Document QgQM3GxGp47wZe7Dj4aZ7vno6

*13 OPT E. X. DU POUT DS NEMOURS & c o mpas i INCORPORATED NEWPORT, DELAWARE PIGMENTS DEPARTMENT eci 0. Ev Ros.se film. J* S* Booge - * F* C. Evans - Newport 7* H. Chalupski ~ a C, J Higgins - " J* H. Tully < Newark A. Siegel, * File Newport. Delaware April 13, 1951 J. H. COOPER NEWARK This report is intended to summarise experience with subject process, which was evaluated in the plant April 10- 1951. The acid flushing process, which consists of dissolving a CPC synthesis slurry in a relatively large quantity of 9$?TsulfurtG acid (7 parts per part of CPC) and drowning in water, offers a substantial improvement in quality and a means of obtaining an essentially kerosene-free crude pressoake. The plant trial was scheduled solely for the latter advantage, since adequate facilities for drying crude CPC are no longer available in the plant. Serious equipment limitations and several operating difficulties prevented a thorough evaluation of the *AF process$ however, it smj be concluded that a number of major equipment changes would be required for continued operation. It is not believed that acid flushing could b adapted to present equipment at forecast production rates. Since it appears that Newark will be successful in drying crude CPC for the Newport plant in tray dryers, and, since Newport is not properly equipped for acid flushing, the secondary goals, improved quality and crude CPC that may be useable without solvent milling in certain codes, actually beeMae more important than a kerosene-free crude presscake. Accordingly, it is planned to determine the equipment and investment that would be required for acid flushing. The acid flushing process is attached with comments showing the reasons for conclusions presented herein. The scheduled second trial of acid flushing was cancelled in view of the equipment limitations plus the fact that the synthesis intended for evaluation had reached 21#C (specification is 195-200*0} and pumping diffi culties requiring an excessive volume of diluent kerosene were anticipated. ' A PDG,JR/gh Attach P. D. GRAHAM, JR CHEMICAL DIVISION r t MID FLUSHING PH0PS3S Haafeiag 1 Pump entire synthesis slurry from synthesis kettle to steam still. (Seme difficulty ms encountered pumping the charge* More kerosene ms required for diluting and flushing than desired. The temperature in the still was 103*0, which is considerably lower than Semi-works experience (150*0.) 2. Add 6,200 lbs* H2SO4 (98%) to the sulfation tank. 3 . Pump synthesis charge into sulfator over a 60 minute period* (Approximately 5 hours ms required for pumping 82% of the charge into the acid due to line stoppage and the volume approaching the capacity of the tank* It was necessary to decant the kerosene from the sulfator prior to flushing the remaining 12% of the charge. The pumping troubles required steaming out pipe lines, which introduced water into the charge; consequently, a complete solution ms not obtained* An additional 1.600 lbs, H2SO4 was required to give a slurry that could be handled,) 4, Discharge acid/pigsient solution to the hydrolysis tank leaving the kerosene layer in the sulfator, (Due to the inaccessibility of the sulfator and inadequate equipment for measuring the levels, approximately 100 gallons of kerosene ms inadvertently discharged into the hydrolysis tank,) Drowning 1, Bun 2,400 gallons of water into the extraction tank, which is to be used for drowning the acid solution. 2, Pump one-half the acid solution into the extraction tank, (Fumping difficulties were encountered which re sulted in drowning two-thirds of the charge instead of half.) X. Add 50$ HaOH to the extraction tank to a pH of 9,0 - 10.0 using extreme caution* (The tank foamed over ae a result of inadequate volume making it necessary to filter about one-third of the charge on the acid bide before the required amount of UaQH could be added.) 2, Filter in press 33A or 33B* 3, Mash sulfate free. (After 24 hours washing, sulfate ms still present* It ms necessary to discharge filter press to avoid additional production losses.) A DUP050069487 N42017.01