Document 1oMQXkqarkLR1devmjopprod

V- WGK ANALYTICAL RESEARCH AND DEVELOPMENT TiEPORT No 1771 , November 19, 1970 OTHER LOCATIONS GENERAL OFFICE W. G. KRUMMRICH PLANT B. Corlew R. McCutchan D. Armstrong W. Engman W. Krull D. Jackson R. Blowers pLE/.b'i TITLE! Aroclor 1260 Quality Problem, Status Report No, 2 PERSONNEL! J. Gloeckner, K. Schutzenhofer, D. Roth (H. J. Horner PROBLEM! Aroclor 1260 produced by Dept. 246 is out-of-specifications on after corrosion chlorides. justification! To produce quality 1260 Aroclor and retain sales. summary. A series of chlorinations in a laboratory scale unit using various sources of raw material were performed. Also side by side chlorinations were made with the plant equipment and the laboratory unit in the department. No positive solution has been determined to date. A designed experiment of the plant cblorinators and specified variables has been started. if: y D. Roth dy 0196793 CONFIDENTIAL wok m rev. j. ee Thls report Is tb** property of Monsanto Ccmpcry and the recipient Is responsible f^r l*s sof-kecplng and disposition. It contains confidential lnformo*'on of Monsanto Company which must not be reproduced, revealed to unauthorised persons or sent oufslde the company without proper outhorlxoflon. This roporf Is to be retained In a secure file or destroyed. TOWOLDMONOQ57316 AR&D Report No. 1771 Page 2 November 19, 1910 Department 2*16 has encountered problems in production of Aroclor 1260. The material is out-of-specifications on after corrosion chloride and sometime out-of-specifications on the Monsanto stability. To determine where in the process the bad material was made, crude 1160 from each of the batch chlorinators was distilled and porocel treated in the laboratory. All five were out-of specification on after corrosion chloride but good on Monsanto stability. This indicated that the problem was not in the distillation step but either the chlorinator or raw materials. To evaluate raw materials, a laboratory scale chlorinator was charged v.lth plant biphenyl and catalyst. Bottled chlorine was used. The material produced was good quality 1260. A second chlorinator run made using biphenyl purchased from Fisher Scientific and bottled chlorine also produced good quality 1260. This would indicate that the biphenyl raw material was satisfactory to produce quality 1260. To evaluate the chlorine supply, the laboratory chlorinator was moved to the department and connected to the plant chlorine supply. The chlorinator was charged with crude 1151! and chlorination continued to 1160. Laboratory distillation and porocel treatment produced in-specification material. The plantproduced material was out-of-specification. A side-by-side run of a plant chlorinator and the laboratory scale chlorinator was performed. The plant chlorinator was charged with biphenyl and catalyst and mixed for 10 minutes. This material was sampled and used to charge the laboratory chlorinator. Materials from the chlorinators were distilled and treated with porocel in the laboratory. Again the laboratory scale chlorinator produced quality material and the plant out-of specification. Comparison of the variables common to both chlorinators showed three areas of difference, (l) Starting temperature of cnJurination: plant was 110"G; laboratory lbOC; (c) tnj.ora.ne addition rate: plant was stepwise of too, 800 and 1200///hr; laboratory was constant; (>) Demister: plant chlorinator has one, laboratory did not. The laboratory chlorinator was adapted with a demister and a second side by-side run performed. The laboratory chlorinator was controlled in starting temperature and chlorine addition rate to correspond with the plant. Laboratory distillation and porocel treatment produced in-specification material for the plant and out-of-specification for the laboratory chlorinator. Pi ant distillation and treatment did not produce in-specification material. OH*79* AR&D Report No. 177a Page 5 November 19, 1970 A designed experiment involving the four operating plant chlorinators is planned. It will include the changing of the following variables. (l) Doubling the charge of PeCl3 catalyst. (?) Increasing the starting temperature to 150C. (5) Increasing the finishing temperature to 190C. (^1) No change - to establish a base. This work is currently being performed and will be reported in the next status report. nil, ' D. Roth dy 0196795 TOWOLDMONOQ57318