Document 67KY2LJdpNJ2GaQzK5yrE334

R. D. Alaburda November 1975 Chambers Works 234-459 180 459 184 1-1-1 11LITHOSOL11 RED 2B ACID PRESSCAKE "LITHOSOL" RED 2B ACID Principle of Process Red 2B Acid Crude is dissolved in hot water with ammonia and clarified with Darco. The product is filtered then precipi tated from the clarified solution with sulfuric acid, cooled, filtered and washed with water. The product is packed as wet cake from the nutsch as "Lithosol" Red 2B Acid Presscake or it is dried and packed as "Lithosol" Red 2B Acid. Reaction H03S nh2 Red 2B Acid Crude M.U. 221.7 + NH4OH---------- Ammonium Hydroxide M.W. 35.0 CH3 H4NO3S + H20 nh2 Ammonium 2-chloro4-ami no-toluene-5sulfonate (I) M.W. 238.7 Water M.W. ch3 2(1) + H2S04 2H03S Sulfuric Acid M.W. 98.1 Lithosol Red 2B Acid M.W. 221.7 Yield The standard yield is 96.0% of theory. + (NH4)2S04 Ammonium Sulfate M.W. 132.1 R. D. Alaburda OPERATING INSTRUCTIONS Chambers Works November 1975 234-459 180 459 184 III-l "LITHOSOL" RED 2B ACID PRESSCAKE Materials and Equipment SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Bill of Materials Code No. Materials Lbs./Chg. Orchem Spec. 848 200 2 Red 2B Acid Crude (2-Chloro-4-Toluidine- 5-Sulfonic Acid) 1 ,300 1. Purity 94.0% minimum 2. Unconv. 2.0% maximum 049 700 Ammonia 28% 294 31 -A 190 000 Darco S-51 75 48-D 946 200 Super Cel 25 139-S 945 000 Sulfuric Acid 563 35-S Product 459 180 "Lithosol" Red 2B Acid 1,250 59-RD 459 184 "Lithosol" Red 2B Acid Pres scake 1 ,250 30-L-l Equipment DMA Bldq. K-2 T-l B-6 T-2 N-l N-2 F-l P-54 Technical Basis Chambers Works Process 234-848 240, Red 2B Acid Purified by R.D. Gano dated July 12, 1971. TA-C-71-490 and conclusion dated August 19, 1971 "Purify Inferior Red 2B Acid Crude". TAC-72 835 and conclusion dated January 24, 1973 "Demonstrate drying in QNA Graining Bowl". TA-C-73-470 and conclusion dated August 6,. 1973 "Purify SubNormal Quality Crude". TA-C-74-272 and conclusion dated November 4, 1974 "Purify Sub Quality Crude". TA-C-75-165 and conclusion dated March 5, 1975 "Purify SubNormal Quality Crudes". M U-23C R 2 DUP050467862 N33031.01 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS ,lL ITHQSQL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111-2 Hazards Hazards Red 2B Acid Is not flammable or volatile. However, it may cause cyanosis or dermatitis. Wear rubber gloves when handling and a respirator if dusty. Ammonia Aqua (ammonium hydroxide) is a colorless, alkaline liquid, m.p. -72C. It is highly toxic by ingestion and moderately toxic by inhalation or contact. It can inflict serious burns. It can react with oxidizing materials. When heated it emits highly toxic fumes of ammonia. Wear rubber gloves, face shield, and acid suit when handling aqueous ammonia. Wash off affected areas with water should contact occur. Filter Cake should be treated as a cyanogenic. Avoid skin contact by wearing rubber gloves and rubber boots when digging the nutsch off. Wash off affected areas with water and report to Medical. Sulfuric acid: A heavy corrosive, strong mineral acid varying from colorless to light brown in color, usually containing some white ferrous sulfate crystals. Will burn skin severely. Not flammable, although in contact with most metals hydrogen is released and can result in a pressure explosion. It is a danger ously strong oxidizing agent, liberates much heat when mixed with water (17.75 k-cal/mole), and spatters violently if water is poured into it. Wear rubber gloves, acid suit and face shield when handling sulfuric acid or where there is a possibility of leaks or spills. Wash off all affected areas with H2O and report to Medical . Super-Cel is a light tank to pink powder which has no known toxic properties. The effects of breathing the dusts are not known, but usual industrial care requires protection from dust inhala tion. DUP050467863 OPERATING INSTRUCTIONS R. D. Alaburda Chambers Works November 1975 234?459 180 459 184 III-3 ' "LITHOSOL" RED 2B ACID PRESSCAKE Equipment Flow Sheet SUBJECT: "LITHOSOL" RED 2B ACID OPERATIOH: RlMU-2K! DUP050467864 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL11 RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111-4 1. Charge kettle K-2 with 8,700 lbs. of water. Wet dip on side of K-2 should be 24 2". Check valves. 2. Put vacuum on blowcase B-6 and suck 1,050 lbs. ammonia 28% (or ammonia recovered 28%) into B-6. Ift spilled on clothing or skin, wash with cold water and be transported to Medical Building, a) Wear face shield. b) Check lines and valves. c) This is 10" in B-6. 3. Blow ammonia to kettle K-2 with the agitator on. 4. Charge K-2 with 1,300 lbs. Red 2B Acid Crude. WEAR GLOVES AND IF PRODUCT IS DUSTY, WEAR A RESPIRATOR. 5. Add 75 lbs. Darco and 25 lbs. Super Cel after all crude Red 2B Acid has been charged. Wear respirator if material is dusty, 6. Make total volume up with water to 70 + 2" wet dip on the side of K-2 (20,000 lbs. water volume)? Shut agitator off when rodding. 7. Mix and heat charge to boiling - 93-100C and boil one hour. a) Use automatic control on steam. b) Keep charge definitely alkaline (orange on Brilliant Yellow paper. Add more ammonia if necessary. c) Avoid fumes by using air on vent line. 8. After boiling vigorously for one hour, make up volume to 70 +. 2" side wet dip again, and heat to 95C, Make up filter press - set lines to return to K-2. 9. Filter charge through press and back to K-2 until filtrate from all press spigots runs clear and free from Darco, etc. Stand by during filtration. Pump from K-2 using pump P-54 and take off on side of cone at bottom of K-2. D DUP050467865 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111-5 10. When filtrate runs clear from all spigots, change lines and run filtrate to Haveg tubs T-l and T-2. Watch dip in T-l and T-2, although charge should fit in with room to spare for the sulfuric acid. Divide charge evenly between T-l and T-2. 11. After filtration is complete, fill K-2 cone with water (2,000 lbs.), heat to 90C, and circulate through the press and back to K-2. a) Wash press for at least 5 minutes. b) Press will hold residue from 3 charges before cleaning is required. Blow dry before discard ing sludge. c) Dump sludge into cans and label "Darco Sludge from Red 2B Acid". d) Start recharging K-2 as in Step No. 1 for next charge. 12. Heat charge in T-l and T-2 to 95C, agitation on. 13. Put steam on slowly to avoid rupturing lead coils. Always turn steam off coils before adding acid. 14. Add the 93% sulfuric acid slowly, splitting the 563lbs. of acid equally between each tub until each tub is acid (blue) to Congo Red paper. Steam off during acid addition. a) Wear an acid suit; place warning sign on stairs. b) Acidification should take place over approxi mately one hour at a steady rate. Acid stream should be about size of a pencil. The product precipitates. If spilled on clothing or skin, wash with cold water and be transported to Medical Building. 15. Test each tub for completeness of precipitation, add more sulfuric acid, if necessary, until a test shows the precipita tion is complete. Take sample, cool to 30C, filter, and add a few drops of sulfuric acid to the clear filtrate. If no precipitate forms, the acidification is complete. If a precipitation occurs, add a few more pounds of sulfuric acid to the charge and request the test. Incomplete precipitation will result in yield loss. Wear an acid suit when performing precipitation test. MU-2361 H 2 DUP050467866 R, D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111-6 16. When charge is completely precipitated in each tub, cool to 25-30C or colder. 17. At 25-30C or colder, drop contents from both tubs to one nutsch, either N-l or N-2. This will require several loadings on the nutsch. 18. Wash cake, after sucking down, with 5 cold water washes for presscake and 10 water washes for the dried "LithosoV1 Red 2B acid, sucking down after each wash. The water should be 3" above the cake level on each wash. Excessive washes will result in yield loss. 19. Suck nutsch dry for at least 4 hours. :3 DUP050467867 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111 -7 "Lithosol" Red 2B Acid Presscake 1. Pack the presscake into ten FDA 510 9043 fiber drums with polyethylene liners. Load 225 lbs. net into each drum. WEAR RUBBER GLOVES AND RUBBER BOOTS WHEN DIGGING THE NUTSCH. * 2. Take at least four composite samples from the lot. Three samples are for the lab and the fourth is for the file. The samples should be composite samples from the drums. Use the wet sand method. Take a composite sample from every three drums. The file sample can be a composite from all samples. Wet sand method: Force a thief tube through the entire depth of the product in the drum. Remove the thief tube and discard the sample leaving the hole undisturbed. Reinsert the thief tube in the original hole and rotate it until it is filled with a representative sample taken from the walls of the original hole. (This procedure is known as the "wet sand" sampling technique). Sample each drum of a lot in this manner, placing the samples in a single plastic bag. Seal the bag, and mix its contents thoroughly by kneading. 3. Label the samples: "Lithosol" Red 2B Acid Presscake. Request: % Solids (Oven dry) - All lab samples % Purity (dry product) (one sample only) % Unconverted and Solubility, (one sample only) 4. Label each drum: "Lithosol" Red 2B Acid Presscake. 5. Seal containers with a polyethylene disc and wipe clean for shipment. 6 I R2 DUP050467868 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOl" RED 28 ACID PRESSCAKE SUBJECT: "LITHGSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 III- 8 ANALYTICAL REPORT ' COST CODE PRODUCT CODE 459 18fT* ar ea INTERMEDIATES --WESTbl d g . DMA SAMPLE OF LITHOSOL RED 2B ACID SENT BYDATE: ANALYZE FOR A. M. p. M. TECH. NO. RESULTS CHARGE NO. LAB ONLY % PURITY C\>i\J?>cAvc:~T 1 UNCON SOLUBILITY MU-156-R6 OnSAMPLE Asrti****- S.-rsi 3 NO. W"* LOT BUILDING CHARGE PN1A AREA OATS ADDN'L. INFOo TJME MU-71J-A-R1 HAZARDS EQUIPMENT v*' TAKEN BY TOXIC 0" CORROSIVE FLAMMABLE NO UNUSUAL HAZARD DUP050467869 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 28 ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 111-9 thosol 111 0Red 2B Acid 1 . Pack the presscake into 10 reclaimed drums with quick locks for drying in GB-3.- WEAR RUBBER GLOVES AND RUBBER BOOTS WHEN DIGGING THE NUTSCH. .2 Label the drum: "Lithosol" Red 2B Acid Presscake. 3. Follow the general operating procedure for operating GB-3. 4. Load the drum into GB-3 then seal GB-3. Accumulate 2 charges of 20 drums before drying in GB-3. 5. Use 50 psig steam on the jacket and dry at 100 to 110C with full vacuum. The jacket temperature will reach 125-130C. 6 . Dry in GB-3 for 12 to 14 hours. The vacuum should be down to 25 mm Hg for at least one hour for adequate drying. Q 7. Sample for moisture at the end of the drying period. 8. If the moisture is less than 0.5%, dump the charge into 11) FDA 510 9043 leverpaks at 225 lbs. net. If the moisture is too high, dry for an additional 2 hours and repeat Step 7. 9. Take three 8 oz. samples; from the drums; one for GAL, one for the file and the third for the Technical Laboratory. Label: "Lithosol" Red 2B Acid Request: Purity Solubility and Unconverted 99.0% min complete 0.25% max 10. Label the leverpaks - "Lithosol Red 2B Acid". 11. Seal and wipe clean each drum for shipment. DUP050467870 R. D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 III-10 ANALYTICAL REPORT ar ea INTERMEDIATES --WEST bio o . DMA rnsT rnr>F iw i PRODUCT CODE 459 180 SAMPLE OF LITHOSOL RED 2B ACID DATE: ANALYZE FOR A. M. P. M. TECH. NO. RESULTS < CHARGE NO. . LAB ONLY % PURITY UNCON SOLUBILITY 1 h2- Ul lA MIMS64M * A J3SAMPLE OPl /n ^ /T/2 ^ No. h*0* LOT BUILDING CHARGE (J/J/Aj AREA LEQUIPMENT TAKEN BY HAZARDS TOXTC^. Er CORROSIVE DATE ADDN'L INTO. TIMS FLAMMABLE MU-7tt>A4lt NO UNUSUAL HAZARD DUP050467871 R, D. Alaburda November 1975 OPERATING INSTRUCTIONS "LITHOSOL" RED 2B ACID PRESSCAKE SUBJECT: "LITHOSOL" RED 2B ACID OPERATION: Chambers Works 234-459 180 459 184 III- 11 "These Operating Instructions have Been issued after a full review of current technology and building experi ence as of (date), and conform with the current process techno!ogy as recorded." (Supervisor1s si gnature) Building Supervisor Senior Supervisor Chief Supervisor, Operati onsJ Chief Supervisor, ut. fiuyMwu? Tech, or Plant Ass flee #4448 Dat'e_ //--/f('7g/ Date Da te / & /7Cv 'Uhc Date DUP050467872