Document X2p0EeD3exLKGQxvnErRb6Gg

St. Louis Rese< f Deparjaaent August 16, 1967 J.ti. Lull -M.0.-3 R.S.WObus -R.B.-3 T.M. Patrick, Jr,-Rea, 8 R.L. l&dworth -Amista H.L. Morten -Res. 1 T.W. Dalton -W.G.K. Mr. D.B. Hosoar AXMISTOH TMP/D8BI, B-l-57 AHQCLQF, RLSSARCH PROGRAM An active program has been urjdorvtay since May to study the vari ables in the Aroclor process especially with the new stability test as a tool. This has aeant repeating cany of the experi ments that have been made in years past in order to reevaluate the stability in terras of the newer analytical procedure. Our program has been laid out with empit&sis on the phases of the present process where deviations in the plant can conceivably occur. Z aia attaching a copy of the outlined program that Dr. Merten has suggested after a careful review of the foraer Swann and Monsanto reports and also your program suggestions of April 1, 19.7. Our conclusions to date nave oeen reported in our progress reports and in several letters to your plant. These a&y be summarised as followsi (1) With all process conditions being met, the rate of chlorine feed can be increased to 16-OQ pounds per hour for 4000 lbs. batch with no deleterious offeet on the stability of the Aroclor 1242, (*) Trie addition of air up to by volume does not raake an unstable Aroclor 1242 when operating under standard condi tions and a normal chlorine rate of 660 pounds of chlorine per hour for 4000 pound charge of biphenyl. (5) The effect of temperatures lower than the specified 120*C. in the process m*y be detrimental to the stability of the Aroclor 1242. This offeet varies with the amount cf catalyst present. (4) Chlorination at temperatures of 120 to 160*C. have no adverse effect on the stability of the Aroclor 1242. Higher tempera tures should not affect stability but other operating problems may result. (b) Tna aeration step Is not critical In the production of stable Aroclor 1242. The Quantity of air nor the temperature of the Aroclor between 100* and 1!>0*C. appears to affect the stability of stable Aroclor. In cases where Aroclor has stability chlorides over 1 ppm, the aeration step is an aid in improving the stability. (6) The plant distillation step shows no tendency to Isolate an unstable fraction. DSW 297213 STLCOPCB4067123 4 Mr. D. B. Hosoar Anniston -2- Auguat 16, I957 Other features of the program aru he Inc Investigated now. The quality of the biphenyl is currently under study with the idea of finding how trace impurities may affect the stability. The following data will'give you a resume* of the various teats we have made. All tests are based on the standard process of chlorinating with chlorine gas at a feed rate of 66o pounds per hour based on a 4000 pound charge. Ferric chloride (0.03$ baaed on biphenyl ciiargc) is well mixed with the biphenyl arid the temperature is maintained at 120~lpQ*C. throughout the chlorina tion. After the chlorination, the crude Aroclor is blown with air at 100 *C. and distilled from 0.25# Ca(0H). At a pressure of >0 nsa Hg., the distillation is cut when the oolumn temperature reaches 23i>24oC. The distillate is agitated for 4 hours with 0.2Js dried attapulgus clay while trie temperature is maintained at 70-30C. Stability chlorides are run by the Monsanto test method based on 16 hours heating at 21Q*'C. Any variation from the above procedure is ahown in the tables. TABLii X AIR-CHLQRIH& MIXTURES (LABORATORY) Air-Chlorine Volume Ratio 0:100 10:90 20:30 50:50 Distillation fields Monsanto stability teat, ppm chlorides TABLE II CHLQRBta F2D RAT&S Chlorine feed Distillation Yields 660 (lab.)I 1530 lab.) 700 Anniston plant BOO 11 M 350 ,r " Monsanto Stability test, ppm chlorides 0.16 0.12 0.49 0.J1 0.22 DSW 297214 STLCOPCB4067124 Up. D. B. Hosmsr August 16, 1957 TABLE III TEMPatATORK STUDIES (0.03* FC1) Temperature. *C. ' 100* > 8 hr. 110*. 8 hr. 120*, 8 hr. 14o*, 8 hr. 90*, 2 hr.* 110*, 6 hr. 95*. 0.phr.|130\7.S hr. 95 . 2 hr.* 130*, 6 hr. 95*. 3 hr.* 120*, p hr. Yields 93,5* 98.5* 93.5* 97.8* 93.8# m 93.0* 98.0* Monsanto Stability, com Cl 0.20 0.12 0.21 0.1? 1.22 0.1 0.1b 0.14 *S* O.Ol . $0.008 0 00 TABLE IV CATALYST COKCatTRATIOli AT 120*C. 71t34i Monsanto Stability, psa Cl 98.1 0.89 97.7 8.87 chlorine passing through-slow chlorine* tlon batch discarded Maple 1 1 1^ 1 1 2 2 2 TABLE V AERATION STEF - WANT SAMPLES - W.O.K. Tims of Aeration Temperature Rate of air, aWain* Stability test. Pi Cl None 0.5 hr. 1 4 4 None 1 4 10Q*C. 100 100 150 --- 150 150 1380 1330 1330 1330 1700 1380 0.96 1*62 1.40 1.10 0.76 0.49 0.46 0.45 DS\W 297215 STLCOPCB4067125 J . Hr. D. B. liosoer 4- August 16, 19^7 rxm+u vi PIABT. DISTILLATION TEST AT AKHXffgOW Aroclor 1242 Baton Ho, SOI 309 314 317 319 321 359 Run Ho. in Series 1 3 . 5*<7 J 10 1 10 Kansanto Stability, pun Chloride . oat oat oa? oaa oa? 0,28 oao 0.2o conclusions above are bated on these tests on the present proc&es, At pi^esent. Dr. Kenton is sending some tlm in tne Annistoa And Kruseirich Plants to see If tie can observe any operational details that nay bo a contributing /actor to the manufacture of unstable Aroclor. da 3-20-57 attaciimunt* A. K. Bllenburg 29l^6 0S>N STLCOPCB4067126