stainless steel impeller is driven at 350 rpm by a 1 l/2hp 1750 rpm motor (SAC 50-1439). 9. No, 2 HQMME Storage Tank (SAC 73-36). This vertical 316 S.S. tank is 3' tangent to tangent. The design pressure is 10 psig at 250F. It is protected by 2" 25 psig graphite rupture disc. The full capacity is 175 gallons. SL 010119 e,,, . CONFIDENTIAL, Of S1u4bthjecJtudtloiciFParroio?sa.: ..:,?!fO f No. 9l~2 4-91 10. No. 2 HQMME Tank Agitator (SAC 61-74). This is a Lightnin Model N33-100, top entering. It is driven by a 1 hp, 1750 rpm motor (SAC 50-1459). 11. VDCM Still Reboiler (SAC 71-1207). This horizontal exchanger is 316 S.S. on the tubeside and has 146 - l1', 12 BWG tubes, 12' long. The ghellside design pressure is full vacuum to 150 psig at 500 F or full vacuum to 120 psig at 650F. Tubeside design pressure is 150 psig at 200F. The tubeside is 2 pass. The heat transfer area is 459 sq. ft. This exchanger is interchangeable with the VDC vaporizer reboiler. 12. VDCM Still Condenser (SAC 71-1267). This horizontal condenser, is also 316 S.S. on the tubeside. It has 187 - 1", 16 BWG tubes, 12' long. The shell and tube sides are both designed for 75 psig at 300F. The exchanger has 588 sq. ft. heat transfer area. 13. Nos. 1 and 2 VDCM Driers (SAC 73-42). These 2 driers were bought as a package unit, Andes-Drilene Model #16M, Type S. Each drier is 30" O.D. x 62" tangent to bottom flange. They are clad with 316 S.S. The design pressure is 150 psig at 400F. Each drier is provided with a 1/2" x 1" SRV set to relieve at 150 psig. Each drier has a 450 pounds charge of activated alumina, Alcoa F-l or equivalent. The liquid is distributed by a cone sandwich with a fine mesh screen. Each drier is fitted with an internal steam coil, 316 S.S., which enters from the bottom. 14. No. 3 VDCM Drier (SAC 73-67). This vessel, salvaged from the Bensocola plant, is 2' O.D. by 5' tangent to tangent. It is constructed of stainless steel. The drier contains a 450 pound charge of activated alumina. The liquid enters the bottom through a 2" nickel pipe with holes drilled in it and a fine mesh screen over the openings. A stainless steel steam coil is suspended from a flange at the top. B. Operation The purpose of the VDCM Still system is to remove the trans- dichloroethylene and toluene from the feed. An integral part of this section is the stabilizing and drying of the product VDCM. The crude feed is pumped to the VDCM still (tray 7) with the VDCM reactor feed pump (the still feed pump is bypassed when the reactor is out of service). The feed rate is automatically flow controlled at the SL 010120 CONFIDENTIAL: Subject to Protective Order of 14th Judicial Lir':rict Court No. 91-1145 4-92 set point rate. VDC and heavies flow down the still into the pot and are pumped from the pot to the Still Reboiler by the Still Reboiler pump. The VDC is partially vaporized in the tubes of Reboiler by steam con densing in the shell. The vapor-liquid stream re-enters the still above the liquid level and below the bottom tray. The Heavies and unvaporized VDC are recirculated to the Reboiler along with fresh material coming in. The vaporized VDC goes up the still, out overhead and is con densed in the tubes of the VDCM Still Condenser by CTW on the shell side. The condensed VDC flows by gravity to the Still Reflux Drum. Reflux to the column is pumped by the Reflux pump at a specified set point rate. Product VDCM is taken off the discharge of the Reflux pump to the VDCM Driers. The product flow rate is automatically regulated to main tain the desired Reflux Drum level. The liquid in the Reflux Drum is stabilized with HQMME. The reflux then serves to stabilize the top part of the Still. HQMME in the Still feed aids in stabilization in the reboiler and bottom trays of the still. The heavies in the VDCM Still bottoms are continuously purged from the VDCM System back to the crude VDC Reactor. This bottoms stream takes off the discharge of the Reboiler pump and is flow controlled through a rotometer. The vent from the VDCM Still Condenser goes through a vent PCV to the VDC vent header going to the vent line off the Vent Scrubber. A nitrogen makeup PCV ties in right upstream of the vent PCV. CONFIDENTIAL? Subject ttoo PPrrootteecctive Order of 14th Juuddiicciiaaj.l hDi. istrict Court Ai Z> 4-93 The HQMME Addition system consists of the No. 1 and No. 2 HQMME tanks along with the Stabilizer Addition pump. HQMME is purchased for the VDCM plant in the crystalline form in 50 pound containers. The HQMME is dissolved in VDC in the HQMME tanks and then pumped to the system. The solution contains about 32% HQMME (150 gallons VDC per 50 pounds HQMME). Currently, the No. 1 HQMME tank is being used as a mixing and storage tank and the contents are transferred to the No. 2 HQMME tank as required. The solution is pumped from the No. 2 HQMME tank to the VDCM Still Reflux drum. Therefore, the two HQMME tanks are steam traced and all the lines carrying the solution are steam traced and insulated. The solution will boil at a fairly low temperature, so close control of the tank tempera ture must be maintained. No. 1 HQMME tank is equalized back to the VDCM still to avoid building pressure from the heated VDC. No. 2 HQMME tank vent is not equalized to the still because of the low pressure rating (10 psig) of the tank. There are several different operating schemes for the VDCM section-batch. Semi-continuous and continuous (using morpholine). With no morpholine the VDCM reactor is bypassed and the VDCM still is used as a purification still. For detailed procedures concerning these different modes of operation, refer to the Standard Operating Procedures manual located in the control room. Operating Conditions: When feeding the VDCM still under a non-MPN treatment situation the VDCM reactor feed pump is used and the VCV to the VDCM still controls the feed rate to the still. The steam rate to the Still Reboiler is SL 010122 .TIA7,; Order C'is'trict Court 1145 4-94 desired level. That is, as the level increases the steam rate auto matically increases to boil off more VDC. The discharge valve on the VDCM Still Reboiler pump should be throttled to give about 50 to 55 psig (with 15 to 20 psig still top pressure). Fully opening the discharge valve will result in cavitation of the pump. The blowdown of the still bottoms stream is controlled manually by a ball valve. Flow is indicated by a rotometer. The valve setting is set by the operator to keep the bottoms dilute enough in the still bottoms not to cause reboiler fouling. This is accomplished by maintain ing the appearance of the still bottoms. This appearance will become milky (with polymer) when the bottoms are concentrated. The desired normal appearance is clear or slightly cloudy. Any polymer present will make the bottoms cloudier and a very thick cloud requires heavies blowdown. The still bottoms blowdown stream is going to the VDC Reactor which has a aqueous solution of caustic soda present. If caustic backs up into the VDCM System, cracking of VDC will occur giving MCA. Thus, at least two valves on the bottoms line should be blocked when the Reboiler pump is taken down. The reflux rate to the still is maintained at 1 gpm for each gpm of feed. This 1:1 ratio has proven to give a good separation between VDC and trans-dichloroethylene. The still vent PCV is set to open at 20 psig during summer months. This will normally prevent venting of VDC. The N2 makeup valve is s.et about 5 psig below the vent PCV. The top pressure will decrease during the cool months. SL 010123 confidential Subject to Proteoti ve Order of 14th Judicial rict List Court No. 91-1145 4-95 Control of HQMME to the reflux drum is based on the content of HQMME in the VDCM downstream of the driers. The activated alumina in the driers will remove part of the HQMME. This undesirable feature must be corrected for by higher contents in the Reflux Drum. The specification HQMME content in the VDCM product is 180 to 220 ppm. This range is difficult to maintain and current practice is to shoot for drier outlet HQMME contents in the range of 100 to 250 ppm: adjustments of the final HQMME content in each batch are made as the VDCM day tank fills up. A minimum of 200 ppm HQMME in any liquid stream in the VDCM plantshould be maintained at all times. The operation of the VDCM Driers is important because the specifica tion VDCM product moisture is 50 ppm. The effluent moisture content must be routinely checked every two hours. When the moisture content exceeds 40 ppm, the flow should be switched into a freshly reactivated drier. The reactivation procedure for the used drier is: 1. Pressurize the VDC out of the used drier into the inlet of the fresh drier by using the cooling nitrogen line tied into the overhead line. 2. When the used drier is empty (indicated by a bullseye on the bottom line) shut off nitrogen and start water washing through the drier from top to bottom. Route the bottoms stream to the sewer through the line from that purpose. Make sure that the double block and bleeds are in service between the drier being washed and the inlet and outlet headers. Continue water washing one hour. 3. Shut off water flow and start steam flow through the Drier to the sewer--continue for one hour, 4. Shut off steam flow, put steam coils in service and start hot nitrogen flow through the driers (top to bottom). Continue for ten hours. Log the outlet nitrogen temperature every two SL 010124 Subject to :- v, O-f i.4itSr: ^uoicj `\v *r3 ci i 4-96 hours on the VDC Drier log. The alumina must reach 200F in order to be satisfactorily reactivated. If the tempera ture does not appear to be going to reach that level, in crease the hot nitrogen flow. Normally 10,000 SCFH flow is adequate. The source of the hot nitrogen is the nitrogen heater in the MC Section. 5. At the end of 10 hours, shut off steam coils and hot nitrogen and start cooling nitrogen flow. Continue the cooling until the outlet temperature is 90F (about 4 hours are required). When cool, leave the driers blocked off under 10 to 20 psig nitrogen pad. VDCM Day Tank and Storage Tank System: A. Equipment 1. No. 1 and No. 2 VDCM Product Transfer pumps (SAC 55-1615 and 55-1822). These pumps are Goulds Model 3196, size 2 x 3 - 10 with a 9 1/8" impeller. The pumps are made of ductile iron. They are driven by 10 hp, 1750 rpm motors (SAC 50-3028 and 50-3411). They use John Crane type 9 seals. 2. No. 1 and No. 2 VDCM Day Tank (SAC 60-1082 and 60-1216). These horizontal steel tanks are 84" O.D. by 16'8" tangent to tangent. The design pressure is full vacuum to 50 psig at 200F. The tank is protected from over-pressure by a 3" 50 psig rupture disc. The full capacity is 5,128 gallons each tank. The recirculation lines into the tanks are pro vided with special eductor type dip tubes. These eductors greatly aid in mixing in the tanks. 3. VDCM Storage Tanks Nos. 1 and 2 (SAC 60-1079, 1080). These horizontal steel tanks are 12' O.D. by 24' long and have a capacity of 21,900 gallons full. The design pressure is full vacuum to 50 psig at 200F. Overpressure is prevented by a 4" 50 psig graphite rupture disc on each tank. The recir culation lines to these tanks also have eductor type dip tubes which aid in mixing. 4. VDCM Loading Pump (55-1613). This is a Goulds Model 3196, size 2 x 3 - 10. It is constructed of ductile iron and has a 9 1/8" impeller. It is driven by a 10 hp, 1750 rpm motor (SAC 50-3026). 5. VDCM Storage Tank Recirculation Filter (SAC 72-73). This is a Filterite filter Model 6CMC25 - 1 1/2 316 Stainless Steel filter. It is 31 1/2" high by 8 1/2" diameter and contains 6 - 10" filter tubes. Its flow capacity is rated up to 60 gpm. SL 010125 CONFIDENTIAL: Subjectt tto Protectj i of -Uth J ac" 4-97 B. Operation The VDCM from the VDCM Driers flows to the VDCM day tank. The VDCM day taik is continuously circulated and regularly analyzed for H2O and HQMME. If the tank contents are out of specification, it may be reworked back to the system as necessary as the tank is filling with production so that when the tank is topped off it in within specification. A 2" rework line is provided which takes off the discharge of the product transfer pump. This rework line ties into the VDCM reactor and to the inlet of the VDCM driers. The day tank contents can be pumped back to the VDCM reactor for redictillation if necessary. The moisture level can be reduced by rework through the driers. HQMME level is also adjusted by rework to the driers. If the HQMME content is too high, the tank is reworked through the driers until the content is in specification. If it is too low, HQMME is added to the inlet of the driers until the desired level is reached. After each batch is cleared by lab analysis in the day tank, it is transferred to one of the VDCM storage tanks. Two day tanks allow the topped-off day tank to be cleared by the lab before transferring to one of the VDCM storage tanks. Each VDCM Storage tank is vented into a vent header through a common PCV to the vinyl chloride free standing vent stack. The tanks are held at a specified pressure (about 15 psig) by a nitrogen make-up PCV. The vent PCV set point is set so as to be closed except when transferring into the tanks. Alarms on the vent system indicate when the vent valve opens to prevent unknown losses. The VDCM day tanks have a similar vent alarm system. SL 010126 CONFIDENTIAL: of Subject t o P r n t p r f- I' 14 til Judicial" 't: LO . ar: e Order ict Court 4-98 VDCM is shipped in tank cars from Lake Charles to PPG terminals or direct to customers. The tank cars are loaded from the storage tanks, after appropriate laboratory reclearance by the VDCM loading pump. This pump discharges through a 3" loading line to the vinyl chloride loading rack. The vapor space of the tank car can be equalized back into the vent system of the storage tanks through a 2" equalization line. It can also be opened up to a blowdown line which goes to the free standing vinyl chloride vent stack. A tank truck loading station also allows VDCM to be shipped by truck to customer. The VDCM loading pump has a discharge manifold which goes to the loading line and to a recirculation line back to the tanks. The recir culation lines in the tanks are fitted with eductor nozzles which air in mixing. The loading line and the transfer line from the Day tank to the storage tanks are tied together by a manifold. Material from the storage tanks can be pumped back to the day tank or plant rework line by using this manifold. o-r -1*a /' \: .n> - . , .' .* * SL 010127 Of U6*ct CNf.IDc. Ut U-UUr **&**6, > c hOcff,feUrff. UTILITIES AND AUXILIARY EQUIPMENT 4-99 Steam and Condensate System A. Equipment 1. Desuperheater (SAC 80-6163). This unit is an 8", 300# Standard Copes-Vulcan Variable Orifice Desuperheater. The unit has a rotometer type float which moves up and down in a tapered chamber. 2. Condensate Collection Tank (SAC 60-951). This vertical steel tank is 5* O.D. by 10'6" high. It has a design pressure of atmospheric at 210F. The vessel is protected from overpressure by an overflow line which comes from the bottom of the tank up to the top and then down to the sewer. The vent line off the tank is fitted with an entrainment separator--this separator consists of a large diameter pipe with an internal dish and doughnut baffle arrangement. The doughnut has holes drilled in it for draining of condensate. 3. Condensate pumps (SAC 55-1513, 1514). These are Goulds Model 3196, size 2x3-13 pumps. They are made of ductile iron and have 12" impellors. They are driven by 15 hp, 1750 rpm motors (SAC 50-2868, 2869). They have John Crane type 9 mechanical seals. 4. Desuperheater pumps (SAC 55-1568, 1569). These pumps are Goulds Model 3316, size 1 l/2x2-9. They are all iron with 7 11/16" im pellors. They are driven by 20 hp, 3550 rpm motors (SAC 50-2878, 2879). B. Operation Steam to Area B comes from the 400 psig steam header from Area A. The steam pressure to the Area B header is reduced to 250 psig by a PCV located at the EDC Plants. The steam temperature is about 600-650F. This steam is further reduced in pressure for use in the Tri-Ethane plant. The primary steam PCV in Tri-Ethane reduces the steam pressure to about 135 psig. Overpressure protection of downstream equipment is given by a 6" x 8" SRV set to relieve at 150 psig. The 135 psig steam then goes to a Desuperheater which lowers the 600 to 650F steam temperature to the desired SL 010128 Subject _ of 14bii J U'-' " of SUb i`5U> ; L*J* tL. ilC o Wo. 7 t) ;;"WAL: Order jCt Court 4-100 temperature. This is accomplished by injecting steam condensate (at about 212F) into the desuperheater through a temperature control valve. The condensate is boiled by the steam, thus lowering the steam temperature. The desired steam temperature is automatically controlled by the rate of con densate injection. The normal desuperheated steam temperature is about 40QPto 450F. The minimum steam temperature is 358F, which is the saturated steam temperature at 135 psig. The 135 psig steam is further reduced to 45 psig for use in some equipment requiring lower steam temperature. The 45 psig steam header and downstream equipment are protected from overpressure by a 4" x 6" SRV set to relieve at 55 psig. The following lists give major equipment supplied by the two steam headers. SL 010129 . 135 psig 1 Lights Still 2. Heavies Still 3. Absorber Bottoms Heater 4. VDC Reactor 5. VDC Still 6. VDCM Drier Heating Coils 7. MC Drier Heating Panels 8. Nitrogen Heater 9. 324 Rework and Specialty Driers Heating Panels 10. Cell Liquor Heater . 45 psig 1 Cl2 Vaporizer 2. VDCM Drier Steam Wash 3. HQMME Tank Heating Coil 4. MC Stripper Reboiler 5. MC Topping Still Reboiler 6. MC Dopp Kettles 7. MC Flasher 8. VDC Vaporizer Reboiler 9. VDC Drying Still The steam condensate from all the above users, except the CI2 vaporizer and live steam injection, is piped to the Condensate Collection Tank. The condensate is pumped from the tank to the Area B condensate collection header by the Condensate pumps. The flow rate from the tank is automatically controlled to maintain a specified level in the tank. A sidestream is taken off prior to the LCV; this condensate stream is the condensate used in the VDC Section. Another sidestream takes off the discharge of the Condensate pumps and goes to the Desuperheater pumps. This condensate is the stream used in the Desuperheater. 4-101 Another steam system is available. This header operates at 30 psig and originates at the OHC plant. This steam system supplies the exchangers in the VDCM Section. No condensate collection system is available for the 30 psig condensate. Overpressure protection on this steam system is provided by a 3" x 4" 50 psig SRV. All the steam headers are provided with small steam traps in low spots or at dead-ends. These traps remove condensate as it collects and are important in that they rule out the possibility of "water hammer" development. If con densate did collect and was suddenly boiled off, the sudden increased volume and pressure can damage lines and equipment. These traps also play an important role in freeze protection. The 135 psig steam system is also tied into the HC1 Plant steam system. This tie-in allows the use of 135 psig steam on the jets which pull vacuum on the burners. This system also has piping available for reversing the flow, that is putting the HC1 Plant steam into the 135 psig line. A tie-in from the 135 psig line to the CI2 Vaporizer steam PCV makes it possible to operate the chlorine vaporizer on HCl plant steam. This feature is used when the Tri-Ethane plant (including steam system) is down and HCl needs chlorine for the burners. Cooling Tower Water System The actual control of the cooling towers is the EDC operator's responsi bility; however, due to the importance of this system the Tri-Ethane Operator should be familiar with the basics, particularly the piping in the Tri-Ethane plant. A thorough knowledge of the piping is important during startups, emergencies and tracing out possible leaks into the CTW system. Sl_ 010130 q.,K . of 14 CiiFj DFOT r n : ~f - liG- Order - ; 'M r t 4-102 A. Equipment A detailed equipment description is not included in this section. In general, four cooling towers are available, with two fans each and two pumps each. The basins of the towers Nos. 1, 2, and 3 are linked together. Also, the discharge of the pumps are linked together. See the attached figure for the layout of all pertinent piping. Well Water System A. Equipment 1. Well Water Recovery Tank (SAC .60-412). This horizontal steel tank is 78" O.D. by 17' tangent to tangent. It has a design capacity of full vacuum to 75 psig at 400F. Overpressure is prevented by a large overflow line to the sewer. 2. Well Water Recovery Pump (SAC 55-1625). This is a Goulds Model 3196, size 6x8-13. It is made of ductile iron and has a 12 1/8" impellor. It is driven by a 75 hp, 1780 rpm motor (SAC 50-3043). B. Operation At full design rates, the MC Reactor Coolers are designed to use 800 gallons per minute of well water. This well water is recovered for further use in the Well Water Recovery System. The water from the coolers flows into the Recovery Tank. It is then pumped to the line feeding make-up well water to the Cooling Tower basins. The flow rate of water from the tank is based on the demand called for by the cooling tower LCV's. If this flow rate exceeds the inlet water flowrate from the MC Reactor coolers, another LCV on fresh inlet well water opens up into the tank to supply the difference. Thus, the water going to the cooling tower basins may be a mixture of water from the coolers and fresh well water. If, on the other hand, the water flowrate from the coolers exceeds the demand by the cooling towers, part of the flow is diverted diverted through another line and LCV to the Sportsman's Lake. SL 010131 of 14th J Mve Order a-.ricL Court A-103 The well water from the MC Reactor Coolers is continuously monitored by a pH meter. If a leak should develop in the coolers the pH will drop and actuate an alarm. In this case, the well water from the coolers should be routed to the sewer immediately. The well water recovery system can then be bypassed if necessary. An alarm on pump shutdown is also available. Loss of the pump can lead to loss of level in the Cooling Towers very quickly. Fresh well water can be quickly routed into the discharge of the pump through a double block and bleed available for this emergency. When not needed, the double block and bleed should always be in service, thus preventing possible pumping of contaminated well water into the main well water header. Well water to the MC Section comes off the inlet line to the MC Reactor Coolers. Well water to the TCE, VDC, and VDCM Sections is metered into that overall area through one line. A tie-in from this line to the HC1 plant also is available and normally provides water for part of the HC1 plant. Nitrogen System Nitrogen is available in the Tri-Ethane and VDCM areas in two systems, a high (90 psig) pressure and a low (45 psig) pressure. This area is a major user of nitrogen. The consumption of nitrogen is an appreciable cost factor. For this reason, the nitrogen in from both lines is metered into the area. The 90 psig nitrogen comes directly off the Area B nitrogen header. The 45 psig line comes from the EDC plant where the pressure is dropped to 45 psig by a self-enclosed regulator. coOtN- FlUENTU-.L Order c court No. SL 010132 of SWuhjorcjJ-/' a;,: Nc The major users from each of the lines are as follows: 90 psig 1. All utility drops 45 Psif? 1. Dopp Kettle dip tube purge 2. Purging of Dopp Kettle feed line 2. Lights Still pad 3. Heated N2 for reactivation of driers 3. Heavies Still pad 4. VDCM Reactor pad 4. VDC Still pad 5. VDCM Still Pad 5. VDC Drying Still pad and purge 6. Cooling N2 for VDCM Driers 6. Stabilizer and Day Tanks pads 7. Stabilizer Storage Tank pads 8. VDC Storage pads 9. TCE Storage pad 10. VDCM Day Tank pad Checks of nitrogen consumption are periodically made to locate areas of excessive usage. A consistent culprit in the past has been the BS and B tank vents on Stabilizer, Stabilizing and Day Tank Storage Tanks. These tank vents are weighted lids which lift and allow venting when the pressure exceeds a design point. They also act to prevent vacuum formation in the tanks. This vacuum breaker consists of a thin flexible fiberglass type diaphram which is held against the tank sealing flange by a weighted vacuum ring. When the vacuum drops to the vacuum of the tank vent, atmospheric pressure exerted against the diaphragm lifts the vacuum ring into a floating position, thus letting air into the tank. The flexible diaphragm is easily cut; therefore, caution should be exerted when opening and closing the tank vent lids. If the diaphragm is cut, it allows nitrogen to continually leak out. Instrument Air System Instrument air is supplied to the area by Elliot air compressors located west of vinyl chloride. Two reciprocating compressors provide additional air. This air is dried and filtered at the compressor area. Area B air pressure normally runs about 80 psig. In the case of loss of instrument air, the con trol valves in the Tri-Ethane-VDCM area are designed to fail in the "safe" position. Some surge time of air is available from the Air Receiver located SL 010133 S U b "j <-; i Of 14th 4-105 by the 324 pump, but this is of very short duration. Some critical control valves in the area are equipped with individual air supply tanks to actuate the valves as necessary during loss of instrument air. TCE Section Refrigeration System The cooling and condensing achieved in the TCE Vent Condenser is critical to the successful operation of the Tri-Ethane plant. The refrigeration system which removes the heat energy from the gas stream is complex and requires a thorough understanding of both equipment and principles of operation. Time spent in learning and reviewing these fundamentals is time well spent. A. Equipment 1. TCE Section Refrigeration Compressors (SAC 56-248,247). These compressors are Carrier Model 5H120 reciprocating units. Each compressor is driven by a 50 hp, 1150 rpm motor (SAC 50-2842, 2843). Each compressor has 12 cylinders with 3 1/4" bore and 2 3/4" stroke. The basin of each compressor has two electrical crankcase heater elements with 200 watt output each. The capacity of the oil basin at normal level is 20.29 gallons. The compressor heads are water cooled with CTW. 2. Freon Condenser (SAC 71-1218). This horizontal shell and tube condenser has 133 carbon steel tubes with 423 square feet on the Freon 22 (shell) side. The shellside design pressure is 385 psig at 300F, while tubeside is designed at 250 psig at 300F. Over pressure of the shellside is prevented by a 3/4" by 3/4" SRV set to relieve at 395 psig The water makes 6 passes on the tubeside. 3. TCE Refrigeration Unit Oil Separator (SAC 60-1023). This small steel vessel is fabricated from 10" pipe and is 1*6" from seam to seam. It is protected from overpressure by a 1/2" by 3/4" SRV set to relieve at 300 psig. The Separator is heated by steam tracing to remove the Freon from the oil. 4. Drier-Filter Cores. These moulded porous are Sparlan Catch-All type C-269 or equivalent. Two of the cores are installed in the drier-filter case. These core elements remove water, trace amounts of acid and entrained particles. 5. Moisture and Liquid Indicators. These indicator sight glasses are Sporlan See-All Type number SA-155 on the oil return line and Type number SA-195 on the liquid freon line. At 100F these indicators show a green color when moisture level is below 45 ppm, chartreuse when in the 45-130 ppm range and yellow when above 130 ppm. The moisture ranges increase with decreasing refrigerant temperatures for the same colors. SL 010134 A-106 B. Operation The general principle of operation of a refrigeration unit is the acceptance of heat into a refrigerant which boils off the refrigerant, the compression and then condensing and cooling of the refrigerant. Thus, in effect the system is taking heat from a process stream and transferring this heat energy into a more warm system (CTW) by utilizing the pressure-temperature relationships of the refrigerant. The refrigerant used in this plant is Freon 22. A better understanding of what is taking place in each part of the refrigeration system may be gained by following the F-22 around a pressuretemperature diagram. First the freon is boiled off in the freon evaporator (TCE Vent Condenser). The pressure does not change in this step, but the temperature of the subcooled liquid freon goes up into the superheated vapor range. This step is pictured as follows: Pressure Evapor -- Chilled HC1 temperature Temperature Sub of 1 A C11 ^ Order t Court 4-107 This freon gas is slightly above its boiling point and is now compressed by the reciprocating compressors. The gas is superheated more during the com pression. This step is shown as follows: Pressure a Temperature ----------- *- Compressing the gas makes it much easier to condense. It is condensed in the Freon Condenser by CTW and partially subcooled. The pressure remains at very nearly compressor discharge pressure. This step is shown as follows: Pressure n SL 010136 Temperature COI.'FID; 7Tj AL: S U b j e ; of I4tii U LiO ^ Z `*"tive Order r, j : ; ~ j-ct: Cour No. ,i 4-108 This condensed freon at the condensing pressure is still too hot to use in the TCE Vent Condenser. For example, at a condensing pressure of 245 psig, the saturated temperature of the freon will be 115F. The freon pressure is now dropped to evaporator pressure across a control valve. In passing across this flash valve, part of the freon is vaporized and thus cools the liquid freon. This subcooling step reduces the pressure and temperature and closes the pressure-temperature loop as follows: Pressure o Temperature -----------The refrigeration capacity of this two compressor system is 30 tons with a refrigerant suction temperature of -20F. The actual suction temperature runs considerably above -20F and the actual capacity of the system is much higher. At 0F saturated suction temperature, the total capacity is 60 tons, and requires 50.6 horsepower per compressor. Flow of Freon 22 in System: The evaporation of Freon 22 on the outside of the tubes in the Vent Condenser causes bubbles of Freon to flow up through the liquid Freon and into the vapor space. The liquid level should be high enough to just cover the tubes. Measurement of the level is done by a sight glass. The sight glass has a vertical pipe tied into the inlet and outlet piping right ; /\ j Orc/ej'! r ,, 4-109 behind the sight glass. Most of the flashing occurs in this pipe, thus re ducing the boiling in the sight glass and thereby increasing visibility. A low liquid level in the evaporator will cause the vaporized Freon 22 to pass across tubes which are uncooled. This results in superheat of the vapor and subsequent excessive loading on the compressor. The vaporized Freon 22 flows through a specially designed loop (to be discussed in Oil Flow Section) into the suction manifold of the compressors. The suction manifold in each compressor is fitted with a felt filter'known as the suction sock. This felt filter catches most of the solids, such as sand or corrosion products, in the gas going to the compressors. The gas is compressed by the machines and discharges to the condensing and subcooling section. The actual cubic feet capacity of the compressors is constant (except where cylinder unloaders are used--discussed later). The displacement of each com pressor is 182 cubic feet per minute. It is important to note that the actual throughput of pounds/minute is thus dependent on the density of the vaporized Freon. The density is dependent upon the pressure and temperature of the suction gas. The power requirement is greatly dependent upon the pounds/ minute flow rate of Freon. Thus if a compressor is fully loaded (motor drawing maximum amperage) at 15 psig suction pressure, an increase of the suction pressure to any point appreciably above 15 psig will cause automatic shutdown due to motor overload. Thus, if the cooling load in the Vent Condenser in creases with a fully loaded compressor, the suction valve at the compressor must be throttled to keep the actual flow of pounds/minute of. Freon to the compressor at the maximum allowable flow. The overall effect of this throttling is to raise the evaporating pressure, which in turn raises the temperature at SL 010138 v` _ .1 ,,, Subject tc ] of 14 th ho. 'T AL: " ' '-'s Order Vict courf.uo which the Freon evaporates. The higher temperature of the Freon 22 results in a higher HC1 temperature. Throttling of the suction valves is normal operating procedure at high rates. The superheated freon gas leaves the compressor and flows up to the Freon Condenser. The Freon is condensed on the shell side of the condenser by CTW in the tubeside. This liquid Freon 22 is partially subcooled in the condenser and flows from the condenser through a drier-filter and to a level control valve. This LCV holds a low liquid level in the Freon Condenser, The level is indicated by a float chamber. The Freon LCV serves a dual purpose. In addition to its function as a LCV, it also serves as an expansion valve for the Freon 22. The Freon pressure is dropped from compressor discharge pressure to the evaporator pressure. This expansion results in partial flashing of the liquid to gas and the consequent subcooling of the liquid Freon. The flashed Freon gas and liquid stream enters the bottom of the Freon evaporator (shellside of Vent Condenser), This completes the Freon 22 cycle. The refrigeration system can be artificially loaded by bypassing hot discharge gas back to the vapor space of the evaporator. This artificial loading is sometimes used at low production rates. CD CO O -- o _l CO Oil Flow in the System: Oil is present in the circulating Freon 22 stream due to leak-by of the compressor cylinder rings and the vapor pressure of the oil itself. This oil is entrained in the discharge gas as a very fine mist and vapor. The oil flows up to the Freon Condenser where it collects and condenses with the Freon. The oil flows with the Freon to the evaporator. The oil is more dense than the liquid Freon and settles out into the bottom of the Freon evaporator. The flow of the oil stream is appreciable and must be returned to the compressor for reuse. A slight level of oil is maintained in the evaporator. The oil at this point is saturated with Freon and is not suitable as a lubricant 4-ni in this cold raw state- The oil flows off the bottom of the evaporator to the Oil Separator. This small tank' is equipped with steam tracing around it which raises the oil temperature and flasher off part of the Freon. The vaporized Freon flashes off and goes back into the side of the evaporator. The flow rate of this vapor stream must be throttled to prevent the Separator and heater from acting like a small thermosyphon reboiler. Opening of the vapor valve will result in a liquid flow overhead and subsequent overloading of the heating capability. Proper operation of this system will give an Oil Separator temperature of 80 to 100F. The oil flows from the Oil Separator through a moisture indicator and then ties into the Freon suction line going from the evaporator to the compressors. The suction line at this point is specially designed so as to carry only fine oil mist down into the compressors. The suction line comes off the top of the evaporator and then makes a loop down to the bottom of the evaporator and back up to the top of the evaporator. The loop back up to the top of the evaporator prevents equalizing liquid oil or Freon into the suction line to the compressors via the oil return line. The pipe loop going back up to the top of the evaporator is sized so as to carry only fine mist, rather than large droplets. A sub stantial liquid flow could lead to damage in the compressor heads. The oil mist in the suction gas flows into the suction manifold of the compressor and drops into the basin through openings located for that purpose. The level of oil in the compressors is visible through a small round glass sight part. It is critical that the level be visibly maintained in the sight part. Loss of level can quickly lead to loss of lubrication oil flow in the compressor and subsequent damage. On the other hand, a high level could cause liquid to back up into the heads--thus blowing them off. The dangers of the latter are obvious. SL 010140 CONFIDENTIAL: Subject to r-:ci:-o\ ve of 14th JutUcir.'- : No * ' " Order ^ ';r ~ 4-112 The basin oil level is controlled by manually throttling the oil return from the Oil Separator to the suction line. This is a needle type valve and thus is susceptible to plugging by small particles. Any adjustment of oil flow should be done by closing and opening the valve 2 to 3 rounds a couple of times before setting its final position. Another path of oil return is also available. This consists of a 1/2" line from the bottom of the Oil Separator which goes directly to the basins of the compressors. The use of this line is dangerous because either liquid Freon or cold oil saturated with Freon can be returned to the basin. The com pressor bearings will be wiped out very quickly if liquid Freon or oil loaded with Freon is used as a lubricant. This line should not be used except in extreme emergency, and then only for a short period of time when you know the oil is above 80F. A better method of emergency oil make-up is direct fresh oil injection into the compressor from an external oil pump. Oil return with two compressors can be tricky and lead to serious com pressor problems. The amount of oil being returned to each compressor is directly related to the Freon flow to each compressor. Thus, if No. 1 compressor is pulling more Freon than No. 2, the oil level would go high in No. 1 and empty in No. 2. This problem is taken care of by equalizing the liquid levels between the oil basins by a 1/2" line (this line is the bottom end of the direct oil return line from Oil Separator). If the basin pressures are equal, the oil levels will equalize by gravity. Equal basin pressures is accomplished by equalizing the vapor spaces through a 1" line. The capacity of this line is limited by a needle type block valve. If the flow requirement between basins is large, unequal basin pressures may still be present. 010141 SL CONFIDENT,? AL: Subject, to Protective Order Of I4th Judicial District Court No. 91-1145 4-113 Unequal compressor loads is a major problem in control of oil return. This unequal load can be caused by improper throttling of the compressor suc tion valves. The suction valves should normally be adjusted so as to give equal compressor amperage. The current draw by the motor is the best indication of compressor load. Unequal load can also be caused by plugging in the suction rocks. This causes an additional pressure drop downstream of the suction socks If one of the socks is more fouled than the other one, the basin pressure will drop on the compressor with the most fouled one. In this case, the suction valves should be throttled to give equal basin pressures until the socks can be changed. The pressure drop across the sock is indicated by the difference in the compressor suction pressure and the basin pressure. Oil can be easily and quickly transferred between the oil basins by utilizing the equalizing line and varying the basin pressures. If the oil level needs to be lowered in No. 1 and raised in No. 2, close the vapor equalizing line, throttle the suction valve on No. 2 until the basin pressure is less on No. 2 than No. 1. Oil will then flow from No. 1 to No. 2 due to the basin pres sure difference. Compressor Oil Flow: Oil is picked up out of the basin of the compressor and flows through a screen to the gear type oil pump. The oil pump discharges through a full flow filter with renewable cartridge. The flow then goes to the front end of the drilled oil passage in the crankshaft, to the rear bearing and seal with some flow going into the drilled crankshaft from this end and to the capacity control oil system. The oil flows back to the crankcase by leakage from the bearings and from an oil pressure regulator which vents the oil to the crank case when it exceeds a certain pressure. SL 010142 CONFIDENTIAL: Subject to ProfeoOrder of 14th Judicial T)i ;-,i i : c Court No. 4 114 The capacity control system is fairly complex (see Figure 1)* Basically the control system operates by letting certain cylinders idle or work by using the suction valves. If a cylinder is idling, the suction valve is prevented from seating off by lifting it with push pins. Thus, the piston pulls in suc tion gas and then pushes it back out through the suction valve. The push pins which load or unload a cylinder are activated by an unloader power element. The unloader power element is a spring loaded piston operated lever. Turning the capacity control valve (located on the front of the compressor) clockwise lets more oil flow to the basin of the compressor from the control oil system, thus dropping the control oil pressure. As control oil pressure drops, the piston is pushed down by the spring, which moves the lever so that the push pins lift the suction valve off the seat and unloads the cylinder. Counter clockwise adjustment of the capacity control valve drops oil flow to the basin, raises control oil pressure and loads the cylinder. Utilization of the capacity control system will allow lowering the capacity to one-third of the full capacity. Another aspect of this system is that on startup of the compressors, only one-third of the cylinders will function until the oil pressure builds up. This prevents gross overload of the motor on startup. Compressor safety shutdown devices: The compressors have several automatic safety shutdown devices. Each one is designed to protect against a particular event occurring. 1. Low Suction Pressure. This switch stops the motor when the suction pressure drops below 6 psig. The purpose of this is to always maintain a positive pressure on the refrigeration system and thus guard against pulling air and moisture into the system. This switch is reset when the suction pressure reaches 35 psig. This is accomplished by cracking open the suction valve, since this switch takes its impulse between the suction valve and the suction sock. SL 010143 CONFIDENTIAL: Subject to Pt <: c~ j vo Order of 14th Judicial District Court No. 91-1145 PRESSURE PUSHES THE RELAY PISTON AGAINST THE SPRING AND OPENS PASSAGES BETWEEN THE OIL PUMP AND THE UNLOADER POWER ELEMENTS. SERVICE rarrier) 4115 SUCTION VALVE DISC ) ? THE LIFTER PINS DROP AND SEAT THE SUCTION VALVE DISC, LOADING THE CYLINDER Jj Li L, D CJ o "U0 u O -U 'J 0: ; -i-i li in -S> C ' * ^ c ^^ , -iQ-J i-t^ L ^ O' CL -I u Oo o u j-i n u <Dn .j5J r: 3 --1 CD 4. THE VALVE THROTTLES THE FLOW OF CONTROL OlL TO THE CRANKCASE, CAUSING THE CONTROL OIL PRESSURE TO BUILD UP OIL ENTERS CAPACITY CONTROL CIRCUIT THROUGH ORIFICE FROM COM PRESSOR OIL PUMP CIRCUIT O 3. COMPRESSION OF THE RANGE ADJUSTMENT SPRING ALLOWS THE VALVE SPRING TO MOVE THE PUSH PINS AND VALVE NEEDLE POINT TOWARD THE VALVE SEAT. A RISE IN CRANKCASE PRESSURE (CAUSED BY A RISE IN EVAPORATOR LOAD) INCREASES THE PRES SURE AGAINST THE BELLOWS AND COMPRESSES THE RANGE ADJUSTMENT SPRING. CRANKCASE PRESSURE ENTERS HERE FROM CAPILLARY. SURGE CHAMBER CUSHIONS RAPID FLUCTUATIONS. FROM CRANKCASE PRESSURE (SUCTION OF OIL PUMP) CONTROL OIL PRESSURE....... CRANKCASE PRESSURE... OIL PUMP PRESSURE... FIG. f - 5H120 CAPACITY CONTROL (BEGINNING SERIAL NO. 0447119) 12 V V C> Co 4-116 2. High Discharge Pressure. This switch shuts down the compressor when the discharge pressure reaches 275 psig. The compressor also has an internal relief valve which opens up at 275 psig to put discharge gas back into the suction manifold. The shutdown switch prevents operation of the compressor against a restriction in the discharge line. The impulse comes off upstream of the main compressor discharge valve. It is reset when the discharge pressure falls to 250 psig. 3. Oil Pressure Differential. As described earlier, oil flow in the compressor leaks back to the crankcase from the compressor bear ings. Excessive wear in these bearings results in low resistance to oil flow and a corresponding low oil pressure. This oil pres sure must be measured in terms of the crankcase pressure; thus, the differential between the oil pressure and the suction pressure represents the actual resistance given by the compressor bearings. The oil pressure differential switch shuts down the compressor if the difference drops below 18 psig. This is the minimum pressure allowed to give adequate lubrication and full operation of the capacity control system. Operation at lower oil pressure will result in only partial loading of the cylinders and possible permanent damage to the compressor crankshaft. The oil impulse comes from the motor end main bearing, while the crankcase pressure comes off the side of the oil pump cover on the other end of the compressor. The design oil pressure difference is 45 to 55 psig. The switch has a 3 minute time delay--it must then be reset manually. 4. Motor Overload. Overloading the compressors will result in over load of the motors. The motors are designed for maximum sustained amperage draw of 66 amps. 5. Solenoid operated valve on oil return line. This valve closes when both compressors are down. This prevents possible flow of liquid Freon into the oil circuit. 6. Crankcase Basin Oil Heater. These electric heaters come on auto matically when a compressor is shut down. The heaters keep the oil warm and thus prevent the accumulation of Freon in the oil. This heater must be shut off whenever the compressor is down and the oil drained. With no oil to remove the heat the elements could get hot enough to burn the oil when it is added, thereby causing a fire and possible injury. It is very important to try to determine the cause of compressor shut down before trying to restart the unit. For example, if a low oil level led to a low oil pressure differential shutdown, restarting could wipe out the compressor bearings. Evaluating what may have kicked off the compressor will lead to quicker and easier startups. SL 010145 q.lh, CONFIDENTIAL: ler 2" w-?Mrict Court ufc 'Co Prof::;'; of I4ch Judicial L'ollt. i c t C c u r c. No. 91-1145 MC SECTION REFRIGERATION SYSTEM 4-117 A. Equipment 1. Compressor (SAC 55-124 and spare is 56-245). This compressor is a Carrier model 5H60 reciprocating type. It is driven by a 40 hp 1800 rpm motor (SAC 50-1557). Each compressor has 6 cylinders with 3 1/4" bore and 2 3/4" stroke. The basin of the compressor has a 200 watt electric heating element. The normal capacity of the oil basin is 2 2/3 gallons. The compressor heads are cooled with well water. The oil filter on this compressor is not a full flow filter. 2. Freon Condensers (SAC 55-529, 718). These horizontal condensers operate in parallel. The design pressure is 300 psig at 300F. The tubeside is 8 pass. The condensers have 90/10 cupro-nickel tubes. 3. Oil Separator SL 010146 4. Drier Filter. This unit uses one of the cores described in TCE Refrigeration System. B. Operation The basic principle of operation of this system is the same as the TCE Section unit. The equipment is slightly different. The condensed liquid Freon is partially subcooled by the suction gas in a double pipe economizer. Also, two parallel condensers are used. The LCV in this case is an H. A. Phillips 270-A Valve Assembly. This assembly is essentially a float mounted to a needle valve. As level goes up, the needle valve is opened further. The valve has a 3/16" orifice opening. The orifice is not big enough when the unit is heavily loaded and the float chamber must be partially bypassed. The chamber has a vent line off the top which ties back into the condensers. The flow through this line should be throttled. The oil flow in the MC Refrigeration system is basically the same as in the TCE system. The only major exception is that the Oil Separator is mounted in the discharge of the compressor and separates oil mist be centrifugal force. The separated oil is returned to the basin of the compressor via a float-needle 4-118 Lv 1 r Another difference in this system is that no direct oil return from the bottom of the evaporator to the compressor is available. The compressor safety switches have the same function and mode of operation as in the TCE Section. The low suction pressure shuts down the corn- pressor at 5 psig and resets at psig. High discharge kick-off occurs at 280 psig and resets at 250 psig. Oil differential pressures below 18 psig will shut down the compressor. Oil differential must be manually reset after 3 minute time delay. Overload amps on the compressor are 49.7. The basin oil heaters come on automatically with compressor shutdown. There is no solenoid in the oil return line--thus, it is important that the oil return line be blocked each time the compressor is shut down. Capacity control is similar in principle as the TCE compressors. The compressor capacity may be reduced by one-third. Special Discussion of Lapp Pumps Lapp pumps are used at several critical locations in the Tri-Ethane plant. An understanding of the operating principles of these pumps is very helpful. The Lapp Pulsafeeder is a combination piston-diaphragm pump. The piston operates only in an oil system--it never contacts the process fluid. The piston moves the oil which hydraulically moves a diaphragm alternately forward and backward. The displacement from this diaphragm movement, in turn, takes the process fluid through a suction check valve on the suction stroke of the piston and discharges this fluid through a discharge check valve on the discharge stroke. The check valves are located such that the discharge check is closed when the suction check opens and vice versus. The capacity of the pump is SL 010147 4-119 regulated by regulating the length of the piston stroke. The further the piston moves, the more the diaphragm moves and the greater the throughput. The oil side of the pump is protected from overpressure by a relief valve which blows off oil under excess pressure back into the oil reservoir. On the other hand, any oil which leaks by the piston on its discharge stroke is replaced by vacuum compensator valve which automatically draws in oil from the oil reservoir on the suction stroke. The operation of the pump is illustrated in the figure on the following page. Any air in the oil cylinder or head will compress and expand with the movement of the piston. This cuts or stops effective diaphragm movement. Each pump has a bleed point on the top of the diaphragm head on the oil side for bleed off of air. Note that this loss of air volume must be made up with oil and that the opening of the bleed should be coordinated with the piston stroke to insure operation of the vacuum compensator. On Lapp pumps with a remotely located diaphragm head, such as No. 2 HQMME pump, the oil system is equipped with air bleeds at both the piston chamber and at the oil side of the remote head. Water sometimes gets into the oil system. This will be indicated by a creamy, milky appearing oil. This contaminated oil greatly reduces the capacity of the pump. The oil should be drained, the oil reservoir flushed with Tri-Ethane and refilled with Mobil Vactra Oil No. 2 or its equivalent. r ' '"? Of(fist Figure 2. Lapp Pump Operating Principles 4-120 Suction Stroke The spring holding the relief valve closed will be overcome if the discharge pressure is too high, releasing oil into the oil reservoir. Discharge Stroke Discharge Check Relief Valve Vacuum Compensator Suction Check 0 Cuts greatly exaggerated to illustrate principles involved. As the oil piston moves on its suction stroke, the suction check valve opens. If the piston has leaked by on its discharge stroke, the spring holding the vacuum compensator closed will be over come, allowing oil to enter the cylinder. As the piston moves on its discharge stroke, the suction check closes and the discharge check opens. SL 010149 coui y 1 Lti s'Stu%'cot uttoyc\lO9`i--1-1'15 of Xio- or aer i ,'3ch to Protective Order of 14th Judicial District Court No, 91-1145 STARTUP AND SHUTDOWN SECTION 5-1 The purpose of this section of the manual is to give a general approach to the startup and shutdown of the equipment in the Tri-Ethane and VDCM area. A detailed step by step shutdown sequence is not given because the sequence will often vary with the timing and conditions of startup. The only exception to this is the fairly detailed writeup on the chlorine vaporizer. Overall Startup Scheme: Startup of the TCE Section generates TCE and HCl. If the HC1 can be used in the Area B HC1 system, TCE Section startup will normally be first. If the HCl must be scrubbed, a different approach should be taken. In this case the MC Section still train should be brought on before startup of the TCE Reactor. Then, the MC Reactor can be started as soon as HCl purity is good, thereby reducing the amount of HCl to be scrubbed. Startup of the VDC Section hinges on VDC Storage inventory. If inventory is very low, this section can be brought up before TCE and MC. Storage of VDC Vaporizer bottoms becomes a problem after a time. However, if a substantial VDC inventory is available, startup of the VDC section can be delayed until after TCE and MC section are up. Startup of VDCM can occur only when the VDC Section is running. This is due to the VDCM Still Bottoms tie-in to the VDC reactor. VDC inventory also determines VDCM startup time. The above described general approach can be used to determine shutdown sequence. TCE and VDC inventories should be considered carefully when shutting down. SL 0I0I50 oA"b^ctCNFl''S'^,. TCE Section ttr ' - -5 i'l. ? r,^>- 5-2 ct c ' ourt In general, the TCE Section equipment is started up in this order: Heavies Still, Lights Still, TCE Reactor. The chlorine vaporizer may be started up any time prior to TCE Reactor startup and left floating on the line. The Heavies Still is normally started up on total reflux. The column is put on total recirculation through the bottoms drier and filter prior to heat introduction. This cold recirculation is accomplished by pumping from the reboiler to the Drier-Filter, then to the Reflux drum via a special line and then back to the still via the reflux line. This recirculation assures a dry column and filters out any solids in the system. The steam is then brought up and the still put on total reflux when ready. The Lights Still can be started up several ways, including total reflux. Probably the easiest way and safest way is to start up the Absorber loop first. This is.done by pumping from the-Heavies Still Feed Drum to the Absorber, from the Absorber bottoms to the HC1 Separator and from there to the Lights Still Reflux drum. This last part is done through a special line which ties the HCl separator LCV to the condensate drain on the Lights Still condenser. This allows complete circulation of the Lights Still. The HCl Separator (and TCE Reactor) may have to be artificially pressured with nitrogen to keep HCl Separator level control. This can be done with a nitrogen tie on the vapor equalizing line between the HCl separator and the TCE Reactor. This loop pro vides a constant overflow from the Lights Still which aids in maintaining a re boiler level during startup. The reboilers are then slowly put in service. Once the Lights Still is up to temperature and no EDC is in the Heavies Still Feed drum, feed can be established to the Heavies Still. The Heavies Still SL 010151 5-3 Reflux Drum LCV has a tie-in back to the suction of the Lights Still Feed pump so that the product on the Heavies Still can be recycled back to the Lights Still Feed. The feed from the TCE Reactor should be floating on the line so that some EDC can be fed to the Lights Still. In this way the Lights Still Reflux drum LCV (Lights Still recycle) can be put in service to return EDC back to the TCE Reactor. This is important as positive flow back to the TCE Reactor ensures that the AIBN feed (it ties in to the Recycle line at the TCE Reactor) is going into the TCE Reactor. Care must be taken to be sure that the valving is done properly when putting the Heavies Still pro duct back to the Lights Still feed pump suction. It is possible to put TCE reactor liquor (i.e., EDC and HvCl) out to TCE storage if the wrong valves are operated. 010152 TCE Reactor and Cl? System Startup This detailed writeup is designed for startup of the CI2 vaporizer and TCE Reactor. In the event that the HC1 plant is taking CI2 from our vaporizer eliminate items 11, 12, and 14 of the detailed startup list. Items 2 and 4 of the pre-startup check list on the CI2 vaporizer are also to be eliminated. The remainder of the check list and startup procedure still apply. Before proceeding on the startup of either the TCE Reactor or the Cl system the pre-startup checklists must be completed. As the sequence of starting up the reactor and CI2 system progresses, the startup check list of each must be referred to and items initialed off as they are done. An item must be satisfied on the check list before proceeding with the next step of the startup. 1. Sample TCE Reactor Liquor for no chlorine--use sample point at the TCE reactor LT and at LSF pump, 2. Start up Lights and Heavies Still and have them on recycle, making spec product. 3. Pressurize TCE Reactor and put the Absorber loop in service. Have the TCE side cooler out of service. r 'i;"'' ' L: Subj:: - c'. - ; vs Or tier of 14th JuUicit.i District Court No, 91-1145 Subject to Protective Of 14th Judicial Distric Order t Court No. 91-1145 5-4 4. About two hours before starting CI2 to the TCE Reactor put on both AIBN pumps. Be sure that flow is going to the Reactor (LS recycle must be going to the Reactor to carry the AIBN into the reactor). 5. Block HC1 to MC FCV and HC1 to HC1 plant PCV. Bypass the TCE vent condenser and check out the vent PCV to the scrubber for good operation. 6. Mix the TCE Reactor with N2 using the bottled N2 that is tied into the CI2 piping. Manually open the anti-backup valve. To do this, remove the cover plate on the anti-backup valve open switch and switch it from "Auto" to "Manual". After mixing the Reactor, close the anti-backup valve by putting the switch back to "Auto". Reinstall the cover plate. 7. Start C2H4 to the TCE reactor at 12,000 SCFH. Vent to the scrubber. Check LSF and TCE Reactor for chlorination before putting C2H4 to the reactor. 8. Check to be sure CTW flow is established through the TCE reactor overhead condenser and side arm cooler. 9. The CI2 sparger valves should be open and the anti-backup valve should be closed at this point. 10. The downstream block valves of both the Cl2 PCV to the surge drum and CI2 FCV should be blocked as the bypasses will have to be used for startup. The bypasses of both the CI2 FCV and PCV are sealed with a serialized seal. The lead operator must authorize use of the bypass on either one of these control valves. Whenever one of the seals is broken, it must be immediately logged in the log book. The entry will contain the seal serial number, time of use of the bypass, and reason for using the bypass. As soon as the bypass has been closed again, it must be immediately resealed by the lead operator and the time and serial number of the new seal will be logged into the log book. These seals carry the same requirements for removal as does a lead operator tag. 11. Check Liquid CI2 line pressure and notify Liquefaction that you are ready for liquid CI2 take. On the startup you will be using about 27 TPD liquid CI2. Refer to the check list concerning CI2 vaporizer startup and check off items as they are completed. There are items that need to be checked before starting CI2 to the reactor. 12. Bleed any condensate out of the CI2 vaporizer steam chest and leave bleeds open for startup. Establish a steam flow through the vaporizer Be sure no liquid CI2 is in the vaporizer as at this point the CI2 vaporizer is a closed system. 13. Be sure that the CI2 PCV to HCl is blocked. If they are on the line and we are starting up notify them that we are to take CI2. 14. Check for liquid CI2 or organic at: a. CI2 PCV to the surge drum rb. CI2 surge drum (bottom drain) c. Cl2 FCV. COf'r'' Subject f 14th Ji-ci. No, '*].? I -e Order -ict Court SL 010153 CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court No. 91-1145 5-5 15. Slowly crack liquid CI2 into the CI2 vaporizer. Watch PI on vapor line out of CI2 vaporizer. 16. Block the N2 pad system on the CI2 line to the TOE Reactor at the CI2 FCV. Leave the N2 bottlesfloating onthe line for future usePut double block and bleed in service. 17. Bypass the CI2 PCV and log the broken seal. Build up to system pressure of 75 psig on the CI2 surge drum. Check the anti-backup valve to be sure it is open. (AP between CI2 surge drum and TCE reactor greater than 3 psi will open the anti-backup valve). Be sure the manual trip device on the anti-backup valve has been deactivated. 18. Crack the bypass on the CI2 FCV to the TCE Reactor (log the broken seal) and start feeding CI2 to theTCE Reactor. A man will have to be at the CI2 PCV and one at the CI2 FCV. Bring the Reactor up to 50 TPD TCE rates. Maintain 75 psig on the Cl surge drum. Watch CI2 vaporizer outlet temperature to be sure it is warm. 19. Check LSF, TCE reactor overhead, and TCE reactor bottom for chlorina tion. 20. When the temperature alarms on the inlet to the surge drum and CI2 surge drum bottom clear green, the low temperature shutdown system (it closes the CI2 PCV and FCV at 110F) is deactivated. However, rather than trying to put the FCV and PCV into service (and risk a premature shutdown) do not put the control valves into service until the CI2 temperature into the surge drum and the CI2 surge drum bottom temperature are both above 130F. 21. Reset the CI2 PCV and FCV shutdown system behind the MC board. Check the CI2 PCV and FCV for good operation and put them in service. As soon as the bypass valves are closed, the lead operator will seal them both and log the seal numbers (and time) in the log book. 22. Check LSF and TCE reactor over head for chlorination. Start cutting C2H4 stepwise keeping a close check on the reactor for chlorination. 23. Put the TCE vent condenser system in service. 24. Once the ethylene is block to the TCE reactor, the HCl can be diverted from the scrubber to the users. Startup and shutdown of the chlorine system should be carried out with the following points in mind; 1. Never leave liquid chlorine trapped in a vessel or line--particularly one which has a heat source other than ambient temperature. 2. Vaporized chlorine will condense in the piping and surge drum when under normal liquid line pressure and normal ambient temperature. SL 010154 CONFIDENTIAL; to FrcM'?'"cive Order Of 14th JudiciaJ i-. r : r.i c{ Court Ho. 91-1X45 3. Any change in liquid chlorine flow will effect the other users, in that the line pressure will change. Sudden, large changes could possibly lead to closing of the excess flow valves on the feed chlorine tanks. The startup of an empty vaporizer is accomplished (assuming the vaporizer is already dry and ready for use) by first establishing a steam flow through the chest. Partial bypassing of the steam traps will be necessary at this point. Maintain 5 psig steam chest pressure. Slowly open the inlet chlorine valve (with all outlet valves closed). The liquid will vaporize until the pressure in the vaporizer is equal to the feed line pressure. At this time, the inlet line next to the vaporizer will feel warm--as there will be an equilibrium condition here such that a small flow of chlorine will flow into the vaporizer, boil off and flow back up the inlet liquid line until it recondenses. When this condition is reached, the inlet valve can be fully opened and flow started forward through the pressure control system, while paying careful attention to the steam chest pressure. Chlorine vaporizer shutdown is accomplished by slowly reducing chlorine flow off the vaporizer to the cut-off point. Then close the block valves at the pressure control valves. At this point the vaporizer is in the equilibrium condition described in the startup sequence. This is a safe way to leave a chlorine vaporizer, and leaves it ready for easy startup. An alternate method is to slowly shut down chlorine flow by closing the inlet chlorine valve, while leaving steam chest pressure at 5 psig. No liquid will form in the vaporizer under this condition; however, liquid chlorine could form in the downstream line and surge drum under ambient temperature conditions. Also, startup involves coordinating the very slow opening of the inlet chlorine valve with the establish ment of downstream chlorine flow. Initial TCE Reactor Pre-Startup Check List 1. Check TCE reactor for no O2 (vapor space). .2 TCE Reactor bottom sampled for no CI2. 3. Lights Still Recycle flow to TCE Reactor. 4. A1BN flow to TCE Reactor. 5. HC1 to HC1 PCV blocked. .6 HCl to MC FCV blocked. 5-7 Date_____ Lead Op. Operator X *C x X 0^0 <. -T* o ^ V\ v ' /> O' ^ S' .'-V? X' . c o. O' y o. 7. TCE Vent Condenser bypassed. .8 HCl PCV to Scrubber in service and operating. 9. TCE Reactor notchlorinated (L.S. feed). .10 Mix TCE Reactor with N. Anti-backup valve open switch back on automatic. Cover plate reinstalled. .11 C2H4, flow to TCE Reactor. .12 Reactor pressure up to 45 psig. N2 pad to HCl separator vapor line double blocked and bled. 13. Side arm cooler out of service (organic side) . 14. EDC feed to TCE Reactor ready. 15. CTW flow through TCE Reactor overhead condenser and side arm cooler. 16. Anti-backup valve closed. 17. CI2 Sparger valves open. CI2 Vaporizer Pre-Startup Checklist 1. Liquid CI2 line pressure up to normal. Liquefaction notified for CI2 take. .2 Steam condensate drained from CI2 vaporizer. Drains open. 3. CI2 PCV and FCV Block valves blocked. Bypasses shut. 01 ISO 4. Cl2 to HCl plant PCV blocked. 5. Liquid CI2 or organic check: a. Cl2 PCV b. CI2 surge drum bottom c. Cl2 FCV .6 N2 pad system to CI2 line blocked off at CI2 FCV. 0? Initial Cl? Vaporizer and TCE Rx. Startup Check List 5-8 Date_____ Lead Op. Operator 1. CI2 Vaporizer warmed up. .2 Anti-backup valve open (pressure on CI2 Surge drum up to 75 psig). 3. CI2 to TCE Reactor at 50 TPD TCE rates - Stepwise, a. Chlorination checks; 1) LSF 2) TCE Reactor overhead. 4. CI2 Surge Drum bottom temperature and inlet CI2 temperature above 130F (alarms green). a. Push reset botton on low temperature shutdown system (allowing valves to operate). b. Stroke Cl2 PCV. c. Stroke CI2 FCV. 5. CI2 PCV in service. Bypass shut, sealed. Seal No. logged in log book. .6 CI2 FCV in service. Bypass shut, sealed. Seal No. logged in log book. 7. Chlorination checks. a. LSF b. TCE Reactor overhead. .8 C2H4 reduction stepwise with chlorination checks. 9. TCE Refrigeration/vent condenser in service. .. M..- Sub^iee ct Qf 14th 01 No- . ^ . i > r C IT SL 010157 .object to t ^'C-r of 14th Judicial No. 91-1145 `O-..: Court 5-9 Shutdown of the TCE Section can be accomplished in several ways. One method which has proven successful is as follows: 1. Decrease reactor rate over reasonable time so as not to adversely effect other liquid chlorine users. 2. Drop still feed rates while cutting reactor rate. Lower the Heavies Still Feed Drum level before lowering Heavies Still Feed. 3. Block Heavies Still feed--then block steam and shut down feed, reflux and Heavies Still feed pumps. Let Lights Still dump. Shut down equipment in Absorber loop. 4. Block Heavies Still Bottoms LCV, then block steam and shut down reflux and bottoms pumps. Let the still dump. The heavies accumu lated in the bottom may be pumped to the reflux drum for startup. When the Lights Still is dumped into an empty Heavies Still Feed Drum, *0 !5 8 a total volume of 1 1/2 feed drums will accumulate. This information is useful when clearing Lights Still reboilers for maintenance. The Heavies Still may be bypassed for maintenance with shutting down the rest of the TCE Section. The VDC Section stills can then purify the product if operated at low rate. Bypass of the Heavies Still is accomplished via a special line which takes off downstream of the still feed FCV and ties in upstream of the TCE Product Cooler. AXBN flow to the Lights Still Recycle is regulated to keep free chlorine from coming out of the TCE Reactor in the Lights Still feed stream. Chlorine breakthrough is checked for every hour by mixing a sample sample of Lights Still feed with an orthotolidene - H2O solution. Presence of free chlorine is indicated by a yellow to red color; i.e. small amounts of free chlorine result in pale yellow color, while a major chlorine breakthrough is indicated by dark red color. This mixture should be clear at all times. If a color is developed, an increase in AIBN flow must be made. This is accomplished by increasing the setting on the AIBN pump or starting the spare pump, or even increasing the strength of AIBN in the feed tanks. Bypassing of the Heavies Still should be avoided since the heavies will react to MCA and DCA in the VDC Section which can eventually concentrate in the vent system of the MC Section. CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Cour No. 91-1145 (t JaJ ' .45 - 5-10 If the chlorination cannot be controlled by either additional AIBN flow- or by use of a higher concentration of AIBN in the AIBN feed, the TCE Reactor must be shut down. Do not use ethylene to control chlorination in the TCE Reactor. If the TCE Reactor chlorinates badly all of a sudden, shut the TCE Reactor down. Do not fight a sudden, bad chlorination with AIBN or ethylene. In either of the above cases, notify supervision immediately. In the event of a shutdown that involves one of the safeguard systems on the CI2 system follow the below listed procedure for shutting down the TCE section and other equipment. 1. Thoroughly check the CI2 system to determine the cause of the malfunction--is it truly an upset or did an instrument fail. 2. If there is no liquid CI2 in the system (and the malfunction is due to instrument failure), break the seals on the bypass valves on the CI2 PCV and FCV (log in log book) and start the CI2 system back up. Get someone out to work on the instrumentation. Refer to the check lists and startup procedures for the TCE reactor and CI2 vaporizer. Check TCE reactor for CI2 before starting up (reactor and LSF). Check for CI2 often on startup. 3. If there is liquid CI2 or organics in the system, notify supervision and shut the plant down as follows: 4. Block the CI2 FCV to the TCE Reactor. Manually trip the antibackup valve on the CI2 to the TCE Reactor after putting the N2 pad system in service on the CI2 line. If the cause of the shutdown was due to the anti-backup valve closing due to a malfunction, remove the cover on the anti-backup valve open switch (field mounted) and switch it from "Auto" to "Manual". Purge the CI2 line into the Reactor and call Supervision. Reclose the anti-backup valve after purging the CI2 line. 5. Pressurize the HC1 separator and TCE reactor with N2- Use the N2 tie-in (double block and bleed) on the vapor line between the HCl separator and TCE reactor. This will keep the absorber loop in service. 6. Block the HCl PCV going to the HCl plant. 7. Take TCE reactor side arm cooler out of service SL 010159 8. Block CI2 PCV to CI2 surge drum 9. Block HCl to MC reactor. Shut down VDC vaporizer feed. 5-11 10. Put MC section on recycle. 11. Put Lights and Heavies stills on recycle. Use line from HSR drum LCV back to LS feed pump suction. 12. Reduce rates on VDC section and put on recycle. Cut off feeds if TCE storage level is less than 2 feet. 13. Shut down the TCE refrigeration system. Also shut down MC refrigera tion system. 14. Put VDCM on recycle if it appears that the shutdown will be more than a couple of hours (or if VDC storage is below 3.0 on the board). 15. Shut down the A1BN pumps. 16. Check LSF and TCE reactor for chlorination. 17. Check all equipment that has been completely shut down to be sure there is a positive pressure to eliminate getting water into the system. confidential- Sub ie c t t o f 14th Joe; c ' r o i. o i-1 i ve Order ^^i-iU5rict Cort SL 010160 VDC Section 5-12 Startup of the VDC Section can only be done after thorough purging of the system to remove oxygen. Either nitrogen or steam may be used to purge the system. Also, the startup of the VDC Reactor and Still must be done in such a way as to keep TCE and VDC from dumping to the sewer. The normal sequence of startup is as follows: 1. Start steam to VDC Reactor and Still--continue steaming until the entire system is at steam temperature. 2. Then start reflux to both the VDC Reactor and Still, and condensate to Reactor. Also, start HQMME flow. Some material will be required from VDC Storage as makeup. Establish approximate normal temperature profiles. 3. Startup VDC Drying Still on total reflux. When product is dry, put on recycle from VDC Storage. 4. Start feeds to VDC Reactor-~check for excess caustic. If the steam flow and caustic excess are properly controlled, no dumping of TCE or VDC will occur with this startup method. Shutdown of the VDC Section should be done in such a way as to prevent dumping. The normal shutdown sequence is as follows: 1. Pull VDC still Phase Separator level as .low as possible. 2. Block VDC Reactor feeds, reflux and condensate flows. Continue steaming. Switch production to No. 1 Storage. The impurities in the columns will now come overhead and care should be taken not to contaminate the large VDC Storage Tank. 3. When No. 1 VDC Storage is full, shut down Drying Still. This is accomplished by blocking the product LCV first. The VDC Still Phase Separator will hold the remaining organics in the column. 4. Continue steaming until the columns are at steam temperature. 5. Then block steam and check N2 PCV's. 0)0^1 r Qi 5-13 MC Section Startup of the MC Section should always be preceded by a check for mois ture in the system and nitrogen purging. The following sequence of startup has proven successful: 1. Put Stripper on cold recirculation. This consists of feeding the Stripper from Flasher Accumulator, flowing of bottoms LCV into the rework line (feed to Topping Still blocked), through the rework line back to suction of Stripper Feed pump. The stripper system pressure will have to be maintained by nitrogen. 2. Actual startup of the Stripper should be proceded by putting slow steam flow to the Flasher to get it at boiling point (steam can then be cut off) and putting the Topping Still on total reflux. 3. Start steam to Stripper reboiler. When Stripper feed temperature reaches 135F, stop recirculation and put stripper bottoms to Topping Still (the stripper feed pump will start cavitating when feed temperature reaches 140F). 4. As Topping Still Accumulator level builds up, put MC Section on internal recycle by putting T.S. product back to Flasher. Bring Stripper up to desired temperature profile. 5. Start up Dopp Kettle. 6. MC Reactor startup can now be accomplished when HC1 is available. Catalyst addition should consist of 15 to 20 pounds about every 15 minutes until the reaction takes off. The VDC Vaporizer should be started up at such a time as to assure 3 to 5% VDC in the reactor when HC1 introduction begins. Startup of the Neutralizer-Drier system can be done as soon as MC Reactor starts reacting. Shutdown of the MC Section should be carried out in such a way as to not put out of specification product in storage. This is accomplished by blocking the Stripper LCV before shutting down the Stripper. The rest of the equipment shutdown is just a matter of blocking steam and process flows and shutting down pumps. Normally the MC Reactor recirculation pumps and Flasher agitator are left running. The Dopp Kettle should be dumped and the feed line emptied. Also, the steam tracing on Dopp Kettle feed line must be shut off. A periodic purge off the bottom of the Flasher must be taken while it is down to prevent accum ulation of tars. SL 010162 CONFIDENTIAL: Subject to Protective Order of 14th Judicial District Court /SOv*CX 'SOC TB4KL3 cts MO* // jroct 7tS0 /^OA64ff 4-v. w; <-/r. 1* zoo/**? wr jft 30*449 6?.3e3 .7 2 96,993 77.74^,50 90.993 -<W <S 96934 .0/ 0 *33.4/9 90.990 '/33.4/7 .0/ 0 atf 040* W 160*09/406 73 iOO/*06 .01 2 *390 4000 99.9434900 .04 Ot a 2 .09 to 2 70^/. 9/C* 7 *402 /AOtO ^^ *346 acj sSSO *s 92 Sas eras ac^v' 69oo 240 97.2 - 330 A3 2d A3 27 *JE> /J0 W -0 40 .Af / <g4fif A 0 >.AS / ./0 40 03/\ 5^*5/ ?7.<? .57* t.3 43 /O.O 40 t.2 20730/ 33 4630/ 4./ <3Wo. ? 43*64 , ^K*<rwr * iq&*K .40 <flT wr* zae^wrUj7c *33 A40 W it-2 as 3,07 03*0 ./7 40 ,t& 43 /?o ,04 tO 93-70 2%03 03.9 34 f .93 /O 99.4727,344 -Of 2 .9/ 2 .03 22 30 22 0n.0 /og/&3 o w'-ra* /am**-? f9.4, /tOOO o.O 42 at 3 73. t A *7* o0a/9r*0*, 39 2*2/2 0.9 .1 > JO ~SO S3 Stas* <3 720 Si -*5 21300 S9O*0*Jt Oktg 94*+-* 70 \4BAjy- ^.... a i-ia. 3rVO*O*tMr *C0T4Vv~ HCL VICL V7B04C6J3 CM7C3 /-* "C4# 7TOrdt now' REVISION* AC/A6~ij.SWtA~A.y*/9/sA*4tcA#s/v.s** ^^CjMl/4444. 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