Document 2jOrMrLLd9oyyaMLxeY8QRjb7

ff /Q y\ i " / MONSANTO CHEMICAL COMPANY ^RINGFIELD, MASSACHUSETTS TO: R. A. Coffey (2) act May 26, 1961 AT: FVC-FTS CONFIDENTIAL SUBJECT: PINAL REPORT: EVALUATION OP 6.5$ DIMTOMETER POLYRATE VCM ON OPALON 330 - P88"60 V. W. Alexander- V H. P. Armstrong R. T. Clark O. P. Cohen A. W. M. Coaker R. I. Dunlap F. A. Duaton "y, 0, Erlcksberg (15) R. K. Perry Y. P. Phillips T* Shirley/Texas City A. P. Torrenaano M, W. Williams W. P. Willis INTRODUCTION Monsanto at Texas City has undergone equipment and process r visions which gives them a process capable of producing vinyl chloride monomer at about a 6.5$ dilatoraeter polyrate level compared to the early 1961 average of 5.2 - 55$ Before placing the entire polymerisation system on this higher polyrate VCM, this p-Number was authorized to try to pr diet any effects it might have on homopolymer (300 series) polymerization and resin quality. Of specific Interest were the effects of high polyrate VCM on resin particle size. SUMMARY Pour batches of Opalon 330 were made in late February, 1961 using unscrubbed 6.5$ dilatometer polyrate VCM produced by Texas City for Springfield evaluation. For comparison three routine batches of Opalon 330 were picked for control purposes. The SDP for Opalon 330 was used throughout the study. Slurry samples of these seven batches were taken for analysis by the control lab. for screen, bulk density, kitchen mixer dry time and extrudability. Virgin and recovered monomer samples were taken from selected batches and tested by dilatomefcer polyrate and g&s chromatography. CONCLUSIONS 1. Based on the results of this study, 6,5$ dllatometer polyrate VCM should give the following polymerization and resin properties for Opalon 330: A. Screen - significantly coarser resin should be produced. Vacuum adjustment will probably be needed. B, Bulk Density - slightly lower RSV0026484 2, Co Extrudabillty normal grade# lightly lower rate. Do Dry Time - no significant change Eo Cycle Time - no significant change at the same vacuum 2a There Is poor correlation between Springfield and Texas City on dilatomefcer polyrate testing. 3,, Subsequent plant experience with VCM up to 6,2# polyrate confirmed the shift to coarser particle size, but vacuum adjust ment was Inadequate to bring particle size in specification. DISCUSSION Number five washed monomer tank was segregated for this study. The tank cars of 6,5# dil&tometer polyrate VCM were unloaded directly to this tank, bypassing the tank farm tanks and the caustic scrubber. Lines common to standard Texas City monomer had to be used for this operation and In kettle charging, For this reason all kettle charges using 6*5% VCM were contaminated with approximately 5 - 10# standard VCM, Particle size for Opalon 330 in 88 Bldg, was fluctuating during the latter half of Februaryr tending to run on the coarse side. This was attributed mainly to a higher VCM dil&tometer level (above 57# average compared with a past normal of 5,1 - 5,,5# average). Luring the experimental study the particle size of the individual batches became variable (reason unknown) giving very flat blend distributions as fine and coarse batches were mixed, A product change in 88 Bldg,, necessitated curtailing the experimental plan and using additional kettles for experimental and control batches. The three standard batches picked for sampling for controls were all out of specification (too fine) on resin particle size. It Is felt that this must have been a coincidence as the product blend do not reflect a series of fine batches during this time. The four batches produced with 6,5# VCM had an average SAP of 99, Using the control batches slurry SAP average of 181 or the routine production blend average SAP of X3& It is obvious that the experimental batches were significantly coarser. Although two of the experimental batches were out of specification (coarse) on slurry samples^ all experimental blends were within specifications (+40 - mesh resin scalped off). Extrusion grades were normal, however the rates were slightly lower than other samples extruded at the same time {196 vs, 225) u No direct comparison can be made between the resins made with the two types of VCM used because the control lab, could not blend the control samples fcr extrusion (particle size too fine). RSV00264B5 3 Kitchen mixer dry time for the xperlraent&l batch s were normal. The dry times for the control batch s were out of specification due to the fineness of the re in particle size. The Springfield dil&tometer results compared to Texas City dllatometer results were further evidences of the lack of correlation between the two control labs. Sampling was determined to be a possible cause of part of the discrepancy. Samples taken from the unloading line during the unloading of the tank cars tested higher and closer to Texas City's results than those taken from the diptube . Sampling procedures have been changed and all routine samples are presently being taken during the unloading operation. The results of the unloading ample of GATX 37873 proved that there was also difficulty in the test itself. This sample of a car which originally tested 6.48$ in Texas City gave a value of 5.63$ in Springfield. The sample was then sent to Texas City where an average value of 6.31$ was obtained. Cause of the discrepancy is presently being pursued by the two laboratories. One limitation of this experiment was that the effect of vacuum adjustment was not tested. During the two weeks after this experiment the dll&tometer blend level was steadily increasing to a high of 6.2$ (based on Texas City tests) .as Texas City had difficulty maintaining a lower polyrate level. The 300 series resins produced during this period became too coarse in particle size to meet specifications and they could not be brought back into specification by the normal method of lowering the vacuum. This problem was finally circumvented by converting the building to the 60Q series resins. RSV0026486 APPENDIX I Kitchen Mixer' Resin Cycle Dry Extrusion Bulk NO. Kevuj.e Time TililO n&irW --wr"THnT" SCREEN Thru 2150 1 8:45 5 tOO W2B-5 204 *459 1 16 46 25 10 2 2 14 95 2160 1 9:45 4*30 W2C-5 174 .454 3 6 30 34 23 4 2 29 108 : 2167 L 2168 1 8:45 4:30 9:00 4*45 V2C-5 204 V2C-5 203 .436 .411 T H 51 3 12 T 5 48 28 15 3 1 15 94 1 19 99 Ave, 9:04 4:41 196 .440 99.. ; 2153 4 8:45 20:00+ -- .478 T 1 X 8 31 29 31 91 188 ' 2155 1 8:55 12:00 **** -- .415 T 1 1. 7 35 36 20 91 17g i; 2165 3 9:00 15; 00 -- .451 T 1 1 6 40 34 18 92 176 1 1 Ave. 8s53 -- .446 -- 181 j"-/ ft batches 3 1/2" vacuum Lot 357 PDR-1 Other batches produced under same conditions 21-46 2148 2154 2159 1 4 3 3 8:55 8*45 9:00 8:55 Blends produced during experimental study* Routine: 61055 61056 61058 61059 Ave. .46? T 12 21 24 21 12 10 43 126 .487 T 6 28 19 18 14 15 47 136 .470 T 1 11 13 29 25 18 72 158 .464 T 4 29 . 26 1 10 9 40 124 7475" ------- 136 assasgaa8 61057 61060 61061 [Bauch 2150} Batch 2160) [Batches 2167 & 2168) .459 T 13 49 22 12 3 2 17 97 .454 T 4 27 33 25 7 4 36 116 .439 T 5 43 28 16 5 4 25 110 & RSV0026487 APPENDIX II - VCM DATA Impurity Pv ,,p Propane Propane Isobutane n-*Butane Butene-1, Isobutene t-Butene-2 0---Butene-2 Isopentane 1,3-Butadiene Methyl Acetylene Methyl Chloride VCM Ethyl Chloride 2-Chloropropene u-6 u-3 U-4 Vinylldene Chloride Dllatometer Polyrate taverage of 2 Springfield Lab) 6.48 GATX 37873 (222A) 6.0 132. 257 1.8 2.2 0.6 9.7 4.0 21.4 00 6.47 GATX 76245 (2) Batch 6.48 Virgin 223A 1,4 2.1 88.88 228 1.6 2.2 0.4 9.0 2.5 13.3 00 3.2 86.6 176 1.7 1.8 0.3 0.2 7.5 2.8 14.4 00 2160 6.48 Recovered 223B 14.8 297 525 5.2 4.3 0.7 9.0 42.4 00 0.6 5.64$ 5.82$ 5.35# 4.90$ Batch STD (5.77) Virgin 223C 1.4 100 212 10.0 4.2 0,7 17.0 2.4 1,7.6 00 5.36$ 2165 STD (5.77) Recovered 224b Batch 6.47 Virgin 224a 2167 , 6.47 Recovered 224c 7.2 3.8 16.4 304 522 17.6 7.4 1.0 100 200 1.6 1.8 0.4 323 509 6.8 4.4 0,6 6.4 40.8 OO 7.6 3.0 17.1 00 0.4 7.4 41.0 00 5.73$ 0.7 2.4 5.07$ 4.9 5.74$ Impurities are recorded in mm. peak height - gas chromatograph data (G.L.P.C.) DI latome ter data (Springfield Individual values $) GATX 37873 6.48 Texas City Test Diptube sample Unloading sample 5.20, 5.24, 5.30 5*48* 5.78 5.25 Ave. 5.63 Ave. GATX 76245 6,47 Texas City Test Diptube sample Unloading sample 5.22, 5.29, 5.33, 5.3^ 578, 5.87 5.30 Ave. 5.82 Ave. \ I RSV0026488