Document vwKr5LQRKN7jjQprmdzBNykR

(conoco) lnt_roffice Communication To R* L* Poe, Chemicals Research, Ponca City From L. R. Holliday Date March 30, 1984 Subject MONTHLY PROGRESS REPORTCHEMICALS GROUP--MARCH 1984 PROBLEM 2801-1--GENERAL CHEMICAL RESEARCH WORK Data Acquisition and Control System--W. L. Sorensen Several purchased items have arrived from DEC and have been installed. These include two graphics terminals, one modem, and the floppy disk subsystem. The one megabyte of RAM memory we purchased was faulty and is being returned to DEC for warranty repair. An HP color graphics plotter was also received and installed. Efforts are underway to make these utilities available for use. The long awaited third CRT has been received from Fischer and Porter. While the software to make the three CRTs operational has not yet arrived, the new CRT was used to replace the bad COPTM CRT in Control Room 4, This allows us to maintain two good CRTs in operation while the bad CRT is idle, awaiting repair. Responsibility for completing arrangements for the repair of the bad CRT has been turned over to Chemicals Research (CD). Work continues as needed in aiding Chemicals Research (CD) with configuration changes and troubleshooting of the HDPE pilot plant. PROBLEM 6803-10--CHEMICAL ENGINEERING STUDIES, GENERAL IBM Computer Support--W. L. Sorensen Work is still in progress to separate Chemicals Research (CD) from Chemicals Research (V) in the area of computer charges and data-file ownership. Additional effort is underway to set up the new accounting procedures for Chemicals Research (V) under the computer department's FARS accounting system. When complete, I will again produce computer charge breakdowns for each section of Chemicals Research (V). PROBLEM 6804-7--SERVICE WORK, ALUMINA PLANT BEPEX Hydrothermal Treatment Test Run--D. 3. Lewis A test run at BEPEX to produce a sample of hydrothermally treated alumina for 3M approval was performed on March 20 to 23. Initial analyses of the material produced indicate that approximately 650 pounds of acceptable material was produced. 3M has indicated that they may be able to use as little as 500 pounds for their qualification testing. All material is being shipped to Ponca City for complete analysis prior to sending out any samples. OCR 000019448 Monthly Progress Report--Chemicals Group Page 2 March 30, 19S4 PROBLEM 6804-11-SERVICE WORK, n-PARAFFIN PLANT Molecular Sieve Pilot Plant--W. L. Sorensen The pilot plant was operated every week this month except for the week of March 12. (The unit was down for waste and drum disposal during that week.) The three-level factorial experiments for the Shell 324 catalyst were completed this month for a temperature range of 450 to 510F and kerosene flow rates of 0.7 to 1.3 gallons per hour. At these conditions, the catalyst appears to be less active and less stable (i.e., deactivates faster) than the previously tested Shell 424 catalyst. In particular, lowering the reactor temperature to 450F seems to "upset" the catalyst and dramatically increase product sulfur levels. This could be due to temperature cycling of the catalyst during the experimental run or that 450 F is the borderline between the catalyst being active or inactive. The Shell 424 catalyst did not show this behavior at these temperatures. Results have been received from testing of a sample of the 1981 molecular sieves. At a sulfur level of 0.8 ppm, the sieves had a higher S-14 number (20.6) than the sieves tested previously with Shell 424 (S-14 of 14 to 17). These results are still being investigated. It is planned to retest the 1981 sieves the week of March 26 at a lower sulfur level to determine if we are correctly interpreting our data. The 1979 molecular sieves were also tested this month and gave the following results: S-14 = 18.2, A-14 = 4.4. Training has been completed for another technician to operate the pilot plant. Currently five technicians are trained as operators. PROBLEM 6805-10--SERVICE WORK--BALTIMORE PLANT--C. A. HECKER In response to our letter initiating 1984 service work, a planning meeting between Chemicals Research and Baltimore plant personnel was held on March 27. Topics discussed included alternate catalyst systems, ultraviolet initiation for chlorina tion, alternate uses for DPA, liquor unit operating problems, black chloroparaffin problems, and the simulation model, among others. A plan for 1984 service work was defined and established at this meeting. An article in the January 30, 1984, issue of Chemical Marketing Reporter indicated that a Japanese company "now has technology which may replace the FriedelCrafts synthesis for aikylbenzenes and aromatic ketones." A patent and literature search of benzene alkylation processes was conducted in an attempt to discover an alternate catalyst technology employed by a Japanese firm. Thus far, no novel process has been uncovered. Efforts are continuing. Nalkylene* Alkylate Plant Simulation Program--A. W. Wardwell This research report is complete except for a small amount of drafting needed on one page. When this has been completed, the report will be sent to printing. CCR 000019449 Monthly Progress Report--Chemicals Group Page 3 March 30, 1984 PROBLEM 6817-6--CATAPAL SB ALUMINA--C. A. Hecker Preparation for work on alumina began this month. Research reports, patents, the alumina training manual, and other alumina-related information were reviewed. Experiments on hydrothermal treatment of alumina and exploratory-type experi ments on increasing solids concentration of alumina slurry were begun. Hydrothermal treatment experiments are an extension of D. 3. Lewis' work on increasing acid dispersibility of alumina by exposing spray-dried alumina to a hot, humid environment for several hours. Ideally, these conditions could be imposed during storage. Initial experiments were an attempt to duplicate D. 3. Lewis' results but starting with an alumina sample with a lower acid dispersibility starting value. Unfortunately, acid dispersibility was decreased somewhat during the first three treatment runs. This was possibly due to (1) early removal of the alumina sample from the humid environment without allowing it to cool sufficiently, or (2) an apparent decrease in acid dispersibility because the results were not corrected back to 72.5 percent AI2O3. Subsequent analyses will include alumina content determination so acid dispersibility results can be compared on an equalalumina basis. Experimental conditions and results for the first eight runs are summarized below. ALUMINA HYDROTHERMAL TREATMENT EXPERIMENTS Alu- Experi- Tempermina ment ature Time Lot No. Number <F) (hr) 759 Untreated 759 156-1 230 5 759 158-1 210 6 759 158-2 210 22 759 162-1 225 5 805 Untreated 805 163-1 230 7 805 163-2 230 22 759 165-1 220 6 Water Added co2 Agi- (Weight Bub- tation Percent) bled Acid Dispers- ibility (Weight Percent) 90.8 Yes 0 No 89.7 Yes 0 No 87.7 Yes 0 No 87.6 Yes 20 No 94.6 92.53 Yes 0 No 83.7 Yes 0 No 54.0 Yes 20 Yes 95.3 Light Transmittance PM (Percent) 4.4 40 3.8 28 4.0 28 3.6 17 2.8 40 3.9 64 2.5 28 2.0 29 3.9 49 Increasing solids concentration of alumina slurry (while maintaining pumpability) would serve to reduce energy costs in the spray drier, as well as possibly provide a means for recycling off-spec alumina. Experimental work, thus far, has only been to observe that spray-dried alumina powder can be resuspended in the alumina slurry to very high solids levels (>50 percent). However, the resulting suspension has a very "gritty" feel, due to the addition of the spray-dried material. Planned experimental work will include measuring viscosity of the slurry at increasing solids levels, correlating these viscosity values to the plant's "flowability" CCR 000019450 Monthly Progress Report-Chemicals Group Page 4 March 30, 1984 measurements, determining the maximum acceptable viscosity, and attempting to reduce viscosity of the resulting slurries to this level. PROBLEM 6816-17--SULFONATION OF LINEAR ALKYLBENZENES PROBLEM 6817-21--SULFATION OF ALCOHOLS AND ETHOXYLATES WITH SULFUR TRIOXIDE Sulfonation/Sulfation Pilot Plant--3. O. Gregg The sulfonation pilot plant was down the entire month. Operations will resume the week of March 26. The equipment for the new SO3 drum transfer system has arrived and will be put into service. The pilot plant will be started up as soon as the drum transfer system is tested and a drum of SO3 is loaded into the storage tank. Tentative plans are to produce three samples. 1. Two drums of 1012-A for Uniclean. 2. Two drums of 1412-60 sodium sulfate for Lever. 3. A sodium sulfate of Alfonic 1214-65 (two drums for Lever and 1/2 drum for Colgate). This sample may be cancelled. Work has begun on the research report describing 1983 sulfonation pilot plant activities. An estimate of expected sulfonation pilot plant waste generation was made for R. B. Martin. PROBLEM 6817-33--CATAPAL SB ALUMINA, ALCOHOLYSIS OF ALUMINUM Novel Alumina--VISTAL ML--D. 3. Lewis Laboratory work on this project continues. A modified vapor phase hydrolysis method has been demonstrated which significantly improves the yield of alumina from alkoxide. This method employs nitrogen stripping to help transport alkoxide into the vapor phase. An IOC was issued describing the VISTAL ML process and comparing the properties of VISTAL ML with Catapal. Table 1 from that IOC is attached and shows the striking differences in properties of the two aluminas. Samples of VISTAL ML have also been hydrotherm ally treated and calcined. The analyses of these treated samples are not yet complete but initial results are encouraging. Hydrothermal treatment increased the acid dispersibility from 14 percent to 44 percent, produced a measurable crystallite size (26A to 48A), and transformed at least some of the alumina to boehmite. Calcining at 1000 C transformed VISTAL ML to alpha alumina (corundum). This transition is typical of Catapal as well as many other alumina products. The appearance of untreated VISTAL ML under an electron microscope is that of small solid spheres. Hydrothermally treated VISTAL ML appears to be hollow spheres. CCR 000019451 Monthly Progress Report--Chemicals Group Page 5 March 30, 1984 An ICR has been submitted on the VISTAL ML process. PROBLEM 6835-3--NEW DETERGENT INTERMEDIATES Methyl Ester Sulfonates (MES)--3. O. Gregg A meeting was held February 23 to discuss MES process development. Attendees were: L. R. Holliday 3. O. Gregg M. E. Osborn M. McWhorter B. E. Leach G. L. Nield W. A. Dickenson The current status of the project was reviewed. Plans were made for demonstra tion batch and thin-film sulfonation runs in the lab so that all involved could make first-hand observations of the process. The batch sulfonation run, followed by batch bleaching and neutralization, was made on March 9. The lab-scale, thin-film sulfonation run was made on March 15. The acid was bleached and neutralized batchwise. Based on observations during this run, the sulfonation pilot plant should be able to process MES without having any physical handling problems. Preliminary work has begun on a speculative economics study of methyl ester sulfoxidation. Miscellaneous D. 3. Lewis is transferring to the Chemicals Research Section (V), effective April 2, 1984. During March, he has been involved in customer calls on Du Pont, 3ohnson-Matthey, 3M, and UOP. The results of these customer calls will be reported in the Chemicals Research Section monthly. L. R. Holliday Research Group Leader Engineering Research Section mk Enc CCR 000019452 TABLE 1 COMPARISON OF CATAPAL SB AND VISTAL ML PROPERTIES Surface Area (m2/g) Loose Bulk Density (g/&) Carbon Content (wt %) AI2O3 Content (wt %) Acid dispersibility (%) NAG (min) PTV (min) Crystallite Size A 020 Plane 021 Plane Composition (wt %) Free Water Tr ihydrate Psudoboehmite Boehmite Impurities (ppm) Fe203 Si02 Na20 Particle Size Distribution (wt %) >90 u <45 u < 2u CATAPALSB VISTAL ML 280 710 0.36 74.2 90 5-20 15-30 314 162 6 71.3 14 - 34 <25 48 < 25 10 6 not recog 55 nized as any 35 of these1 50 37 80 426 2 40 18 19 0 38 0 0 1003 Analysis may be affected by extremely small particle size. 2Probably due to contamination from apparatus. 3 AI I particles are perfect spheres generally <ly diameter. CCR 000019453 (conoc ) Interoffice Communication To R. L. Poe From W. R. Carradine Date March 29, 1984 subject MONTHLY PROGRESS REPORTRESEARCH ASSOCIATE--MARCH 1984 PROBLEM 6801-11-INFORMATION TRANSFER TO VISTA The information transfer committee is continuing to work on preparation of a list of items to request from Conoco R&D. We are hoping to have the first list (containing most of the items) completed early in April. PROBLEM 6817-30--ETHOXYLATION TECHNOLOGY PROBLEM 6804-10-ALCOHOL PLANT SERVICE We now have a laboratory thin-film evaporator (ASCO) unit ready for operation. We are planning to use this apparatus for several projects in these areas. Initially, we will be stripping ethylene oxide, dioxane, and free alcohols from normal, NovelTM, and "super NovelTM" ethoxylates. We are also planning stripping studies on alkoxide, growth product, and knock-out pot thermal olefins. PROBLEM 6817-35-ALCOHOL QUALITY IMPROVEMENT PROBLEM 6804-10-ALCOHOL PLANT SERVICE A number of projects (Section 225 replacement, new oxidation procedures, better alkoxide stripping, new diol removal technology, etc.) in these areas have been proposed by various persons. Several of us are now involved in discussions which will hopefully result in some consensus concerning those projects worthy of pursuit. Communications lines are open, and we should be able to make proposals which will lead to improved alcohol plant operations. The extent of my involvement, of course, will depend on which projects are chosen for additional study. W. R. Carradine fc CCR 000019454 (conoco) Interoffice Communication To From Date Subject R. L. Poe, Chemicals Research, Ponca City W. H. McNeese April 2, 1984 MONTHLY PROGRESS REPORT, VCM/PVC GROUP, MARCH 1984 PROBLEM 6803-10 CHEMICAL ENGINEERING STUDIES, GENERAL VCM from Ethane Process--D. A. Barclay A meeting was held on February 22 with Chem Systems Research Inc., Fairfield, New Jersey. They disclosed details of their proposed process for making VCM from ethane. The technology is based on research and patents by ICI, to which Chem Systems now has development rights. Work is proceeding on the economic and technical evaluation of the proposal. A recommendation on whether support for their development program should be provided will be made in the near future. PROBLEM 620-17--PVC RESIN DEVELOPMENT CTA Production Run--A. W. Wardwell, P. C. Schirber Support was provided for the March CTA production run in Aberdeen using 2-mercaptoethanol as the chain transfer agent. Twenty-three batches (1.3MM pounds) of 5265 and one batch (56,000 pounds) of 5305 were produced. Except for a few batches containing a high percentage of fines, all the resin produced was on spec. Runs with 2-ME provided by Morton-Thiokol showed it to be an acceptable alternative to the Phillips product. Flake production was minimal throughout the run; however, a higher percentage of flakes was observed in the dryer sifter overflow from D-745 batches than from D-700. Total reactor charge volumes averaged about 22,600 gallons. A trip report was issued detailing the run data and resin analysis results. 2-ME Spill Handling--F. C. Schirber A letter was written to Pete Markey in Aberdeen summarizing results of an investigation to determine the best available absorbents for handling 2-mercaptoethanol spills and the best method for transporting safety equipment and containment materials to the spill site. In a conference call with Pete Markey, Tom Grumble, and A1 Sayther from Aberdeen, it was decided that Hazorb spill containment pillows and SorbAlI absorbent would be placed near high-potential spill locations. In addition, a mobile spill cart similar to the one used in R&D West will be used to store additional spill handling materials and equipment. CC R OOOOZ9455 R. L. Poe Page 2 April 2, 1984 Arrangements will be made to have the spill cart fabricated in Ponca City and sent to Aberdeen before the temporary CTA addition system is in place. Also, lab tests will be run to ensure compatibility of 2-ME with the absorbents chosen. Chain Transfer Agent--D. A. Barclay Flake Production--An IOC covering flake production of Reactors 700 and 745 during the February CTA test was issued. The conclusion was that at the nominal charge volume of 23,000 gallons, D-700 produced no flakes, while D-745 was producing a moderate level of flakes. This reflects the agitation difference between the two reactors. Materials Compatibility Testing--Vitoi# and Kalrez elastomer samples were checked after one month's exposure to 2-mercaptoethanol. The Kalrez o-rings and VitonG plaques were unaffected. One Vitorf o-ring showed no change in weight or dimensions, but the other had significant swelling. It is suspected the failed o-ring may not be Vitorf^ polymer but standard rubber. The test is continuing, and the materials will be examined next at two month's exposure. A test of Hypalon and Nordel polymers was begun. The one-month exposure results are not yet available. PROBLEM 6820-20 PVC CAPACITY/QUALITY OPTIMIZATION Hard Particle Problem--D. A. Barclay The colloid-initiator study in R-210 (15-gallon reactor) was completed. Resin analysis is underway. Polymerization time results show significant interaction between colloid and initiator. High colloid concentrations reduce the initiator efficiency. Cold Water Methocel Makeup--A. W. Wardwell Filtered Methocel Study All analytical results have been returned, except gel tests, on the resins from the runs in the 50-gallon reactor. Most test show no significant differences in resin properties between filtered and unfiltered colloid. However, the Chemby test results show that using filtered colloid gives a definite decrease in the number of black particles. Powdered Methocel Addition Study Gel test and porosity results are pending on these resins. Particle size shows a definite trend, with the particle size increasing as the fraction of powdered colloid is increased. This effect is pronounced for the runs made with 25 and 30 percent powdered colloid. The Chemby test also shows a trend, with the number of black CCR 000019456 R. L. Poe Page 3 April 2, 1984 particles decreasing as the amount of powdered colloid increases. This effect is most noticeable when the amount of powdered colloid is between 0 and 20 percent of the total amount of colloid. Antifoam Test Methocel solutions made up with cold water have a tendency to foam on makeup. A test was made to determine if a silicone antifoam would reduce the time required for the foam to subside. The antifoam did reduce the foam subsidance time by at least a factor of 2. Plans Two additional runs are planned for this program. The first will test the effect of silicone antifoam on resin properties. The second will test the effect of gellation of colloid on resin properties. PROBLEM 6820-25 AGITATION STUDY-D. A. Barclay A table of the current PVC reactor agitation configurations was developed. This will provide a ready reference for scale-up use and plant test calculations. D-700 Agitation Test--The data from the agitation test in D-700 have been loaded into a computer data base. Final results analysis should be speeded up considerably by use of the SAS programs which can access this data. R-120 Torque Measurement--A tare torque calibration was done on R-120 (50gallon reactor) in the pilot plant. The power draw caused by reactor bearings and seeds was determined as a function of agitator speed. This is subtracted from power measurements on PVC batches to get the actual power delivered to the fluid. An IOC detailing the results has been issued. New Suspending Agents--An outline of necessary agitation experiments for scaling new suspending agents to the plant reactors was given to Pete Schwab. The PVA/Methocel suspending agent testing will proceed on this basis. PROBLEM 6820-32--SMALL REACTOR PVC PILOT PLANT Control System--P. C. Schirber Work is in progress on rewriting the configuration of the DCU for the PVC pilot plant in an effort to: - Streamline the reactor sequence programming - Identify unused or obsolete inputs, outputs, and controllers CCR 000019457 R. L. Poe Page 4 April 2, 1984 - Upgrade the system to provide more security, flexibility, and convenience of operation. This exercise will also make configuration changes much easier in the future. A manual charge phase which enables addition of water and/or VCM at any time during the reactor sequences was tested with water over the weekend. The program logic worked as expected and is ready to be tested on a recovered VCM run. Procedures for operating the manual charge phase were submitted to Dean Weimer to be included in the latest operating manual revision. Work continues on the Hewlett Packard system for monitoring heat release from the reactors. The quartz temperature probes and thermometer have been received, and the HP calculator, plotter, printer, disc drive, and multiprogrammer all seem to be in good operating condition. PROBLEM 6838-3 PVC FLEXIBLE COMPOUND SUPPORT PROBLEM 6838-7 PVC RIGID DRYBLEND DEVELOPMENT Laboratory Intensive Mixer Modifications--A. W. Wardwell A design for a cover for the laboratory intensive mixer (a modified Waring blender) was made and given to Paul Middlebusher for construction. The cover will be made from polymethylmethacrylate and will include a holder for a baffle, which will aid the mixing. When the cover is finished, tests will be made to determine what baffle angle should be used and whether flexible compounds can be made in the blender. Work was done on an alternate blade design for use if the blender is unsuccessful at mixing flexible compounds. The cover should be completed within two weeks. PROBLEM 6839-10 SERVICE WORK, VCM PLANT Mesh Coalescer Testing--D. A. Barclay The VCM plant has reactivated testing of a mesh coalescer system for removal of sodium compounds from caustic-washed EDC. A coalescer removes the entrained water and, thus, sodium compounds from the EDC. This project is directed toward incineration of the tars which currently have too much sodium to be fired in the incinerators. (Sodium will attack the firebrick lining.) Their renewed testing has been encouraging, but final sodium levels in the EDC have reached 5 ppm instead of 1 ppm obtained in the original work. The procedures and test setup were reviewed. No cause for the higher Na levels could be found. It was recommended that the temperature-solubility effects be examined. The R5cD work in 1980 suggested sodium compounds increased in EDC solubility as CCR 000019458 R. L. Poe Page 5 April 2, 1984 temperature increased. Since this is not removable by the coalescer, a higher EDC temperature would result in higher Na levels. They plan to investigate this. PROBLEM 6839-11, SERVICE WORK, VCM PLANT Transfer Line Exchanger Pilot--J. O. Gregg Dow Corning has provided literature describing their heat transfer fluid testing procedures. Samples of Dow Coming's Syltherm800 and Monsanto's Therminol75 have been ordered for thermal stability testing. MISCELLANEOUS 1. D. A. Barclay attended a seminar on operation of Halon 1301 fire protection systems used in the control rooms of the pilot bay. 2. D. A. Barclay, A. W. Wardwell, and W. H. McNeese attended a meeting with representatives of Dow to discuss Methocel suspending agents for PVC3. J. O. Gregg attended managerial grid in Houston from February 26 through March 2. 4. J. O. Gregg attended the technical writing course in Ponca City from March 12 through March 16. Engineering Research Division aa 000019459 CCR (conoco) Interoffice Communication T From Dat Subject R. L. Poe, ChemicalsResearch (V),Ponca City D. R. Weimer April 3, 1984 MONTHLY PROGRESSREPORT-PVC PILOT PLANT-MARCH 1984 SMALL REACTOR PVC PILOT PLANT--C. 3. MCDONALD AND D. R. WEIMER PVC Pilot Plant Operations The pilot plant was operated 20 days during this reporting period. Projects Runs R110 R120 R210 R220 6820-33 High Processing Resin 6820-31 Suspending Agent Evaluation 6820-20 Methocel Makeup 6820-34 High Heat Stability Resin 6820-17 Resin Development RVCM 6820-33 High Processing Resin 6820-31 Suspending Agent Evaluation 6820-17 Resin Development RVCM 6820-31 Suspending Agent Evaluation Resin Development 6820-17 Reactor was used for the 2ME corrosion test 15 days this period. 11 6 5 5 2 4 1 5 1 1 4 10 4 The R120 reactor was in service only 6 days during this period. PVC Pilot Plant Maintenance 1. Flange couplings for the R120 agitator drive were completed and installed. The new couplings have stabilized agitator motion. Construction drawings are in progress to modify the seal housing for double run bearings. 2. Colloid makeup tank agitator bearing and seal were replaced. 3. Semi-annual equipment lubrication was performed. 4. The R210 charge line from the charge pump to the charge manifold was replaced because of plugging. 5. Installed breathing air in Lab 1512 for personnel protection when pouring up hazardous chemicals to be used in VCM polymerizations. CCR 000019460 R. L. Poe Page 2 April 3, 1984 6. Insulated RVCM tank condenser. 7. Rebuilt single- and double-stage Corken compressors. 8. Repaired temperature indicator, seals, and bearing on colloid makeup tank. 9. Inconel 600 rupture disks were installed in both 50-gallon reactors--R110 on February 29 and R120 on March 14. 10. Replaced all valves on the recovery compressors discharge lines. These valves were leaking internally and prevented isolation of the recovery compressors from the RVCM tank when compressor repairs were necessary. 11. Replaced a leaking flex hose on the discharge of a recovery compressor with stainless steel tubing. 12. A large number of excess and outdated initiators were disposed of by the Conoco hazardous chemicals disposal system. 13. The Applied Automation OPTICHROM 2100 GC which had been loaned by Chemicals Research to the OKC PVC plant for reactor head space analyses was brought back to Ponca City. Checkout and modifications of the unit are in progress in preparation for expansion of the present pilot plant unit. 14. The PVC Pilot Plant Operating Manual was updated and will be ready for distribution in the near future. 6820-33--2-ME CORROSION STUDY--C. 3. McDONALD MED is currently analyzing the metal coupons from the accelerated latest 2mercapto ethanol (2-ME) corrosion study. Both stressed and unstressed metal coupons of 304L and Inconel 600, were used in the study. Unstressed Ni was also used. The coupons were subjected to a water/VCM mixture containing 2 percent 2ME for 550 hours. 6820-17--SEEDED POLYMERIZATION-C. 3. McDONALD The effect of time of mediator additions to a polymerization seeded with CaSt was studied in the 15-gallon reactor. The study was performed at the request of Cort Schupbach of Patent and Licensing for support of the patent application disclosing this process. As the time into polymerization that the mediator was charged increased, particle size also increased (CaSt was added at charge). Results are shown in Table 1. CCR 000019461 R. L. Poe Page 3 April 3, 1984 TABLE 1 Run No. Time of QMS Addition Particle Size COV 210-559 210-562 210-560 At Charge (With Cast) 10 Minutes After Heat-Up 30 Minutes After Heat-Up 132 190 'Set-Up' 0.339 0.446 6820-17--EFFECT OF CO2--D. R. WEIMER AND C. J. MCDONALD The CO2 in the polymerization charge runs reported last month were repeated to verify the results of longer polymerization times. The table below shows the results. Phm C02 Base Pressure (psig)1 Reactor Pressure Just Prior To Pressure Drop (psig) Kill Pressure (psig)2 Poly Time (Min) 0 120 118 90 312 0.05 126 136 106 332 0.10 132 142 112 352 (1) Base pressure taken when reactor contents reached 134F. Both runs with CO2 gave a gradual increase in pressure up to beginning of pressure drop. In both cases, the increase was 10 psi above the base pressure. (2) Kill pressure was approximately 30 psi below reactor pressure just prior to pressure drop. Resin quality of the CO2 runs was not significantly different from that of the standard run. Particle size, bulk density, gels, color, and heat stability were evaluated. MISCELLANEOUS C. J. McDonald attended Technical Writing Class March 12, 14, 16. C. J. McDonald attended a Hazon 1301 System Seminar on March 15. OCR 000019462 R. L. Poe Page 4 April 3, 1984 PERSONNEL C. K. Snell is on medical leave for an indefinite period of time. D. R. Weimer kah CCR 000019463