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UNION CARBIDE CORPORATION CHEMICALS AND PLASTICS ENGINEERING DEPARTMENT , . RECEIVED SEP 161968 R. N. Wheeler REPORT OF VISIT TO DOW'S POLYVINYL CHLORIDE PLANT PLAQUEMINE, LOUISIANA August 6, 1968 By C. E. Bowman J. H. Field W. R. Manning R, N. Wheeler (Report Prepared by W. R. Manning) September 11, 1968 SOUTH CHARLESTON WEST VIRGINIA ucc 039083 & * REPORT OF VISIT TO DOW'S POLYVINYL CHLORIDE PLANT PLAQUEMINE, LOUISIMA TABLE OF CONTENTS pa-ge INTRODUCTION.................................................................................................................................I SUMMARY AND RECOMMENDATION ..................................................................................... 2 DISCUSSION ......................................................................................................................... 3 Dow Personnel.................................................................................................................. 3 The P-S-G Bulk (Mass) Polymerization Process .................................... 3 Dow's Louisiana Division .............................................................................. 6 Labor Policy.................................................................................................................. 6 The PVC Plant Site.....................................................................................................7 Plant Facilities........................................................................................................... 8 Plant Staffing...................................................................................................................9 Plant Capacity................................................................................................................ 10 Services Available From Dow............................................................................. 12 Royalty Schedules .................................................................................................... 12 Tax Exemption................................................................................................................ 13 Pilot Plant....................................................................................................................... 13 Resin Properties and Application Areas of Interest to Dow......................................................................................................... 13 References....................................................................................................................... 15 APPENDIX.......................................................................................................................................... 16 Details of Plant Design and Layout ......................................................... 17 Table I - Polyvinyl Chloride Plant - Louisiana - Manufacturing Economic Data........................................................23 Table II - QX-38l6 Characterization Data From LAD Development LAB....................................................................................25 Table III - UCC Evaluation Data on Various P-S-G and UCC Resins......................................................................26 Table IV - Dow PVC Bottle Compounds...............................................................27 Table V - Rigid PVC Compounds - Injection Molding .... 30 Table VI - Rigid PVC Compounds- Pipe Extrusion..................................... 32 Analytical Method - Determination of Fisheyes in Polyvinyl Chloride.................................................................................................. 31* Figure 1 - Vicinity Map........................................................................................... 39 Figure 2 - Plaquemine Area .................................................................... U0 Figure 3 - Plant Layout (Dow's Plant) .................................................... Ul Figure H - PVC Plant Plot Plan......................................................................1*2 UCC 039084 REPORT OF VISIT TO DOW'S POLYVINYL CHLORIDE PLANT PLAQUEMINE, LOUISIANA August 6, 1968 INTRODUCTION Dow Chemical Company has under construction at its Louisiana Division site in Plaquemine, Louisiana, a PVC resin plant which is being offered for sale upon completion. The plant is designed to use the bulk polymerization process developed and licensed to Dow and others by Pechiney-St. Gobain (P-S-G), a French company. P-S-G is willing to guarantee a capacity of 3^ million pounds per year, whereas Dow's estimate of plant capacity is kZ million pounds per year. Dow's stated reason for offering the plant for sale is that Dow intends to go out of the PVC resin business and concentrate its efforts in vinyl chloride monomer and other business areas. The plant is estimated to be 85 percent complete. Dow intends to complete the plant this fall and is asking $5*575 million for the completed plant, including about 8.5 acres of land. On August 6, 1968, an inspection was made of this plant by the following persons, representing Vinyl Resins Operations Area 70: C. E. Bowman, Department Head J. H. Field, Operations Manager W. R, Manning, Engineering Manager R. N. Wheeler, Production Manager This report presents the data obtained and the conclusions resulting from the plant inspection and from conversations with various Dow representatives at the Plaquemine Plant. Note: Union Carbide had previously signed a secrecy agreement with P-S-G in February, 1966, under which Carbide representatives had inspected P-S-G bulk polymerization facilities in St. Fons, France, and had received disclosures concerning details of the process from P-S-G. A report of that visit is contained in Reference 1 at the end of this report. UCC 039085 -2* SUMMARY AMD RECOMMEKDATION The plant is very well laid out and well-constructed. It is evident that high quality materials and labor have been employed throughout. A high degree of automation has been provided for with high-quality, American-made instruments. Apparently a great amount of attention has been paid to safety aspects of plant design. It is our opinion that the plant will be capable of producing resin at the rate of ^2 million pounds per year, as estimated by Dow. Provision has been made in the design for ultimate expansion to four times the initial capacity. Although the plant site is bounded on all four sides by Dow property, access to a public highway and to a railroad is provided. Complete plant facilities, including distribution facilities, are available so that the plant could be operated as an independent entity. However, it would be necessary to purchase certain utilities and other services from Dow. It is recommended that Union Carbide consider the purchase of this plant from Dow, preferably at a lower price than Dow's asking price. This recommendation is made subject to the following conditions: (1) That a favorable economic position can be shown for Union Carbide to manufacture P-S-G resin in the Dow plant either for sale or for captive use by the Fibers and Fabrics Division. (2) That market area support can be obtained for the sale at attractive prices of the P-S-G resin that would not be consumed internally in UCC. (3) That a suitable licensing agreement can be worked out with P-S-G. Dow has reported that P-S-G is unwilling to simply transfer the Dow license to the purchaser of the plant. Instead, P-S-G wants to negotiate a new license agreement, reportedly with higher initial fees and higher royalties than those in the Dow agreement. UCC 039086 -3- DISCUSSION Dow Personnel The Dow representatives contacted were: Jim Means, General Manager, Louisiana Division Bud Carpenter, Manager, Chlorine Based Polymers Business Harry Gay, Business Analyst, Investment Services Fred Cossman, Production Planning, Distribution Services Emil Haas, Production Manager, Plastics A1 Paradiso, PVC Plant Superintendent Boh Huston, Research Supervisor John Barksdale, PVC Project Leader John Harvey, Industrial Relations Manager Louis Hoblett, Head of Research, Louisiana Division The P-S-G Bulk (Mass) Polymerization Process Note: Only a brief review of the P-S-G process is presented here. Additional details can be found in References 1 and 2. Little additional information over what we had previously obtained from P-S-G on the actual operation of the process was obtained from Dow, since they were unwilling to discuss operating techniques at this stage in our negotiations. The new Dow plant is designed to use the two-stage bulk polymerization process developed and licensed by Pechiney-St. Gobain, a French company. P-S-G has practiced bulk polymerization since about 19^0, and the process has undergone a gradual evolution to its present state of development. In the U. S., Hooker Chemical and B. F. Goodrich have also obtained licenses. Hooker completed a plant in the spring of 1968 at Burlington, New Jersey (reported present capacity is about 60 million pounds per year, expandable to 120 million pounds per year) and Goodrich is reported to be building a plant in the Philadelphia area, capacity unknown. In the bulk process, monomer and catalyst are reacted to approximately 10 percent conversion in a vertical, turbine-agitated reactor called a prepolymerizer or PREPO. After 10 percent conversion, the charge from the PREPO is transferred into the second-stage polymerizer, called a P0P0, where additional monomer and catalyst are added and the polymerization is continued to TO-185 percent conversion. Reaction time in the P0P0 is 8 to 10 hours. The P0P0 is a horizontal, internallyagitated autoclave especially designed to balance heat removal and agitation require ments. The agitator is designed both for liquid service (early in the reaction stage) and for agitation of a finely-divided solid powder (later stages of reaction). UCC 03908? -k- At the completion of the polymerization, the excess monomer is recovered for reuse in the process. The recovery is accomplished by venting the autoclave directly through a filter mounted on the autoclave to a water-cooled condenser followed by a propylene-cooled condenser until the autoclave pressure is reduced to about 35 psi. Stripping compressors are then used to reduce the pressure to near atmospheric. Finally, a vacuum pump is used to evacuate the polymerizer. The vacuum is broken with air and the postpolymerizer is evacuated a second time. During each evacuation, the vacuum pump discharges to the air to avoid introduction of water from the vacuum pump seal into the recovered monomer. The dry resin remaining in the autoclave is transferred by air conveyors to a finishing building where the resin is screened for packaging or bulk storage. Oversized material from the screens is ground in two stages and packaged for sale as second quality resin. There is no need for dewatering or drying, since water is not used as the processing medium. The absence of emulsifiers and colloids in the bulk process produces a resin which is reported to have the following properties and fabrication characteristics: Low gels Excellent plasticizer acceptance Excellent clarity Good bulk density Good heat and light stability Narrow particle size distribution Although the resin is produced by a non-solvent process, it is similar to homopolymer suspension resins in many respects. A simplified process flow diagram is shown on the next page. UCC 039088 -5- MA8S PVC PLANT uoc 039089 -6- Dow's Louisiana Division The facilities of Dow's Louisiana Division are located on approximately 3000 acres just north of Plaquemine and 10 miles south of Baton Rouge. (See Figures 1 and 2 at end of report.) The property is approximately bisected by Louisiana Highway 1, a four-lane concrete main state artery. Property lying east of Highway 1 fronts on the Mississippi River at two places; somewhat less than half of this property is occupied by manufacturing facilities, which comprise 11 production plants, power and steam generating facilities, a research and develop ment department, and administrative services. The property lying west of Highway 1 is largely undeveloped. The Dow plant is served by the Texas and Pacific Railroad which is part of the Missouri-Pacific system. It connects with three other railroads in the Baton Rouge area. There are also twenty truck lines operating in the Baton Rouge area, and excellent barge service for solid or liquid materials is reported to be available through leased facilities of the Port of Baton Rouge. Contract delivery service is available, providing three deliveries a day from Baton Rouge. The Louisiana Division has been operating for 10 years. It was the first chemical complex to locate on the west bank of the Mississippi River in the Baton Rouge area. The Division employs over 1000 people on its own payroll. An addi tional UoO people work in contract maintenance and service jobs, and another 900 are currently employed on construction projects. Labor Policy The Louisiana Division has no contracts with labor unions. All division employees are classified as salaried personnel, which allows the division to operate with a single set of policies and practices for all employees. This program was established at the beginning of the division's operations in 1958. Dow has been well pleased with this policy, and is very interested in maintaining it. They would strongly encourage the purchaser of the PVC plant to operate on this basis also, and they are willing to furnish advice and assistance in setting up this type of operation. Among the advantages claimed are: company identification rather than union identification, greater flexibility in work UCC 039090 -7- assignments, performance of maximum amount of maintenance work by operators, minimum jurisdictional problems, individual consideration, elimination of negotiations and strike threats or work stoppages. They reported that union people work (on contract) alongside their own salaried people with very few problems. According to Dow, several other companies in the area have the same type of labor policy, including Monochem, Borden, U. S. Rubber, Rubicon Gulf Oil, and Hercules. Dow reported the labor supply and quality to be good. This seems to be at variance with reports in recent literature of considerable labor strife in the vicinity of Baton Rouge. However, most of the trouble may be with construction workers; rather than with operating and maintenance people. Dow regarded the presence of Louisiana State University in nearby Baton Rouge as a definite asset, stating that many people with one to four years of college education are available for operating technician positions. The PVC Plant Site The PVC plant is located on about 8.56 acres in the northeast corner of the Dow property (see Figure 3). Dow proposed to fence off this property on all four sides, leaving it entirely surrounded by Dow property except for an asphalt access road to Highway 988 -- locally referred to as the River Road. River Road provides access to Louisiana Highway 1 by two different routes -- Louisiana Highway IIU3 to the south and Addis Lane to the north. All of these roads are two-lane, hard-surfaced roads. Dow has recently acquired, at a reportedly high price, about 15 acres of property to the north of the PVC plant site. This property is now occupied by several small residences. When questioned about the availability of this land to the purchaser of the PVC plant, Dow personnel indicated that they would be reluctant to part with any of this property. Growth would not be encouraged at the PVC plant site, beyond the planned expansion of the PVC plant itself to about four times present capacity. They were willing to consider selling or leasing some of the property west of Highway 1, if the PVC plant purchaser vanted additional land for auxiliary operations or expansion. UCC 039091 -8- They also indicated that access to the river from the PVC plant site would he strictly limited. They said that some usage of their dock, located about 1500 feet downstream of the PVC plant site, might be permitted for bringing in liquid materials, but that extensive use of their dock would not be encouraged. The PVC plant site is served by a railroad spur that passes through Dow property. The PVC plant would therefore be dependent on the use of Dow's spur for car-switching service. Two switches are made on week days, but none on Sunday. Plant Facilities As a result of our inspection of the Dow resin plant, we have concluded that it will be a complete unit capable of being operated independently and safely. It would be necessary to purchase some services from Dow and perhaps to have some functions, such as accounting and other office services, performed at our Taft plant. The general quality of engineering, materials, and workmanship in the plant appeared to be excellent. The equipment arrangement was spacious, and a great deal of attention had been devoted to safety considerations in plant design. The following is a summary listing of what is included in the plant. For additional details, please refer to the appendix section "Plant Layout and Design." The layout of the plant is shown on Figure 4. The plant includes: (1) Office, laboratory, and control room building with locker room, showers, and instrument shop. (2) Polymerization structure housing one prepolymerizer and four postpolymerizers -- easily expandable to double capacity. (3) Monomer storage facilities and recovery equipment. (H) Finishing structure for screening and transferring resin, with trans fer systems capable of handling double the present polymerization capacity. (5) Warehouse and bag, drum, or box packaging station. (6) Bulk silos and bulk car or truck loading stations. (7) Catalyst storage building. ucc 039092 -9- (8) Motor control building and air compressor. (9) All needed utility supply lines except a power line from Gulf States Utility Corp. facilities to the PVC plant. Dow had planned for three major products, with 30 percent of the total production to be distributed in bags and 70 percent in rail hopper aars or in hopper trucks. A possible problem that Dow apparently is not aware of and has not provided for is residual vinyl chloride in the resin. Hooker has had this problem with the product from a P-S-G resin plant. P-S-G apparently has not had a problem, possibly because of aeration of the resin in the homogenizing silos emplbyed by P-S-G for bulk resin storage and blending. Plant Staffing The staffing of the plant that Dow had planned is as follows: 1 - Superintendent 1 - Assistant Superintendent 1 - Quality Control Supervisor 1 - Operations Supervisor 4 - Shift Supervisors 4 - Control Board Operators 3 - Vacation and Overtime Relief Operators 4 - Reactor Operators 4 - Finishing Operators 4 - Utility Operators 5 - Quality Control Technicians 1 - Clerical 8 - Reactor Cleaners 2 - Packagers 1 - Janitor 44 - Total For the doubled plant, Dow planned to add 4 reactor cleaners only. We believe that the plant could have been designed for operation with fewer people, but with the existing layout, little reduction in staffing appears to be possible. ucc 039093 -10- Plant Capacity The plant capacity that would now be guaranteed by P-S-G is 34 million pounds per year of a resin of K value = 65 (K value is a measure of molecular weight). This is increased over an initially guaranteed capacity of 30 million pounds per year because of the addition of external condensers to the prepolymerizer and the postpolymerizers. However, Dow's production objective in the initial plant is 42 million pounds per year. We believe the plant will achieve this capacity. To reach this capacity, Dow has incorporated a number of modifications to the basic P-S-G design, such as larger monomer charging lines, larger autoclave discharge lines, more remotely operated valves, spare filters in the autoclave degassing system, quick-opening manheads on the autoclaves, and extensive use of Hamer Line Blinds to permit operators, rather than maintenance workers to blank lines. Also, the entire resin finishing, transfer, and storage system was designed by Dow to have a capacity of 84 million pounds per year. The plant can be easily expanded in several different ways. Addition of one prepolymerizer and four postpolymerizers (simply doubling what is there now) would double the polymerization capacity. Dow estimated that this could be done for $2,500,000. P-S-G now states that one prepolymerizer and three .postpolymerizers are capable of producing about 34 million pounds per year. Thus, addition of one prepolymerizer and two postpolymerizers would provide a total capacity of 68 million pounds per year. Dow estimated that this addition would cost $1,800,000. Dow indicated that the instrumentation had been arranged so that the postpolymerizers could be easily operated as two groups of three. A third alternative would be to add two prepolymerizers and five postpolymerizers to achieve a polymerization capacity (based on P-S-G's guarantee) of 102 million pounds per year. Dow did not provide an estimate for the cost of this alternative, but it would apparently result in the lowest total investment per annual pound of capacity of any of the three methods considered. The variation of plant capacity with the K-value of the resin is illus trated by the graph on the next page. Following is a summary comparison of Dow's capacity objectives with the capacity guaranteed by P-S-G: Plant Capacity (MM Lb/Yr -K = 65) Existing Plant First Expansion Ultimate Dow Objective Guaranteed by P-S-G k2 84 168 34 68 136 UCC 039094 -11MASS PVC CAPACITY -12- Services Available From Dow Dow would supply vinyl chloride monomer from the Plaquemine plant "across the fence," under our existing contract. Dow would also provide steam, potable water, nitrogen, fire protection and emergency services, and railroad spurs for switching service. Fees for these services, as well as other economic data provided by Dow, are tabulated in Table I in the Appendix. Dow is willing to provide, for a fee, consultation on its salaried operations and contract maintenance programs, as well as on such items as local and state tax structure and procedures, prevailing business and political climates, public relations, training, employee benefits, safety, and state statutes regarding waste disposal and the procedures for obtaining waste disposal permits. Royalty Schedules Dow indicated that negotiations with P-S-G were still in progress regarding the terms of Dow's settlement with P-S-G. P-S-G apparently will not permit the purchaser of the plant to assume the licensing arrangement that Dow has but wants to negotiate a new licensing agreement. The fees have been increased, as shown by the following comparison of the fees quoted to UCC by P-S-G in June, 1966, with those reported unofficially by Dow as being asked now by P-S-G: Initial Fee Running Royalty for Ten Years 1 Quoted to UCC By P-S-G June, 1966 $240,000 k% on First $3,500,000 of Annual Sales and Usage 3% on Next $5,000,000 Sales and Usage 2% on Balance Unofficially Reported By Dow August, 1968______ $1*00,000 h% on First $1*,000,000 of Annual Sales and Usage 3% on Next $6,000,000 Sales and Usage 2% on Balance The initial fee includes process documents, personnel training, and startup help. -13- Dow's reported fee schedule was very nearly the same as that quoted to UCC in 1966. Dow's agreement provided for feedback to P-S-G of developments put in production by Dow, but other licensees could not use Dow developments without paying royalty to Dow. Copolymers were not included in the Dow agreement, and so far as is known, the P-S-G process has not yet been developed to produce copolymers. However, P-S-G believes that the process can be developed to produce copolymers. Tax Exemption A ten-year tax exemption has been granted to Dow by the State of Louisiana for the PVC plant. However, this exemption would be cancelled if the plant is sold, and the new owner would have to make a new application. Pilot Plant Dow has operated a pilot plant on the P-S-G process for the stated purposes of increasing plant capacity, developing product variations, and possibly finding new and patentable developments. This pilot plant is not on the PVC plant site and is not included in the sale of the PVC plant. However, Dow indi cated willingness to negotiate its sale if the purchaser of the plant wanted it. The major equipment in the pilot plant consists of a 25-gallon singlestage polymerizer, a 100-gallon prepolymerizer, and a 200-gallon postpolymerizer, all of which are vertical vessels. Resin Properties and Application Areas of Interest to Dow Dow stated that it was the superior resin properties of the P-S-G resin as compared with suspension resins, rather than economics, that attracted their attention. At best, they expected the P-S-G resins to be no more than 10 percent cheaper than suspension resins, because the inherent advantage of the simpler process is largely offset by the initial fee and the royalty to P-S-G. Evaluation data presented by Dow are tabulated in Table II in the Appendix. (Dow's method of determining fisheyes in PVC is included in the Appendix.) UCC 039097 -14- Evaluation data obtained in UCC labs on resin supplied by P-S-G and by Hooker, together with data on two typical UCC suspension resins, are tabulated in Table III. Applications areas of principal interest to Dow were: bottles, clear film and sheet -- both rigid and flexible, and pipe and conduit. It is worth noting that these areas all permit the use of low-molecular weight resins, for which the Dow plant would have high productivity. Areas of secondary interest to Dow were: spread coating of metal, fluid bed coating, and phonograph records. Not much applications development work had been done in these areas, and not much data had been accumulated. All of Dow's compounding technology that applies to P-S-G resin would be included with the sale of the plant. Dow has developed compounds (both pellet and powder blend) for blow molding, injection molding, and sheet and profile extrusion, involving both FDA and non-FDA applications. Dow has also developed powder-blend PVC pipe compounds, which have been approved for potable water use by the Plastics Pipe Institute and the National Sanitation Foundation. Also available are compounds for drain, waste, and vent piping. (See Tables IV through VI in the Appendix for data on Dow's compounds.) Dow believes that P-S-G resins may be good extenders for dispersion resins but has done little work in this area. In comparison with suspension resins, Dow hoped to get a price premium of somewhat less than one cent per pound for resin for bottles but expected no premium for resin for pipe. On compounds, they hoped to get a premium of one cent or more over compounds of suspension resin. UCC 039083 -15References (1) Evaluation of Pechiney-St. Gobain's Bulk Polyvinyl Chloride Process, August 3, 1966, by F. E. Bailey, W. R. Manning, and M. E. Sutherland. (2) Memorandum, dated November 8, 1966 -- Revisions and Additions to Report: "Evaluation of Pechiney-Saint Gobain's Bulk Polyvinyl Chloride Process," dated August 3, 1966,'by W. 3. Lanier. (3) Polyvinyl Chloride Plant -- Louisiana, by Dow Chemical Company (Plant Sale Brochure) (U) Economic Evaluation of the Acquisition of Pechiney-St- Gobain Process FVC Resin Plant From Dow Chemical Company, September 12, 1968, by R. W. Brown and W. R. Manning. ucc 039099 -16- APPENDIX ucc 039100 -17- Details of Plant Layout and Design The layout of the plant is shown in Figure H. The plant includes: (l) Office, Laboratory, And Control Room Building With Locker Room, Showers, and Instrument Shop. (Building 951 on plot plan). This building is a one-story building of concrete block construction, painted inside and outside; approximate dimensions are TO feet by 80 feet; it is completely air-conditioned. The front part of the building (west) comprises a receptionist area, a conference room, six offices (approximately 10 feet by 12 feet), and a hall running the width of the building. The receptionist area, the offices, and conference room are attractively furnished. The rear part of the building is occupied by the quality control laboratory (north, approximately 20 feet by Uo feet), the control room (center, approximately 25 feet by Uo feet), and instrument shop, locker rooms, and rest rooms (south). The quality control laboratory was equipped with a Brabender Plasticorder and a two-roll mill in addition to the usual plastic laboratory equipment. The control room is well arranged. All instruments are of American manufacture and are mounted on metal panel boards or housed in metal cabinets. In most cases, action is a combination of pneumatic and electric - sensing signals are transmitted pneumatically and control-activating signals are transmitted electrically. Pneumatic instrument leads are of plastic and all leads are mounted in metal troughs. A high degree of automation is apparent, especially in the polymerization process. Step switches with manual interrupt and visual display are provided for automatic sequencing of the charging, polymerization, monomer recovery, and autoclave discharging operations. The progress of the reactions is followed by means of Btu meters. The instrument shop is approximately 12 feet by 12 feet; it was not furnished at the time of our visit. The locker and shower room had obviously been designed for easy maintenance, with painted walls, terrazzo floors, and ceramic tile in the shower stalls. UCC 039101 -18- (2) Polymerization Structure Housing One Prepolymerizer and Pour Postpolymerizers, Easily Expandable To Double Capacity. The polymerization structure is of open steel construction with roof. Overall dimensions are about JO feet by 110 feet. It is 5 bays long, 3 bays wide, and 3 stories high, except for a center section which is 4 stories high. Mounted above the partial roof of the center section is a monorail (to be used for removing the agitator from the prepolymerizer or the prepolymerizer itself), and support steel for vent piping. The four postpolymerizers are located at ground level in two adjacent bays (west side) at each end of the polymerization structure. These vessels are horizontal, stainless-steel clad, 4200-gallon-capacity autoclaves, designed for 225 psig or 650 mm Hg, and equipped with specially designed agitators. The post polymerizers and their agitators were made in France. They are mounted on large concrete pads which in turn are mounted on load cells for automatic weighing. The agitators are driven by 40-80 HP two-speed motors through Lufkin gear boxes. The single prepolymerizer is mounted to hang through the second level of steel, and is centrally located with respect to the four postpolymerizers. It is a vertical, stainless-steel clad, 1850gallon-capacity autoclave, equipped with a Lightning agitator. The prepolymerizer was also made in France. The prepolymerizer and the four postpolymerizers are all equipped with external condensers to increase the capacity for heat removal. The use of condensers is a recent development in the P-S-G process, and may actually have been suggested to P-S-G by Dow. Monomer recovery equipment included in the polymerization structure includes one Sulzer recovery compressor (a vertical, 2-cylinder machine made in Switzerland) with 100 HP Allis-Chalmers drive, one Nash Hytor vacuum pump of 500 cfm capacity, and several filters in the degassing system. The compressor, vacuum pump, and associated filters are located at ground level in two bays on the southeast corner of the polymerization structure. UCC 039102 -19- Safety features included in the polymerization area include an open deluge system with automatic and remote manual activation, open building construction, vinyl chloride detectors and alarms. Class I, Division I, Group D code construction for all electrical equipment, lockouts on agitators, automatic valves, remote control room (100 feet), and reactor vents 20 feet above highest roof. Generous use has been made of Hamer Line Blinds in the polymerization area to permit operators to blank lines without calling on pipefitters. Dow indicated that cleaning of the polymerization vessels was expected to be a major problem. This is contrary to what we were led to believe by P-S-G, who indicated that cleaning was relatively easy. Dow estimated that the prepolymerizer would have to be cleaned every fourth run, and the postpolymerizers after every run. Estimated cleaning time for two men was two hours for a postpolymizer, about ^0 minutes for a prepolymerizer. (3) Monomer Storage Facilities and Recovery Equipment. The monomer storage and recovery facilities (other than the compressors mentioned above) are located in a two-level, 25 foot by 50 foot open steel structure at the southeast corner of the plant site. This area is identified on the plot plan as "Day Tank." The monomer storage tank is located at ground level and is a IT ,000-gallon steel tank, lined with a zinc silicate coating. (Dow personnel indicated that they had used this type of coating with good success in vinyl chloride tanks for about seven years.) Mounted above the storage tank on the first level of steel were a water-cooled condenser and a vent condenser cooled by a packaged propylene refrigeration system. Provision was made to circulate all recovered monomer through one of two small tanks filled with solid caustic for neutralizing free hydrogen chloride. New and recovered vinyl chloride was transferred from the storage tank to the polymerization area by means of a pump. Safety features included in this area included an open deluge system with automatic and remote manual activation, open type construction, and electrical equipment of Class I, Division II, Group D code construction. IJCr 039103 -20- (U) Resin Finishing Structure. The finishing structure is an 18 foot by 55 foot open steel structure approximately 70 feet high, comprising 5 operating levels. It contains a 200 HP Hofflnan vacuum system with a Young Unicage baghouse for transferring resin from the autoclaves to quarantine storage bins; 2 Sweco scalping screens, 2 Derrick finishing screens (10 feet by 12 feet, 2 compartments, 3-layered stainless steel screens); 1 Young knife-mill grinder; 1 Schutz-O'Neil mill with water-cooled jacket; grate magnets; automatic samplers; 1 Semco pressure-pot dense-phase resin transfer system with Porushair inlet air filter elements (system designed by Semco Engineers of Houston); and a freight elevator to the fourth level to carry off-grade resin in bags to a dump-back port for reprocessing. South of the finishing structure are two quarantine bins, 600 cubic feet, epoxy-lined steel, 9 feet diameter by 7 feet straight side, with 6o conical bottoms. North of the structure are two first-quality resin storage bins, 1300 cubic feet, epoxy-lined steel, 11 feet diameter by 10 feet straight side, with conical bottoms. (5) Warehouse and Bag, Drum, or Box Packaging Station. The warehouse, identified on the plot plan as "Bagging and Shipping - 95^," is a 50 foot by 100 foot, one-story Builer-type building with steel framing and PVC side paneling. The building is built on a concrete pad. On the west side is a depressed driveway and loading dock with space for two trailer trucks. Inside the building at the north end is a three-tube bag packaging machine, with automatic check-weigh scales and take-away conveyor. No provision is made for automatic palletizing, and bagged resin storage space is quite limited. Dow planned to bag resin on day shift only, and to haul bagged resin every day to a warehouse outside the plant. No provision was made to load bagged resin into railroad cars. Dow also planned to have a maintenance shop occupying about onethird of the warehouse building. ucc 039104 -21- Two medium-sized bins, located above the roof of the warehouse at the north end, supply resin to the bagging machine and for loading into hopper trucks. (6) Bulk Silos and Bulk Car Loading Station. Bulk resin storage is provided by four 500,000-pound storage silos. These are 21.5 foot diameter by 67 feet high, epoxy-lined steel tanks with conical bottoms. Resin .blending is accomplished in a 160,000-pound gravity blending bin incorporating a Flotronics blending system. This system consists of a series of vertical standpipes inside the bin with holes at various levels to allow resin to flow inside the standpipes and be discharged at the bottom. A 200 HP Hoffman vacuum resin transfer system is employed to move the resin from the finishing area to the bulk storage bins and from the bulk storage bins to the blending bin. A Semco dense-phase resin transfer system is used to move the resin to the bulk car loading station. A single railroad hopper car loading station is provided. The resin discharge line at this station is equipped with several Chicsan pipe joints which enable discharge of resin into any one of six openings in a hopper car. Provision is also made for unloading hopper cars back to resin storage. (7) Catalyst Storage Building. Catalyst storage is provided in a separate walk-in building identified as "956" on the plot plan. This is a 12 foot by 20 foot building with stainless steel panels inside and out, insulated with several inches of styrofoam between the panels. Two refrigeration machines, each capable of maintaining the required temperature (around 0C) are provided. The building is shielded on the south and west sides from the rest of the plant by concrete walls about one foot thick and eight feet high. UCC 039105 -22- (8) Motor Control Building and Air Compressor. The building, identified on the plot plan as "953-MCC" is a 20 foot by 30 foot, one-story building housing motor control equipment. The area north of the motor control building, identified as "Utilities" comprises an air compressor and two Oriad air dryers. The compressor is a 3-stage centrifugal compressor, 2600 cfm at 100 psig, made by Joy Manufacturing Company, driven by a 500 HP, 3580 RPM electric motor. This compressor supplies process air, instrument air, and air for three Semco resin transfer systems. (9) Utility Supplies. Cooling Water - A ^20-foot-deep water well is located between the control room and Polymerization Area No. 1. This well supplies 3500 gpm of water for process cooling on a once-through basis. Temperature of the water was said to be 72F - 1F all year round. Electricity - Dow prefers that the new owner of the PVC plant negotiate a separate contract with Gulf States Utility Corp. for electric power. However, the plant is now tied into the Dow electric power system, and Dow proposes to leave this tie-in intact, so that the PVC plant can receive emergency power from Dow if necessary. Steam and Condensate - Steam would be available from Dow through an existing 235-psi line. There is no provision for condensate return. Nitrogen - Dow could supply nitrogen from a Linde plant now being installed nearby. Potable Water - Dow could supply from their existing system. Natural Gas - This is not required for operation of the PVC plant, but both Humble and Texaco have pipelines available near the Dow plant, if natural gas should be needed in the future. Water for Firefighting - Water for the deluge systems would be available from Dow'3 emergency water system. Waste Disposal - For a fee, Dow would permit the use of their drainage canals for cooling water and of their sewer system for sanitary waste disposal. uce 039106 -23- TABLE I POLYVINYL CHLORIDE PLANT - LOUISIANA Manufacturing Economic Data^^ (350 Days/Year - 2k Hours/Day Operation) 1. Raw Material* One Train 30MM #/Yr, v Units/# PVC1 ` Two Trains 60MM #/Yr Units/# PVC Vinyl Chloride Monomer Catalyst & Chemical Nitrogen 1.05 .lUU ftVlb 1.05 .144 ft3/lb 2. Utilities* 235# Steam Motor Power - kwh Water - gal. (Drinking Water) 3. Maintenance* .44 lh/lb .4 .033 .44 lb/lb .4 .033 Maintenance Labor Shop Services Maintenance Material Contractor's Services 4. Taxes* 5. Insurance* 6. Manpower* Supervisory & Technical Skilled Operators Laboratory & Clerical Non-skilled *Refer to following pages for further detail. 8 19 6 11 8 19 6 15 Notes: (l) These data were supplied by Dow on August 6, 1968. (2) Basis is pounds of salable first- and second-quality resin (92-94$ first quality; 6--8^ second quality). UCC U39107 TABLE I (c ontinued) Raw Materials Vinyl Chloride Monomer Catalyst & Chemicals Nitrogen - Price of monomer - use unit price as stated under existing contract with Dow. - Currently estimated to cost $.002-$.003 per pound of PVC produced. - $2.80/MCF one train; $2.10/MCF two trains Utilities (approximate current public utilities rates) 235# Steam & Condensate - $ .85/M# Motor Power - $ .0120/kwh (one train); $ .0089/kwh (two trains) Water - $1.0Q/M gal. (drinking water) Maintenance - For all items listed on preceding page - estimated cost per year $250M (one train) and $370M (two trains) = 5% of Capital Investment. Taxes - Dow has a property tax exemption on its manufacturing facilities at its Louisiana Division. Inventory, land and certain non-production facilities are, however, subject to property taxation. The Purchaser of the PVC facility should file a separate application for property tax exemption. The Louisiana Division Administrative Services will assist in an advisory and counseling capacity to obtain a tax exemption. Insurance - Assuming $5000M is the insurable value, the insurance cost is estimated to be $12M to $15M per year ($.25 to $.30 per hundred of insurable value). These estimated premiums might be higher or lower dependent upon results of negotiations with given underwriters. Manpower - For economic purposes/studies, use wage and salary figures on pages 18-19 in the general brochure. Depreciation, Factory Expense, R & D, Selling and Administrative Expenses Subject to purchaser's internal accounting practices. The Louisiana Division can provide supporting services at the following estimated cost per year: a) Emergency fire water, fire truck, ambulance b) Water disposal, coolant water c) Railroad switching ($20/car) d) Consulting services (taxes, industrial relations, etc.) $25,000 $25,000 $ 7,000 pc co :-{ -A"> ) o CO Tadlc 0X-3SI6 CHARACTERIZATION DATA FRCM UP-PEVCLOFMCHT UP (Data Supplied by Dow, August 6, 1968) J- V' 1 -V $! vi c 1 QX No 3S16.1 1 X< ASTM ASTM ASTM ASTM ASTM ASTM tfl 01243 01095 01895 /UK 7 (5t~X 01755 (o/cc\| g/cc XEc/lOO |s[c/lO<}\ PPH CC 1-17D 0.565' 0.592 7.5 H.F. 0.415 69 $0tC 3Sie-2 1-17 .666 .586 213032 -- .594 6.4 N-F, 6.1 7.1 .432 .491 69 1-17 .795 .600 6.1 10. 1 .534 77 5462 .89 1-17 .845 .535 .489 6.4 7.6 6.0 N.F. .486 .413 115 \\\Q 3916.5, 8694 .91 86943 .92 1-17 -I-I73 .934 L100 .955* L1003 .925 L101 .90S L1013 .920 ,561 .567 .564 .567 .551 .554 .554 .553 7.4 7,7 7.2 7.2 9.0 8.6 8.5 6. 5 9.0 N.F. N.F. N.F. 8.3 8. 1 7.7 0.2 .406 .504 .496 .499 .541 .544 .546 .546 03 85 87 90 69 90 91 foz -- 513034 .99 1-17 -1-173 .996' LlOl ,966 flOg .99Q .482 .497 .504 .501 .471 -- 6.9 7.5 7.6 6.0 8.5 -- 9.0 9.4 10.2 9.8 14.7 -- .409 .444 .461 .464 .430 119 120 122 06465 1 .11 1-17 1 . 133 .479 .493 6.9 8.3 6.4 9. 1 .423 .460 121 1-17 1 .297 .465 9.2 N.F. *406 113 ASTM Dow Tenta- Tl VE Vo Ml N, /i 2 5.0 B 5.2 0 -- A 5,0 -2.7 -3.0 3.3 3.3 2.3 2.7 2.7 2.7 --- 2,0 2.2 2.9 -- 9 A 8 A A, 8 A B 0 A B C A a B B 2.6 4,3 0 1-17 0.675 1-17 .049 1-17 *097 1-17 1 .02 1-17 1 .063 1-17 1 .296 1-17 0 .646 1-17 .035 1-17 .OCO .568 .505 .512 .408 .440 ,449 N.F. N.F. N.F. It. 1 N.F. 10. 1 N.F. N.F. N.F. N.f. N.F. N.F. .399 .366 .420 .414 .363 .4: 93 74 92-97 100 100 123 -- 4,0 3.7 3.2 3.7 NDU B 0 0 C E .561 .476 .462 0.0 9.3 9.0 N.F N.F, N.F.. ,419 .399 .420 00 105 103 -- 4.0 3,4 E E . ----------------- LAO-D-1 -- Screen Analysis- +50 +70 +100 +140 +230 -230 0.0 0 .5 .4 .2 0 WT. % ON SCREEN , MESH SIZE ADOVE \ 3 83 97 0.2 8 1.2 2 91 95 97 100 5 0 .6 75 95 95 >e9,T .3 10 100 0 0 .2 36 a? 92 8 1----- LAD-0-2 -- Mrll Gel /i 3 4 567 f Jo. or cel* l r. Vi T r E. t - : , r >50 -- --- >50 2 - - -- __ 25 2 -- -- >50 0 -- .. -- c. iO C. 07 0.00 .2 0 .2 .4 , .2 .2 .2 .4 .2 .4 2 1 0.6 1 11 0 9 10 15 16 17 69 93 7 -- e 2 -- 91 95 5 72 89 95 5 -- 13 0 -- -- 79 97 3 >100 25 2 80 98 84 98 2 -- 13 0 -- -- 2 16 0 __ 83 97 3 -- 15 0 -- 0. 16 . 10 __ . 13 -- . . 16 ... . 12 -- . 13 .2 .6 20 .2 .6 .2 1 .2 0.6 2 2 100 100 80 97 81 95 79 95 0 3 > 25 1 5 >100 4 56 0 1 -- -- . 15 -- . 15 .2 .5 7 .2 .2 5 .2 .8 10 , 2 .4 7 .6 2,6 14 .4 2.2 6 .4 6 10 .6 7 27 93 6 0 > 25 0 .23 91 95 5 25 0 .Cl. 56 759 10 62 87 10 .05 32 64 36 62 87 13 -- >100 1 . 10 65 65 15 61 . 13 61 77 23 62 . 11 80 90 10 10 1 . 10 .6 7 .2 3 1.6 11 42 72 94 5 10 45 63 90 26 * 86 90 10 -- -- -- >.0 >`.o . 13 . 14 . 19 TABLE III UCC EVALUATION DATA ON VARIOUS P-S-G AMD UCC RESIMS Supplied to Hooker by P. S. G. B-34s General TeatReain Inherent Viacoaity Heating Loss Apparent Denajty Contamination Plaaticiser Sorbtion ICMT 2.0 Min. Holding Power 30 Min. Hcddlng Power Flnol-10-10 Dry Blend Tim Flexol-13-13 Dry Blend Time Volume Reaiativity Dry Reain Flow H.R.P. - 10 Mil % thru 200 meih Median Particle Size 1.03 32 * 106 99 80 3.8 5.7 * __ 14 2.4 116 B- 34 SHPX47104 1.001 0. 56 33 2/25 103 113 93 94 3.7 5.9 69 4.9 10 3.6 92 Produced By Hooker B-34 SHPX53544 1.006 0. 44 34 3/73 105 111 97 62 B-34 #3 0. 993 0. 58 33 5/22 98 105 99 85 B-34 SHPX60760 0. 996 0. 39 33 4/32 100 103 100 91 4.3 4.3 4.5 7.3 6. 5 6. 5 74 82 59 4.4 5.0 4. 5 15 8 6 7.8 7. 1 11.7 86 92 85 B-34 TLDX87 1.027 0. 36 33 2/15 111 99 76 3.8 7.4 75 6.0 1 5.9 98 Produced in France Evaluated Mar. -1966 B-38 Hooker 1.08 0. 1 30 2/7 113 101 100 91 4.7 -- -- 3.2 6 2 125 P.S.G. GB12I0 0.97 0.2 31 -104 no 90 -- 4. 5 .. -4.0 75 5 120 P.S.G. GB1510 1. 10 0. 1 33 -102 121 97 -- 5.3 QYTQ-7 Tvolcal 1.0 0. 1 31 3/30 90 MR 93 70 (unmodified! 7.0 QSAN-7 Typical 1.03 0. 1 31 3/30 90 107 93 .72 5.6 -- -- -- -- 35 (mawM 80 (d 4.4 3.5 3.8 60 25 25 41 1 122 150 140 ro Ot ' (*) Contaminated with dirt at Bound Brook (F fc F), unable to evaluate. (1) Slurry rating/ayntron apeck count. (2) Percent of atandard (Eacambia-1225). (3) Standard teat reain from Pechiney St. Gobain - France. SC: So O -27- TABLE IV Dow PVC Bottle Compounds (Data Supplied by Dow, August 6, 1968) Dow PVC bottle compounds utilize FVC resin manufactured by the mass (or bulk) process. Because of the purity, lack of gels, and high stability of the low viscosity mass resin, MX-38l6*2, Dow's calcium-zinc stabilized bottle compound, MX-3785 *15, has received acclaim from all of the major PVC bottle processors in the United States. The same can be said for Dow's non-food grade PVC bottle compounds, in that the low viscosity mass resin used allows easier processing with gelfree, high clarity bottles as the end-product. In addition to the advantages of using the mass resins, Dow's PVC bottle compounds have unique lubrication systems which allow no sticking and subsequent burning in the extruder and yield bottles with surface gloss and clarity barely distinquishable from glass. These compounds, both food and non-food grades, have been proven on many different types of PVC bottle blowing equipment with extruders rang ing in size from 2? to Inches in barrel diameter. I 039111 -28TABLE IV (Continued) DOW PVC BOTTLE COMPOUNDS (Mass PVC Resin Only) (Data Supplied by Dow, August6^1968) MX-3785.12 Non-FDA, high impact, low viscosity MX-3785.13 Non-FDA, high impact, med. viscosity MX-3785.1^ Non-FDA, high impact, high viscosity MX-3785.15 FDA (Ca-Zn), high impact, low viscosity MX-3785.16 FDA (octyl tin), high impact, high viscosity MX-3785.17 Non-FDA, high impact, low viscosity, no dye, for in-house pigmenting MX-3785.18 FDA (octyl tin), high impact, low viscosity ucc 039112 039113 TABLE IV (Continued) PROPERTIES OF DOW PVC BOTTLE COMPOUNDS (Dada Supplied By Dow, August 6, 1968) MX-3785.12 MX-3785.13 Light Transmission (50 mil specimen) 85$ 85# Haze (50 mil specimen) 5# 5% Bottle Drop Impact (13^ oz. 27 gram, Boston Round) 50# failure height 8 ft. 8.5 ft. Heat Distortion (264 psi. load) 66C 66C Brabender Equilibrium Torque (#5 roller head, 60 gram charge, 60 rpm., 170C Jacket) 2200 mg. 2500 mg. Specific Gravity 1.33 1.3^ MX-3785.1^ 85# 5% 10 ft. 64 C 2700 mg. 1.34 MX-3785.15 MX-3785.16 83# 6% 85% 5$ 7 ft. 62C 9 ft 66 c 2700 mg. 1.33 2600 mg, ro 1.35 ? -30- TABLE V RIGID PVC COMPOUNDS MX-3693.0 INJECTION MOLDING (Data Supplied by Dow, August &, 1968) With the inherent soap and suspending agent ingredients in conventional PVC, it has been virtually impossible to challenge the polystyrene and styrene/acrylonitrile materials on a clarity basis even though the self-extinguishing characteristics of PVC were most desirable. This compound, based on mass polymerized PVC,-which does not have the handicap of residual suspending agents-can truly be claimed to be ultra clear and thus replace the styrene and/or acrylic based materials where self-extin guishing characteristics and impact are desirable. This material is also suitable for profile extrusion. Physical Properties Tensile strength psi Tensile modulus psi Flexural strength psi Flexural modulus psi Notched izod impact ft. lbs. Heat deflection temperature @ 264 psi - annealed Light transmission % Haze # Flammability Shrinkage in./inch Specific gravity 7,200 410,000 12,500 420,000 1.5 165 F 85-90 3.5-5 S.E. .004-.006 1.38 ASTM D638 D638 D790 D790 D256 d648 D1003 D1003 D635 dfw UCC 039114 -31- TABLB V (Continued) RIGID FVC COMPOUNDS INJECTION MOLDING MX-3693.1 (Data Supplied by Dow, August 6, 1968) This compound can be classed as general purpose, having medium Impact and heat distortion characteristics. It is also being used in the profile extrusion area. Physical Properties Tensile strength psi Tensile modulus psi Flexural strength psi Flexural modulus psi Notched izod Impact ft. lbs. Heat deflection temperature @ 264 psi - annealed Flammability Shrinkage in./inch Specific gravity 7,200 410,000 12,500 420,000 1.5 ,l65*F S.E. .004-.006 1.38 ASTM D638 D638 D790 D790 D256 D648 d635 MX-3693.2 This material is an ultraviolet stabilized version of MX-3693.0. The clarity properties closely resemble those of the ultra clear MX-3&93-0. No discoloration was observed after 1500 hours in a rotating drum, UV test apparatus. dfw ucc 039)15 -32- TABLE VI RIGID FVC COMPOUNDS PIPE EXTRUSION (Data Supplied by Dow, August 6, 1968) The following compounds are listed by the Plastics Pipe Institute and National Sanitation Foundation as Type 1 Grade 1 with a hy drostatic design stress of 2000 psi. They are designed for use in dry blend form and yield high output rates on conventional equipment. MX-3968.8 is classed as intermediate impact being between a Type I and a Type II in this respect. All materials listed sur pass minimum requirements of ASTM D-1784. Properties mx-3968.3 MX-3968.4 MX-3968-5 MX-3968.8 Form Dry Non-Dusting Powders Specific gravity Bulk density g/cc Tensile strength psi Tensile modulus psi Flexural strength psi Deflection temperature @ 264 psi - annealed Notched izod impact ft. lbs. Flammability 1.39 0.50 7,250 430,000 12,500 72C 0.85 S.E. 1.39 0.64 7,400 430,000 12,500 70C 0.75 S.E. 1.3? 0.64 4,300 415,000 12,500 70*0 1.0 S.E. 1.39 0.60 7,200 415,000 12,500 71C 2.4 S.E. dfw -33- TABLE VI (Continued) RIGID PVC COMPOUNDS MX-3968.7 PIPE EXTRUSION (Data Supplied by Dow, August 6, 1968) Drain Waste and Vent Applications MX-3968.7 is a lead stabilized, dry blend material, listed by the National Sanitation Foundation as meeting the physical requirements for DWV applications. The lubrication system is designed so as to have high output rates over a wide range of condit ions. Physical Properties ASTM Flexural strength psi Tensile strength psi Tensile modulus psi Notched izod impact ft. lbs. Heat deflection temperature @ 264 psi - annealed Bulk density g/cc 12,400 7,250 430,000 1.1 76 C 0.56 D030 D638 D256 d648 dfw THE DOW CHEMICAL COMPANY ANALYTICAL LOUISIANA DIVISION PLAQUEMINE, LOUISIANA 70764 504 667-432 This \% a file copy. For Outtide Distribution Obtoin Copies With liability Clouse METHOD and Without Dow Reference. (Data Supplied by Dow, August 6,- 1968) February 10, 1967 LAD-AM-67.2 DETERMINATION OF FISHEYES IN POLYVINYL CHLORIDE 1. Scope This method describes the measurement of the intermolecular action between polyvinyl chloride and plasticizer in the fully gelled compound with respect to the appearance of extraneous, not easily processed particles (fisheyes), and their rate of elimination with milling time. 2. Safety Precautions Only experienced personnel should operate the mill referred to in this method. Do not wear loose clothing, ties or rings while operating the equipment. Exercise caution while operating blenders and mixers. 3. Principle A portion of resin is mixed with plasticizer and milled at a specified temperature for a specified time. The milled sheet is observed visually for fisheyes. These particles, or fisheyes, consist of spots with low plasticizer concentration. They are harder than their surroundings and, because their flow temperature is higher, are dispersed only with difficulty. They appear as "windows" or "stars" in a sheet. 4. Apparatus (a) Two-roll laboratory plastic mill, 6" x 13", roll speed 20 rpm back, 28 rpm front, with a controlled temperature range from 250F to 350F minimum. (b) Balance, 0-1000 gm Mettler or equivalent. (c) Pyrometer, surface, 0-4008F, Pyrometer Instrument Co., or equivalent. (d) Illuminator, General Electric Duoline, 14" x 17" or equivalent. (e) Gauge, dial. Federal Model 22-P-10 with special spring for plastics, or 0-1" Micrometer, or equivalent. (f) Reading glass, 2X magnification. (g) Take-off board, see Figure 1. (h) Cutting tool, brass, see Figure 2. (1) Timer, interval, 1-60 minutes. (j) Ball mill, porcelain. 5. Reagents (a) Dioctyl Phthalate (DOP). (b) Paraplex G-62. Rohm and Haas, Philadelphia, Pa. 1 of 5 Pages February 10, 1967 -352 of 5 Pages LAD-AM-67.2 (c) Mark XV, Argus Chemical Co. (d) Stearic Acid. (e) Carbon black, Witcohlac No. 100, Witco Chemical, Monarch 71, Cabot Corporation, or equivalent. 6. Sample Preparation (a) Master blending of additives. Load the ball mill with the additives in the following proportions in quantities depending upon the size of the mill. Additives Parts by Weight Dioctyl Phthalate Paraplex G-62 Mark XV Stearic Acid Carbon Black 41.50 8.00 2.00 0.20 0.18 Roll the mill for 2 hours or until the additives are dispersed. Transfer the dispersion to a round large mouth bottle or any container that can be mixed by rolling or stirring before taking a portion out for resin formulation. (b) Resin Blending Weigh 400 g of resin and 200 g of the master blend into 1000 ml beaker (stainless steel) , and mix with large spatula "until master blend is well distri buted ^15 minutes) . 7. Procedure (a) Heat the mill rolls to the desired temperature depending on the molecular weight of the resin. See Table 1 for temperatures. Measure the roll temperature with the surface pyrometer before using the mill. (b) Adjust the roll clearance to produce a 10 0.5 mil sheet. This adjust ment may be made by milling a test sheet to .obtain the correct setting. (c) Weigh 50 2 g of the formulated resin and feed to the moving rolls. Start the timer at this point. (d) Make cuts in the blanket to keep the bank in motion until the bank rolls continuously on its own accord. (e) Stop the mill when the desired time has elapsed. Cut the blanket horizontally across the top of the roll, and drape the blanket end over the wire on the "take-off" board. Start the mill and pull the board away from the rolls as the blanket comes off. (f) Place the forepart of the blanket on the illuminator and count the number of fisheyes visible through a 2X reading glass in a 6" x 6" square. 8. Report The report shall include the complete sample identification and the minimum milling time in minutes to reach 2 or less fisheyes in a 6" x 6" square. 9. Notes (a) A fisheye will appear as a small round "window" or "star" in a black milled sheet when held to a light. They should not be confused with air pockets or tears in the sheet, both of which will stretch, while a fisheye will not. uce 039119 Fcbruary io. 1907 -363 of 5 Pagi-s LAD-AM-6 7 ..7 (b) The following factors affect the fisheye count and should be closely controlled, (1) Mill temperature (2) Additive concentration (3) Sample size (4) Thickness of the milled sheet (5) Milling time (6) Formulation procedure (7) Avoidance of foreign contaminates such as dirt, extraneous polymer fibers, etc. 10. Company Reference Vinyl-Vinylidene Plastics Method No. 509, "Determination of Fisheyes in Polyvinyl Chloride", September 29, 1966. C. A. Barrios Research and Development di U( * t"-s February 10. 1967 -371 oi 5 Pages LAD-AM-67 2 TABLE I. MILL OPERATING TEMPERATURES Resin Type QX-3816.1 QX-3816.2 QX-3816.3 QX-3816.4 QX-3816.5 QX-3816.6 QX-3816.7 QX-3816.8 QX-3816.9 Inherent Vise. Range* 0.59 - 0.64 0.68 - 0.73 0.76 - 0.81 0.82 - 0.86 0.88 - 0.93 0.94 - 0.98 1.04 - 1.08 * 1.10 - 1.16 1.23 _ 1.28 Mill Temp 300 300 310 310 310 325 325 325 350 *ASTM Test D 1243 O ucn 039121 FIGURE I TAKE-OFF BOARD 'FIGURE H MILL CUTTING TOOL BRASS i ^'approx. -39- DOW INDUSTRIAL SITE FIG. I VICINITY MAP LOCKWOOO, AMMWWt ft NfWNAtf( IMC ucc