Document 5D2yey7gv7mKBb9GZ3jOMZbaR

FR COMPANY USE ONLY P%0css nAT,, August 5,, 1974 TEST AUTHORIZATION NO. TA-C- 74-719 & TEST CONCLUSION OFFICIAL PRODUCT NAME______Tertiary-Butylbenzoylbenzoic Acid Molten PRODUCT CODE NOPOUNDS PRODUCT PROPOSED 59,080 AREA"Ponsol"BUILDING NAMEIntermediates TITLE See Page 2. PREPARED BY:_______ D. S. James RESPONSIBLE FOR TEST AND TEST CONCLUSION:_____D.t.-S.r...COSMOS. p u r po s e o f t e s t - To document operational changes in "Ponsol" Intermediates by (1) use of nitrogen vs. CO2 to purge K-9'; (2) modifying solids charging pro cedure in K-9; (3) use of T-21 (as well as T-20) for drowning; (4) use of jet and jacket initially at same time in S-9; (5) use of lower distillation tempera ture endpoint in S-9; (6) elimination of crystallization point as criteria ation completion. ST` Twenty-eight charges. . STANDARD INVOLVED: TA-C-70-441; CWP 770-114-950 ANALYTICAL CONTROL: 2D No change Change described under Test Details TECHNICAL BASIS FOR CHANGE: Plant experience. TEST DETAILS; (Include Safety and Waste Disposal) See Test Results. SAFETY: No change from standard process. WASTE DISPOSAL; No change from standard process. RESULTS OF TEST; See Page 2. RECOMMENDATIONS; See Page 2. i I DISTRIBUTION: R. j. Pohl J. L. Files C. H. Lake T. E. Lewis D. O. Miller (3)^ G. L. Porter D. Putnam (3) C. J. Slentz F. Laucius D. S. James. A. F. Burk D. *M. Crous.e DATE CH . SUPV ft, retH SUPERINTENDENT, ANALYTICAL (Whan Required) DATE AUTHORIZED BY: \, , / /-A-?//. //, /SVy_______ SUPERINTENDENT, MANUFACTURING (Or Delegates)' /lw_____ - DATE DATE DATE SUPERINTENDENT, DYE QUALITY CONTROL (When Req'd) DATE SUPERINTENDENT, TECHNICAL (If Any) ATE Page 2 TA-C-74-719 & TEST CONCLUSION Tertiary-Butylbenzoylbenzoic Acid Molten TITLE; Document! Use of nitrogen vs. C02 to purge K-9; modifying solids charging procedure in K-9; use of T-21 (as well as T-20). for drowning;.use of jet and jacket initially at`same time in S-9; lower distillation temperature endpoint in S-9; elimination of crystallization point as criteria for distillation completion. RESULTS OF TEST: Twenty-eight charges have been run with the following changes in' the operating procedure: ..... 1. Use of nitrogen instead of carbon dioxide to purge K-9 before charging ODCB. 2. Alternate additions of aluminum chloride and phthalic anhydride to K-9, with initial temperature of K-9 at 15-20t,C., then allowing temperature to rise to 45-50C. during addition. 3. Use of T-21 as well as T-20 as a drowning vessel for charge from K-9. 4. Use of both jet and jacket initially in S-9 to start distillation. 5. Distillation of the charge in S-9 until the temperature reaches 130C. and rides one hour at 130C. since temperature never reaches 150-155C. 6. Elimination of the crystallization temperature as distillation endpoint criteria and .use odor test only. All charges made with the above operational modifications have been of satisfactory quality and have been successfully used to make good quality 2-Tert.-Butylanthraquinone Crude Wet. Recommendations: Continue to operate process with the above cited changes. DUP050467776