Document R2dV022NBMBL2xng5dQ48opEk

E. |. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 YANDERPOOL STREET NEWARK, NEW JERSEY Serial No. Copy No. KN-52-9 9 si/|py <) t Period Covered NEWARK PLANT PIGMENT COLOR RESEARCH NEWPORT PLANT REPORT PINAL REPORT PHTHALOCYANINE PLANT ASSISTANCE JULY, 1951 * JANUARY, 1952 FILE: DATE: # 223.* 5/26/52 I HJ3787 DUP050068945 Serial No. !?2-9 Copy No. 9 Copy tos 1. Numerical Pile 2. Research Office (223 **) 3. Library Pile (223=^) b, J. I. Tally/A. Siegel 65*. H. A. Perkins, Jackso" n Lab. (2) 7 E* F, Klenk, Jr., Newport Plant Assistance 8. C. E. Rossee, WiliHington 9 V. H. Chalupski, Newport 10. J. H. Cooper, Newark 11. Extra 12. Extra 13. Extra NEWPORT PLANT PIGMENT COLOR RESEARCH REPORT FINAL REPORT PHTHALOCYANINE PLANT ASSISTANCE JULY, 1951 - JANUARY, 1952 SUBMITTED BY* P. D, Graham, Jr. APPROVED BY* J, B. COOPER DATE SUBMITTED* April 22, 1952 DATE ISSUED* 5/26/52 DUP050068946 mrnvmm. SOMMAM ASP COBCXPSIOTIS A. "Monastral" Blue B Bo "Mcnastrai" BXu BG C. "Monastral" Green A. 4-Chlorphthalic Acid Bo Synthesis and Sulfation C. Solvent Milling Do Extraction E. Quality F. "Emulsification Filtration" "MOHASTBAt" BLOB B8 A. Quality B, "Emulsification Filtration" A* Chlorination ! Addition of Ingredients 2o Chlorination Catalyst 3* Sulfur Chloride Filter 4. Batch Sise 5* "Emulsification Filtration" 6. Jet Masstone 7 Copper Oxychloride 8. Reflux Condenser 9. holding Period at Temperature Be Extraction of Crude Green C. Solvent Milling D. Extraction and Finishing ! Alkaline Extraction 2. Acid Extraction E. Yield w bh w bl PAGE 1 1-2 2-3-** 2 2-3 34 4-8 4 4-5 5-6 6 6-7 7-8 8-9 8-9 9 9-17 9 10 10 10-11 11 11-12 12 12 13 13 13-1** 14 15 15 15-16 16-17 17 DUP050068947 2 EXHIBITS m Exhibit (I) Preparation of V-Chlorphthalic Add Exhibit 12) Solvent Milling of ,fMOnastral" Blue LB Exhibit (3) Acid Extraction of "Monastral" Blue LB Exhibit (k) Quality of "Monastral" Blue LB Exhibit (5) Quality of "Monastral" Blue BG Exhibit (6) Quality of "Monastral" Green Exhibit (7) Standard Chlorination Procedure Exhibit (8) Standard Solvent Milling Procedure for "Monastral" Green Exhibit (9) Standard Extraction Procedure for "Monastral" Green Exhibit CIO) Table A - Newport Plant Chlorination field Table B - Solvent Milling Laboratory Yield for "Monastral" Green Table C * Comparison Green Finishing fields with and without Alkaline Extraction 18 19 20 21 22-23 2^-25-26-27 28 29 30 31 31 31 DU P050068948 KN-52-9 May 8, 1952, mmmxm-This report is concerned with the work of the Phthaloeyanine Plant Assistance Group at Newport from July, 1951 to January, 1952 The ma^or efforts during this period were directed toward an improvement in the tinctorial properties, increases in production, standardization of processes and reduction of manufacturing costs of the three phthaloeyanine colors, "Monastral" Blue IB, Blue BG and Green, produced by the Pigments Department. This report re presents a continuation of KN-51-42 (Ref. 1). The original Newport Phthaloeyanine Plant was designed to produce two CPC pigments, "Monas traln Blue LB and Green, at rates of 22,000# and 15.500#, respectively, per month in a five day week. The basis synthetic processes were developed by Imperial Chemical Industries of England and the Organic Chemicals Department of DuPontI but the present process includes many modifications and novel features resulting from work of the Color Research Group. Operation of the plant commenced March, 1948. There were no provisions in the original project for the production of "Monastral1* Blue BG, the solvent milled chlorinefree species of Blue CPC. It was first produced at Newport in March, 1949 on a campaign basis using Blue LB equipment with no revisions. The omission of 4-chXorphthalic acid in the synthesis and a longer solvent milling cycle, are the only major differences of operating procedure between Blue LB and BG. An expansion of the Phthaloeyanine Plant was started early in 1951 and is expected to be completed by July, 19J?2. The new rated capacities will be 64,000# of Blue (including LB and BG) and 31,000# of Green per month on a seven day week basis. The manufacture of Blue LB at Newport is based on the reaction in a highly refined kerosene, of phthalic anhydride, urea and copper chloride, catalyzed with ammonium molybdate. A predetermined portion of the phthalic anhydride is replaced with 4-chlorphthalie acid, whieh is synthesized at Newport, to produce a low chlorine (3.8-4.5JS) CPC. The introduction or the chlorine in this manner promotes stability to crystal growth in aromatic paint thinners. The synthesis slurry is sulfated with sulfuric acid to facilitate separation of the kerosene,and to Improve the tinctorial properties. The pigment slurry is then hydrolyzed, extracted with alkali, dried and solvent milled to reduce the particle size to a standard strength level. The milled slurry is distilled to remove the solvent, extracted with weak acid and shipped to the Newark Pigments Plant.as a 15$ slurry for the manufacture of toners, lakes and .dispersed pastes. 1 .H DUP050068949 *2 In the manufacture of " Monastral" Green, chlorine-free Blue is chlorinated at elevated pressures and temperatures to a chlorine content of approximately extracted* dried and solvent milled* The milled slurry is extracted with acid and alkali and shipped to Newark for final processing* There were no significant changes in the standard job procedures for the ^-ehlorphthalic acid, synthesis and sulfation procedures in the period covered by this report* An increase of approximately b% in strength by laboratory evaluation was obtained by reducing the ball mill pigment loading 15$ in ten experimental charges An increase in the acetone/CPC weight ratio from 8?A to 10A for solvent milling resulted in a 1-2$ strength improvement. Four new ball mills were installed during the latter part of 1951 for Increased production of Blue LB. The initial production from these mills was weaker and duller than that from the original mills $ but after several weeks , improved significantly. The reasons for the apparent deficiency were not clearly established? however, it was suggested that minor differ*, ences in the construction of the lifter bars and speed of the mills might be partially responsible. The strength of Blue LB averaged 3$ weak versus standard BT~30^~D. The hue and intensity were satisfactory. The weakness, as compared to performance in 1950, appears to be associated with the adoption of two significant cost reducing variables, the "Kerosene Flotation" (KF) sulfation procedure and the omission of the alkaline extraction. The use of ammonium hydroxide was eliminated from the pulp for shipment at a slight savings and as an operating nuisance, with no apparent degradation of quality. The "Emulsification Filtration" (EF) procedure was evaluated as a replacement operation for sulfation of Blue LB? but resulted in unsatisfactory tinctorial properties in the standard plant cycles and was abandoned, B. Blue BG was produced twice on a campaign basis in the last two quarters of 1951. The quality of the first campaign averaged 103:100, ws red and vs intense versus Newport standard BT-297-D, SW 373* This campaign was conducted at a % increase in synthesis batch size. The quality of the second Blue BG campaign was less satisfactory in that a number of charges pro* cessed in "P" mill, which had been out of service for extensive repairs prior to the campaign, were excessively dull and red, DUP050068950 3 apparently indicating inadequate milling, The "Emulsification Filtration" technique was evaluated during the ftovamber, 1951 Blue BG campaign and, in contrast to laboratory milling of the crude, failed to give a satisfactory product in the plant. The sub-standard "EF" lots were rendered usable by a second solvent milling in the plant. Green CPC was produced at the highest possible rate throughout the period covered by this report. Significant improvements in production rates and qyality were realised. The order of addition of Ingredients to the autoclave was reversed, thus effectively eliminating a premature exothermic reaction between the sulfur chloride and CPC, A substantial improvement in quality and a slight increase in the production rate resulted. Antimony trichloride gave a yellower and more intense Green, when evaluated experimentally as a catalyst in place of aluminum chlorides but was not adopted as standard practice In view of a substantial cost penalty associated with its use. A screen-type filter was installed in the sulfur chloride system to remove a sludge of iron and CPC, which, if present in the chlorination, may cause dullness of the Green CPC, A noticeable improvement in intensity was attributable to the use of the filter. The chlorination batch size was increased by 10$ (20$ . above original project size) with no effect on ease of operating or on quality. An additional 10$ increase was attempted for two charges and appeared satisfactory quailtywise, but was not >; studied farther, since it was agreed on December 1, 1951, to dis continue all variable study in the Green process for three months^ The ''Emulsification Filtration" procedure was used satisfactorily for Blue-for-Green crude manufacture in October, 1951 at a significant savings in manufacturing cost. As a result of the process freeze in December 1, 1951, further evalua tion was postponed for three months* A plant trial of a large quantity of aluminum chloride in the chlorination for the purpose of producing a jet aasstoae was successful, as judged from the results of lacquer evaluations at Newark. DUP050068951 -4 - The use of copper oxychloride as a replacement for copper chloride dihydrate was satisfactory tinctorlally on an experimental basis in July* 1951 A critical shortage of the dihydrate was pre dicted, hut did not materialize) consequently, the use of copper oxychloride was abandoned, since a lower yield was obtained in the laboratory evaluation. It was found that inefficient press washing of the crude Green filter cake was responsible for some dullness of the final product. A significant improvement was made by standardization of the process and closer attention to detail by the Operating Depart ment personnel. The elimination of alkaline extraction of Green was tried experimentally in October, 1951. A savings of approximately $10.50 per cwt. Green was estimated for its omission. However, severe foaming in the subsequent acid extraction, which could not he readily controlled, necessitated resumption of the alkaline extraction. Some tinctorial deficiencies ware found to be associated with ineffective acid extraction and washing of the Green. The operation was improved substantially by better maintenance of equipment and process standardization. A yield of 98.45# on a 100# OPC basis was obtained In the laboratory for the finishing operations from solvent milling through to completion. On a commodity basis, the yield was 95.76# or approximately 6# higher than the actual plant yield for the month of November, 1951. In a second laboratory yield study, it was shown that the omission of the alkaline extraction had essentially no effect on Green yield "wonasTRM."jw.ro vn A. 4-Chlorphtiia3i.c_Ac3.a fhe standard job procedure for the manufacture of 4-chlorphthalie acid as described in Exhibit (1) was used through out the period covered by this report. The process is designed to deliver approximately 38 lbs. of organic chlorine per batch, which is subsequently used in the Blue LB synthesis without analysis. B. Sintaasia-ga sulfation The synthesis and sulfation procedures recorded as Exhibits <1) and (2) in KN-51-42 (Ref. 1) were used without change from July, 1951* to January, 1952. DU P050068952 - 5- As part of the plant expansion program, Project 9199, a new sulfator, 100-24-B, was installed. The new tank is essen tially the same as the original sulfator, 100-2H-A, except that it is slightly larger and equipped with a kerosene overflow line instead of a siphon for. decantation of the kerosene. As a result of delays in procurement of equipment, a temporary agitator was used in the new sulfator for several weeks and appeared to he re sponsible for some difficulty in processing. However, after receipt of the designed agitator, it was established that there were no significant differences in the sulfators either from an operating or quality standpoint* c* The standard procedure for solvent milling of "Monastral" Blue LB is recorded as Exhibit (2). With the exception of several The weight of crude CPC was reduced in August, 1951, from 362 lbs. to 31^ lbs. for ten charges to determine its effect upon rate of strength development, A laboratory evaluation of samples removed from the mill after grinding showed that the lower pigment loading would permit milling to a h$ higher strength level than the 362 lb. loading (96:100 versus 100:100, when compared to standard BT-304-B5* However, when the charges were processed in the plant, the 314- lb, charges gave an average strength of 102:100 versus BT~340~D as compared to 103:100 for the 362 lb. loading. Pro duction was continued at the standard rate of 362 lbs. per 21 brs. (102.5# of project capacity), since the smaller charge represents a 13# loss in capacity. An increase in the acetone/CPC weight ratio from 8.7A to 10A was evaluated in October, 1951, The Initial results indicated a 1-2# strength advantage in favor of the higher ratio. An equivalent decrease in the amount of acetone used in the flush was instituted to prevent an overload on the distillation facilities, and the 10A aeetone/CPC ratio was continued as standard practice. Operation of the four new shot mills, purchased on Project 9199 for expansion of Blue LB production, was started as follows* mi Date Lot Oct. 10, 1951 8623 - 308 Hov. 25, 1951 332 "K" Dec. 17, 1951 361 "L" Dec. 27, 1951 383 DUP050068953 *6- Laboratory valuation of plant mill samples indicated a slower rat of strength development in the four new mills as com pared to three of the original mills, "A", "B" and "C", The reason for the deficiency of the new mills was not clearly established; however, several differences that exist between the old and new mills are worthy of mention. The lifter bars in the original mills are flat steel plates bolted to the shell, while the bars in the new mills are semi-circular in shape and welded to the shell and thus provide less lifting action on the shot. The new mills operate at a 4$ lower percentage of critical speed than the original mills, as a result of design changes in the gear arrange, ment, Another possible explanation of the weakness and dullness, experienced when the new mills were put into service, was the unusual difficulty in cleaning the grinding shot. Even after re peated flushes, voluminous quantities of a dark colored contaminant, which analysed 45-65$ Iron, could be removed from the mills. This condition also existed in one of the original mills, "B", which was removed from service twice for extended periods for mechanical re pairs. The tinctorial deficiencies associated with the new mills were even more apparent in the manufacture of Blue BO* (See "Monastral" Blue BG section of this report), Laboratory grinds in small steel mills confirmed the dullness and weakness of the plant grinds when shot coated with rust was used. D, Extraction The acid extraction procedure, shown as Exhibit (3), was used throughout the period covered by this report. The alkaline extraction, which was eliminated from the standard procedures October 1, 1950, was not used in 1951, E. Quality The average monthly quality of "Monastral" Blue LB is shown as Exhibit (4), The hue and intensity were satisfactory throughout the period, but the average strength was 3$ weak versus standard BT-304-P, The average .strength for Blue LB for the first six months of 1951 was also 103 s100 versus BT-304-D (Ref.l). The 1951 average Blue LB strength was 3$ weaker than the 1950 average strength (103*100 vs lOOslOd). The two major changes in the plant, which appear to b responsible for the deficiency, are significant cost savings items, the "Kerosene Flotation" sulfation procedure and the elimination of the final alkaline extraction, which were incorporated into the plant procedures in January, 1951., wad October, 1950, respectively. In December, 1951, when full utilisation of the new mills, purchased on the expansion project, was realized, a number of week (5-9$) and vs dull - s dull lots were produced. This deficiency was associated with the unusual difficulty in cleaning the cast shot used for milling 55 however, after a considerable number of charges, the ultimate strength of CPC milled in the new mills was reasonably uniform and approached the general level of production prior to the installation of the new mills. DUP050068954 7 The average chlorine contest for the last six months of 1951 was b>,36$. The range of chlorine content for 195 lota was 3.6 to 5,0$ with twenty-six of the 195 lots outside the specifi cations (38 to Various laboratory experiments were tried in an effort to improve the strength of finished Blue IB pulp. In the interest of brevity4 only one typical experiment win be reported. Blue LB packed lot 1623 34-7* which was lOVaoo versus standard BT-3C4-D, was treated as follows A, Rewash with 50C water B, Extract with % 12S^. C, Extract with 3$ D Extract with 3% NaOH 102*100 102*100 102*100 103*100 Additional laboratory washing after filtration of the slurry, as well as an extraction with either sulfuric acid or ammonium hydroxide, improved the strength by 2$. A sodium hydroxide extraction was less effective. Occasionally, experi ments of this type resulted in strength improvement, as high as apparently indicating serious deficiency in the extraction and washing in the plant. However, on the average, the improve ment by laboratory filtration and washing was only 1-2#, Elimination of the ammonium hydroxide, which is normally added to the final Blue LB pulp to Insure a pH above 7*0 for ship ment in polythene-lined steel drums, was evaluated by in-process sampling and found to give a 2-3$ stronger product. An extended plant trial did not confirm the strength advantage. However, since an operating nuisance caused by the ammonia fumes coule be eliminated with no apparent quality degradation, the addition of ammonium hydroxide to Blue LB packed lots was discontinued in September, 195U The I}Emulsification Filtration" (hereafter called MEF") procedure differs from the sulfation method of isolation in that the synthesis slurry is pumped directly into water to form a water-in-oil emulsion, which is extracted, filtered and dried, A significant ingredient savings, mostly due to sulfuric acid and sodium hydroxide, is realisable with the use of the "HP* process. DUP050068955 8An evaluation of the "BF1 technique at Newark in the laboratory and Seiui-Works gave very encouraging results for Blue BG (see discussion under "Monastral" Blue BG), hut showed some tinctorial deficiencies for Blue LB. As a result of an anticipated shortage of sulfuric acid, two trials of the "EP" procedure ware made with Blue LB with fall knowledge of the slight inferiority found at Newark. From an operating stand point, the only serious trouble was an excessively long filtra tion cycle believed to be caused by a breakdown of the emulsion; however, tinetorially, the products were considerably inferior to sulfated controls and standard BT-304-D. Compared to standard BT-304--P, the plant quality of the two nEF lots, N623 - 297 ami N623 - 318, was 107*100 and v dull and 102*100, vs green and v dull, respectively. No further experimentation was planned for the use of the "EF" procedure in Blue LB manufacture. A. Quality Two campaigns of "Monas tear' Blue BG were conducted in the period covered by this report. Blue BG from the first cam paign in August, 1951, averaged 103 s 100, ws red and vs Intense versus Newport standard BT-297-B^ SW 373* The campaign was con sidered satisfactory; although from a quality standpoint, the previous campaign was slightly superior. Five of the twenty-one lots were 9 dull or dull versus standard BT-297-B, SW 373, while three were s red or red. The crude Blue, which was synthesized at a % increase in batch sis, did not appear to develop strength to the same level as crude synthesised at the normal batch size. The .alkaline extraction was eliminated from the entire campaign at a significant savings in operating cost with no apparent quality degradation* The standard milling conditions, i,e., 34? lbs. per 30 hours, were used for all batches. No tinctorial deficiencies were encountered at Newark in the conversion of the August, 1951 Blue BG production to BT-297-B* The quality of the November. 1951 Blue BG campaign was unsatisfactory as shown in Exhibit (5). The first eight lots, N657 - 515 to 159, which were milled from crude synthesized at 105% of the normal batch size, averaged 107*100 versus standard BT-297-D, S 373, or h% weak compared to suitable controls at the standard batch size. As a result of weakness and dullness, the milling cycle was Increased from 30 to 40 hours for lots N657 - 163 through 177. Evaluation of in-process mill samples showed a slight improvement in strength and intensity associated with the additional milling. DUP050068956 During the November, 1951 Blue BG campaign, "D" mill was restored to service after extensive repairs to the shell and shaft* All charges in nDM mill subsequent to the repairs were excessively weak and very dull as evidenced by lots 1657 - 162, 165 and 166 in Exhibit (5) The actual reason for the inability of "D" mill to produce satisfactory Blue BG was not conclusively established, but was believed to be associated with the improperly cleaned shot, which after numerous flushes appeared to be clean\ however, analyses of the material removed by the flushes gave *f5-65$ iron on a solids basis, Rewashing, re-extraction with sulfuric acid and remilling failed to improve the quality of the batehes from "D" mill, A small scale chlorination of the sub-standard Blue BG yielded a satisfactory Green$ hence, the batches were scheduled for consumption .in Green production. The chlorine content of the Blue BG in the November, 1953. campaign was satisfactory with the exceptions of lot R657 - 151, which was 0.?#, and lot 1657 - 177# which was 1.5#, as a result of an operating error in which the lot was mixed with Blue I. b. The "EF" process for Blue BG, which is essentially the same as that described .la "Monastr.al55 Blue LB, Section "F", was tried experimentally in the plant in November, 1951 lots N657 I69, 170 and 171, as shown in Exhibit (5) were excessively dull in contrast to laboratory milling of the same crudes, which gave .a strong, green and intense product versus standard BT-297-D* SW 373 The weakness of lot B65? - 169 .as compared to lots 170 and 171 was the result of using 5!D" mill for the first "EF" evaluation, since "D" mill invariably produced a weak product regardless of its method of isolation*. Remilling of the dull HEFn type BG (lot N657 - 171) in the laboratory improved the quality to 85*100, green and intense versus standard BT-297D, SW 373 indicating that the plant cycle of 36 hours was probably inadequate for proper development of the desired tinctorial properties of the nEF" type crude* It was . decided to discontinue plant evaluation of the "EF" process apd refer the study to the Newark $eml-W6xks for further development* mWSMJM0L A. CU.orlaatt.yn The chlorination unit was operated at maximum capacity throughout the period covered by this report*.. A number of process modifications, which resulted in increased production, decreased costs or an improvement in quality, will be discussed separately in the following. DUP050068957 10 In the chlorination step. when th sulfur chloride was charged to the other ingredients in the autoclave, quite frequently, a reaction between the sulfur chloride and the crude CPC would occur, with the temperature rising to b(p - 60C The resulting pigment was invariably dull compared to standard Green AGT~722-D, SW 2609* In August. 1951, twelve experimental ehlorinations were made with reverse addition of the ingredients; i.e., crude CPC added to the chilled sulfur chloride* The' only operating difficulty,insufficient ventilation for fume removal, ms corrected with the installation of a jet eductor. The chlorination cycle was decreased by approximately 30-*) minutes by reverse addition, since the large volume of chilled sulfur chloride <5-X0} cooled the autoclave rapidly," while in the original procedure, a very gradual, addition of sulfur' chloride was required. With th adoption of .reverse addition of ingredients .in September, 1951, production of excessively dull Green was eliminated. a. Ten experimental ehlorinations ware made in October, 1951, with .antimony trichloride (ex J*7. Baker) as a replacement for the' aluminum chloride catalyst. In both the laboratory and the plant a slightly yellow and intense product was obtained versus standard AGT-722-D, SW 2609 and controls with aluminum chloride* In view of the cost penalty for Baker's antimony chloride of approximately S.OO/ewt. Green, .a less expensive grade of antimony chloride arshaw) , which would reduce the penalty to approximately $1.50/cwt. Green, was evaluated. After the first four ehlorinations with the Barshav product, the evaluation was discontinued, since the .heating cycle of the autoclave charge averaged 3-1/2 hours as compared to ' 1-1/2 hours with aluminum chloride* The products chlorinated with Harshawls antimony chloride did not exhibit the yellowness .and intensity of those with Baker!s antimony chloride, but were essen tially equal to those made with aluminum chloride. An extended trial of'Baker*s.antimony chloride ms scheduled. 3* Analyses, of the sulfur chloride, which is recycled in the chlorination, operations, showed an accumulation of sludge, predominantly iron oxide and CPC. The CPC undoubtedly reached the sulfur chloride tank by "dusting" from the rotating dryer. ' Several laboratory scale ehlorinations, made with a small amount of sludge from the plant sulfur chloride, resulted in dullness, comparable to that obtained in the plant. Consequently, it was recommended that, the sulfur chloride be filtered at a point Just prior to chlorination to remove the sludge. An 80-mesh Monel line filter was installed in July, 1951 .and, after numerous operating difficulties were overcome, was used .successfully.. The analyses of the sludge collected in the filter on three separate occasions mg as follows % DUP050068958 - 11 * Solids Extracted Solids iron as Fe smsi 29.5* 23.3 20.0 im/si 30.5# fo.l 8.0 isam 26.Q$ 34.0 20.8 it analyses were made? but: the three shown in the above table are typical, A second strainer (Cuno self-cleaning) was introduced into the pipe line between the rotating dryer and the sulfur chloride absorber. Sine it was & rather small strainer for the amount of sludge being removed* an excessive production loss was .incurred* In addition* the 80 mesh strainer was so effective in removing sludge that it was not necessary to continue evaluation of the Cuno filter. A significant improvement in intensity of Green CPC became apparent with the full-time operation of the sulfur chloride line filter. A second line filter in parallel was installed in December, 1951 to prevent any loss of production during cleaning of the filter. 4. m^Mm The chlorination batch sis ms increased in September# 1951# by X($ (244 lbs. crude C'FC Blue to 268 lbs.) for a two-week period. Eubout evaluation in both the plant and laboratory-showed no detectable quality deterioration compared to earlier controls* In October, 1951 ? the 268 lb. batch, size was adopted as standard practice, resulting in a increase in Green production. A second increase of IQfo in chlorination batch size (268 lbs. crude CPC Blue to295 lbs.) was used for two chlorinations in November, 1951* A violent reaction was encountered' in one of the ...two batches during.the initial heating in the autoclave. The reason for the reaction was not determined| however, it was believed to be associated with the heating rate and not toe larger batch size. The quality of the two experimental batches, by both laboratory and plant milling, was esssmtialiy equal to average production; however, no additional trials were made since the standard Job procedure was "frozen" as of December 1, 1951, for a three-month period to deter mine the uniformity and reproducibility of the process. The "EF" process, which is described under "Monastral" Blue BG, was used experimentally in October, 1951, for crude Blue-for-Green C.PC in six chlorinations. Dots H624- - .670 .and 671, shown in Exhibit. (6), represent toe first plant use of the f,EPM process in Green and were completely satisfactory from a quality standpoint. The approximate savings for the "EF* process, were., estimated to be in the neighborhood of $6.00/cwt. of Green CPC. An extended campaign was scheduled for November, 1951* The quality of the, Green produced from the "IF* type crude is shown., in Exhibit (6) as lots N624 - 695 through 725. During toe extended DUP050068959 12 trial, two operating difficulties were encountered, which may or . nay not he attributable to the ,!E?t5 procedure* In several chlori netions , the pressure during the initial heating rose rapidly to 300 psi The difficulty was corrected by reducing the rate (lower water temperature) of heating* The second difficulty was that of excessively long rotating dryer cycles required for the distilla tion of sulfur chloride By increasing the steam pressure and installing a valve on the rotating dryer jacket for more complete removal of condensate, the rotating dryer cycle of the "BP* type batches was reduced significantly near the end of the trial. Further evaluation of the ,{EF:i process was temporarily discontinued in view of the three-month frees on the standard job procedure. 6. Two chlorlnations ware made in September, 19.51 ns a con tinuation of the jet masstone study previously reported (Ref 1) with quantities of anhydrous aluminum chloride in excess of catalytic amounts* Two-roll mill lacquer evaluations of the ' experimental products indicated that a lacquer masstone approxi mating the depth of GT67lHD Clot 4-51), although bluer, was obtained* The only operating problem encountered in the tried, evaluation was excessive fuming. caused by the liberation of hydro gen chloride when the crude was charged to the extraction tank. ' It was agreed that some investment for fume disposal equipment would be needed if the Newport plant werw required to produce the jet masstone type Green CPC. I further work was planned. 7* In expectation of a critical shortage of copper chloride for the synthesis of CPC, copper oxychloride ex Rohm and Haas was evaluated as a substitute raw material* An earlier evaluation in the manufacture of. "Monasfcral" Blue LB and Blue BG had shown copper oxychloride to be. satisfactory quailtytd.se j however, there were indications of a yield loss attributable to its use. line chlorlnations were`made in July, 1951, from crude Blue synthesized., with copper oxychloride* By laboratory milling of plant crudes, the chlorlnations with copper oxychloride appeared to be entirely .satisfactory tiactorially. Packed lots, N621* - 595* 6 and 7, as shown in Exhibit (6), were produced .from the copper oxychloride .syntheses and are completely satisfactory versus standard AGT-722-D, SW 2609= With the limited, evaluation, it was not possible to .collect reliable yield data. It was concluded that copper chloride dihydrate could be replaced with copper oxy- . chloride in the synthesis of hlue-fpr-green crude should a critical shortage of the former develop. DUP050068960 13 The Andale condenser , which is mod for refluxing sulfur chloride during chlorination. was inspected 9/13/51 after 127 chlorinations. it was found to he free of solids, which in the past, particularly when antimony oxide (Tiaonox) was osed as the catalyst3 collected on the head plate, and blocked the flow of sulfur chloride. Following the inspection, ten chlorinations were made with antimony trichloride as a substitute catalyst for aluminum chloride. After the ten chlorinations. the condenser tubes were completely free; however the condensate return line to the auto* clave was blocked. The analyses of sample from the condensate return line was as follows.? Solids 29,0% Extracted Solids (CPC) 3-o-$% Iron as F@ 16,5$ in December, 1951$ during a shutdown for inspection of the autoclave., the reflux condenser was removed from .service and replaced with a spare. On hundred and sixty*three chlorinations were mad sine the previous cleaning. The condenser tubes appeared to be essentially clean. Condenser inspections -will be scheduled for each 200 chlorinations. 9 Ial&lagwJ3&lJiL In July, 1951* eight chlorinations were made with a three- hour holding period at 1?5C (versus the standard four-hour period) to develop information for deereasing the cycle. The quality by laboratory milling of plant crudes was essentially a standoff with suitable controls at the -four-hour period; however, four of the chlorinations were unaccountably dull. There did not appear to be any significant blueness associated with the shorter holding period. Further valuation of the three-hour holding was abandoned in favor of several more important variable studies. Bo The extraction step subsequent to chlorination appeared to be responsible for some deterioration of Green CPC quality based on in-proeess plant samples Severalexperiments, both in,the plant and laboratory, were made in m effort to determine the source of difficulty. One laboratory grind was made in the presence'of an added contaminant (10$.a a CPC basis Recovered, from the press filtrate by evaporation. The analysis of the contaminant was as follows: * DUP050068961 - 14 - Chlorides 33 3$ Copper 11.35& Total Iron 0.30$ Extracted Solids (CFO) 0.16$ After the standard laboratory milling, the contaminated sample was 121:100 and very dull versus standard AGT722-D, SW 2609? while the control was 94100. a..blue and intense, indicating a very serious milling deficiency in the presence of the contaminant. This is undoubtedly an exaggerated situation; hut does indicate what may 'happen to a lesser'degree when crude Green is not properly extracted and washed. Measurements of pH of .representative samples of each presscake from the crude Green filter press ranged from 4.6 to 6.9 for one particular charge. Laboratory grinds were made of several samples covering the pH range, but no substantial differ ences in quality were found. When one of the samples was acidified to a pH of 2.5 using filtrate from the extraction of crude, a slight loss in intensity was observed after laboratory milling when com pared to a control. A pH of 2.5 was selected for the experiment, since on several occasions in the plant the presscake was found to be only 2.5 after the standard washing. A concentrated effort was made to improve the filtration and washing characteristics of the plant extraction step and, based on in-process samples, a signifi cant improvement in intensity was obtained. c* nm>mmmmi--nn .< The standard procedure for solvent milling .as recorded in Exhibit (8) -was used throughout the period covered by this report with the exception of .an experimental reduction in tae quantity of sodium nitrite. Severe foaming was encountered in the acid extraction, when the alkaline extraction ms .omitted from the process This was the result of decomposition of nitrous acid. The quantity of sodium nitrite was reduced by 50% for ten mill charges with no apparent quality deterioration; however, there was no detectable reduction in the amount of foaming in the acid, extraction. Since past .. experience has shown that one-half the standard quantity of sodium nitrite was not always sufficient to prevent reduction of the.polychloro CPC, no further study of this variable was made. The pH of numerous mill charges was .checked .at the end of milling to determine the alkalinity. If was found that the pH ranged from 7.5 to`9.1, presumably dependent upon the washing efficiency of the preceding extraction step. On several occasions, such as lot 1624 - 730 shown in Exhibit (6), the presence of a brown colored vapor, presumably nitrogen dioxide, was observed after milling even though the .. slurry was .alkaline. Usually, as in the case of lot 730, the CPC Green turned out to be dull-very dull, when-such a condition existed; however, there were exceptions in which the final product was-Intense versus standard AGT-722-D, sw 2609* DUP050068962 " 15 - i* Laboratory evaluation of in-process samples from the plant indicated that the alkaline extraction could be eliminated from the standard procedure for finishing of Green CPC with no loss of tinctorial properties, Tb estimated savings for the omission of alkaline extraction was $X0*50/cwt, Green (or $13*50/cwt. Green if the extraction equipment could be reassigned to another operation), The first plant trial of omission of the alkaline extraction was lot A624 - 671, shown in Exhibit (6), which was made with no operational, difficulty and was completely satis factory tinctorially, Additional trials of omission of the alkaline extraction resulted in a severe foaming problem during the heat-up cycle, although the quality was usually satisfactory, as evidenced by lots USE1* - 672 through 691 compared to alkaline extracted controls, Several attempts to reducing the foaming were made* Oetanol was tried in the plant as an anti-foam agent, but had no apparent effect on foaming* Sulfamic acid, which would react with the nitrous acid liberated on acidification of the sodium nitrite, actually intensified the foaming -when added' 'to a hot slurry in the laboratory. Later trials of sulfamic acid, added to a cold solution in the laboratory showed that the foaming could be reduced significantly* however., no plant trials were made, since the cost of sulfamic acid was considered prohibitive, The foaming in the plant was reduced somewhat by careful control of the heating rate, but sot eliminated, in November, 1951, as a result of the failure of the main ventilating fan for the acid extraction tank,..,it was necessary to resume ah extraction of .CFG prior to the acid extraction to remove the sodium nitrite. For approximately four weeks (November 9 - December 7, 1951), the. CFG slurry was .filtered on tfcc Alkaline side prior to the acid extraction* Starting with lot 162^ * 72S (see Exhibit (6) attached), the alkaline extraction was .again eliminated using a temporary exhaust fan for removal of fumes. The foaming continued and, in several cases, was so severe that it was decided to resume alkaline extraction as standard practice December 26, X9*>1, starting with packed lot N62h 753. 2, Acid Extraction The standard procedure for add extraction of Green CPC, as shown in Exhibit (9),- was 'used throughout the period'covered by this report. The results of-many in-process plant samples treated in the laboratory showed that plant extraction and particularly washing were slightly inferior to the corresponding laboratory pro cedures (I-25& weaker and yvs-vs dull), A concentrated effort' by the Operating Department was .made to improve the washing character istics of the filter press and a noticeable Improvement resulted. Of the samples tested in the latter three months of 1951, less than half-showed shy improvement by laboratory processing# DUP050068963 A series of .laboratory extractions with sodium hypo chlorite was made on .samples of difl.1 Green packed lots to deter mine whether the source of dullness could he removed* The follow ing table very clearly shows the improvement, which indicates that the crude Green is inherently capable of delivering-.quality superior to shipping standards, but as processed under existing plant con ditions was Inferior in intensity* m H62k AfJr^b.jaSSUSSi* 97*100 dull 100*100 equal 97*100 s.dull 101*100 intense 981IOO dull 100*100 vs intense 9? *100 v.duii 101*100 vs dull 100*100 dull 104:100 Intense 93*106 dull 103 *100 intense 93*100 dull 103*100 intense 98:100 dull 100 *100 intense 95*100 dull 100*100 Intense 96*100 dull 99*100 intense 95ilOO ws blue,vs dull 100 *100 intense 97*100 ws blue.ws " 101*100 intense 100*100 s.duii 100*100 ws yel..ws int 98*100 s.blue,s,dull 100*100 blue, vs intense 99*100 dull 102*100 intense 100*100 s val ,, ..dull 104:100 intense The yield in the chlorination area, i.e., from crude Blue to dried crude was calculated and compiled batchwise for the third-quarter of 1951 as shown in.Exhibit (10), Table A. The "Average Goal*1 was determined by multiplying the weight of crude Blue charged to the autoclave by the purity (based on extracted solids) by the goal conversion factor* The "Actual field" is the percentage of goal based on a batch weight tabulation with purity analyses for every batch* A thorough laboratory yield study of the finishing area, i.e*', solvent .milling, distillation of acetone, acid extraction . and packaging, was made using one-half Pint mills. As shown in Exhibit (10), Table .B, the average purities of the crude and finished Green-was 95*91$ and 98.57$* respectively. The actual yield as 100$ CFG. was 98.4$$, On a commodity basis, ignoring purity of both the crude and finished Green., the average yield of the laboratory study was 9576$. On a comparable basis, the Green finishing yield for the plant .in Bovember, 1951* .was' 89,39$*. or approximately 6$ less than laboratory performance. DUP050068964 17 A second laboratory yield study was made in December, 1951, to determine the effect of omission of the alkaline extraction of Green CPCo The results of four lots, bandied very carefully, show that an average yield of 98.. 5$ was obtained when the Green received both the acid and alkaline .extraction as reported in .Exhibit (10), Table 0* When the alkaline extraction was omitted, the average laboratory yield for the same four lots was 9806$* IffiEREHCM: (1) KH51*^-2 Pigment Color Research Repost - Newport phthaioeyanine Plant Assistance * January., 1950 - July, 1951. (2) 2007-X97 to 253 Newport Phthaioeyanine Plant Assistance .Notebook$ October, 1950 - October, 1951* > (3 ) 2007"25e- to 268 Newport Phthaioeyanine Plant Assistance Notebook; October, 1951 - January, 1952* (V) CPC Weekly Quality Reports * Plant Assistance File X6JU (5) Phthaioeyanine Plant Assistance Monthly Summaries ** File 7. (6) Newport Plant Production Resorts * Plant Assistance File 4-f * > DU P050068965 - 3.8 - mmuu To mix tank #1 add? 256 gals* water* Start .agitator* 500 Its* 50$ WaOH solution, 236 lbs. phthallo .anhydride over a 4-5 minute period.* Cool to below 5oC. pump to glass-lined 750 gal, chlorination..kettle jacketed with brine* Cool contents of kettle to 8C, Then add; 250# chlorine uniformly over a h hour period., holding temperature' between 8 and 12C. Agitate 30 minutes* Measure pH and adjust, if .necessary, with chlorine or 50$ HaOH to hJjJ-uB, Then add: 238# KaCl over a 30 minute period. Adjust pH with MCI to 1*5-1,8 adding HC1 over a 30 .minute period* Filter slurry in #17 filter press* . Air blow 15 minutes* Discharge filter press into press pan* Solids Total chlorine - 35$ Inorganic chlorine 2hf Organic chlorine Presscake weight v 770 lbs* DUP050068966 "19" mm&Mi to a 122? gallon steel Jacketed hall mill., 6* x 6% loaded with 21*000 lbs. east 1/8H shot, adds 362 lbs# dry 13 erode CPC OS max. kerosene). 275 gals* acetone (jainiwixa purity - 98,5g>. Mill for 1 hour. ' Then adds 110 gals, acetone* Mill for 5 hoars. Then adds 165 gals, acetone. Mill for 15 hours (Total milling time is 21 hours). Then adds 100 .gals, acetone. Hotats mill a few minutes and pump charge to solvent recovery equipment. Then adds 100 gals, acetone flush. " .Pump flush. DUP050068967 20 a&MSISiU3i Dilute contents of the aeid extraction tank #i-7> which may contain either two or three will chargee from which the acetone has been distilled, to 60'* with water. Heat charges to 9?G with sparger steam. Add: 200 Its. 78# sulfuric acid. Record pH. Hold charge at 95G for two hours. Start filtering In 51 or 57 press - Press to !f0 p.s.i.g. Press wash to 2000 ohms or fiye hours, whichever is sooner. Discharge filter press'to ribbon mixer. Add. water to mixer to .approximately solids, Mix 1-1/2 hours and pump to storage tank. * DUP050068968 - 21 Moattulear July, 1951 Aligns t 1951 Sept. 1951 Oet* 1951 Bov. 1951 Bee. 1951 Lots, H623 - 186 to 215 B623 ~ 216 to 247 H623 -. 240 to 281 B623 282 to 319 H623 - 320 to 329 B623 - 330 to 380 EXHIBIT (4) 102 *100 s green, s.Intense 104:100 vs green ,vs intense 102 *100 vs green,ws intense 102 ilOO ws green,ws Intense 102:100 vs green. 104:100 vs green, ws dull "A DUP050068969 22 QPALITI g? "HOlMaiatt". B.TOS-BS. Lot tear >57 129 - 131 * 132 * 133 - 13V - 135 - 136 * 137 - 138 - 139 - l4o - l4l - 142 - 143 August, 1-951 55 t* ft SI ft ' 1? u t? ts tl r? ft T# .ft n IS ft f.t ts ft tl S is - 144 * 145 - 146 - 14? 148 - 149 - 150 rt tt tl ts S3 ts n tt ts (I ft it 18 w - 151 - 152 November, 1951 n - 153 fS 5? - 154 Si <5 e x h ib it (SI Quality w BI-897-D. SW 373 102*100 vs red,9 Intense 9 101*100 vs red, s intense 103*100 intense 104*100 vs green, vs intense 102*100 s intense 103*100 s intense 104*100 s intense 103*100 s red, a dull 101*100 vs red, s dull 106sXOO vs red, s dull 106*100 vs intense 1011100 vs red, vs dull 104*100 vs red, vs dull 103*100 vs green, s intense 103*100 intense 100*100 red, dull 101*100 vs red, vs dull 102*100 intense 106*100 b red, dull 105*100 s intense 106*100 vs red, vs intense 106*100 a red, s dull 1078X00 s intense . 108*100 s intense 108*100 vs intense DUPO50068970 Lot M57 ~ 155 -157 ~ 158 * V59 - 160 - 161 * 162 - I63 l&* - 165 - 166 - 167 - 168 - 169 - 170 - 171 - 172 - 173 - 17** - 175 - 176 - 177 " 23 EXHIBIT (?) Coat'd. lovembex4 .?195i n tl tt It tt II ft ft n it ft tt it n tt it tt it 11 >t 11 tt n tt tt tt it IT n it a tt n it n tt tt tt 1138100 red dull 108*100 ws red ws intense 103*100 vs intense 103 ?100 ws red 107*100 vs red, vs dull 103*100 ws red, ws dull 110s100 red, dull 105*100 vs dull 103*100 vs Intense 210*100 s red, s dull 110*100 s red, dull 103 *100 ws dull 103*100 vs green, vs Intense 116*100 v dull 100*100 v dun 100:100 v dull 109*100 vs red, dull 103*100 vs green 103*100 vs green, ws Intense 102:100 s green, s intense 103*100 vs green, s Intense 95*100 red, dull DUP050068971 EmMLS*X OSH! OF E,MONASTRAIrt OHOT CPC PRODUCED 2fj&& SmliiX vs ..AS^:^2rR.-gW.21S2 wI* IS It n si ft ii ft it it {! M I? ft K n o n t* f 981IOO doll 9-8.HOO dull 97*100 dull 975100 dull 9.8*100 dull 955100 v dull 95*100 v dull 96*100 dull 98*100 dull 100*100 dull 97*100 s dull 98?100 dull 981100 dull 98*106 dull 95*100 dull 96*100 dull 95*100 vs dull, ws blue 975100 ws dull, ws blue 100*100 wo dull' 99*100 vs intense 101*100 vs -yellow, vs intense 99 5100 S intense loo? 100 m yellow, vs intense 100*100 vs yellow, ws intense 1001100 ws yellow, ws dull 99*100 ws yellow, s dull 599 August 600 601 602 603 u t! tt 6w 605 606 It, n n n si 609 610 it it 611 612 613 is ft 0 mn 615 616 n .n 617 618 n ft 100*100 8 dull 97*100 V dull lOOslOO vs blue, dull 10b*100 vs yellow, ws dull 99slOO vs blue, vs intense 99*100 S blue, S dull 93s100 s blue, s dull 96100 s blue, s dull 95*100 blue, vs intense 1001100 dull' 101*100 dun 100*100 ws dull 100*100 s dull 100*100 s dull 1005100 dull 100*100 vs yellow, s dull 100*100 vs yellow, s dull 99*100 dull 100*100 s yellow, dull 100$100 vs yellow, dull DUP050068972 Packed Lot N-621* 619 620 621 622 Si 625 626 627 628 629 630 N-624 - N-62*f - - 25 - BBBaXi&t coat'd. 'MBtoSb n s; s? ts IS ft n ft itptetiber f* IS ft ss IS ft n M Vi n it 0 tt 1! S3 {8 IS 5S ft October " n " 0 n * n ?l s? " t8 mam, 100 s 100 vs yellow, vs doll 100*100.vs yellow, dull 971100 vs line, s dull lOOslOO vs yellow, dull 99*100 ws yellow:,dull 98$100 vs yellow, vs dull 100*100 vs yellow, dull 99*100 dull 100*100 vs blue, s dull 97*100 ws blue 97*100 ws intense 97:100 vS intense 97 sXOO intense '97slOO vs intense 99*100 ws blue, vs intense 99*100 s intense 98*100 ws blue, vs intense 98*100 dull 97*100 vs blue, vs duU 98*100 vs intense 100*100 vs blue, vs intense 101*100 vs dull 100:100 vs dull 100*100 dull 100:100 vs yellow, s dull lOOslOO s yellow, v dull 101*100 s yellow, dull ' 100*100 vs yellow, vs dull 100:100 vs yellow, s dull 101s100 s dull - dull 95:100 v blue, intense 981100 v dull 92 8100 blue, v dull 95*100 s blue, duU 97*100 $ blue, s dull 98*100 s blue, dull 99s100 vs blue, s dull 981XOO intense 100*100 s yellow, vs intense 100*100 yellow, s intense 101s100 yellow 100*100 yellow 101*100 s yellow, vs dull .100*100 s yellow, s dull lOOslOO s yellow 99*100 vs yellow, vs dull 100 % 100 ws yellow, vs dull 101*100 vs yellow, 9 dull 100*100 ws yellow, VS dull DUP050068973 Packed Lot 668 - 66$ - 670 * 671 - 672 :6M . 675 - 676 - 677 - 678 N624 679 680 681 682 683 68M- 68? 686 687 688 - 690 - 691 - 692 -m 6fi9y3j1 -- 669965 - 697 - 698 - 699 - 700 - 701 * 702 - 705 - 706 - 707 - 70S - 709 - 710 - 711 - 712 - 71h - 715 - 716 - 717 26 - Mont) October n tt it it .n n n t? n iovember n n n xt n n t* n n 51 n ts u u TS n n n VS H n n mmMJfl Coat'd. ;ii.MT^Z2g^_svL2609 101:100 vs yellow, 101:100 yellow 100*100 vs yellow 100*100 s intense 100:100 s intense 102:100 dll'll 99*100 intense 100*100 s Intense 100*100 ws dull 100*100 s dull 102*100 dull dull 100*100 ws dull 100*100 ws blue 30*100 vs blue . 100:100 s blue, vs Intense 101*100 s blue, s dull blue 100*100 vs blue, s intense 99*100 s blue, vs intense 99*100 blue 95*100 blue, s intense 97*100 blue , s intense 100*100 s blue, vs Intense loo.sioo dull 95*100 blue. Intense *100 blue, s intense 97 ao.0o0 vs blue, intense ws blue, .vs dull slOO vs dull dull 100*100 vs blue, vs dull 100*100 dull 101*100 dull 95*100 dull 97*100 of .00 dudlul n 97*100 vs blue, vs dull 97*100 dull 97*100 s blue 101s 1.00 dull 100I100 s dull-dull 98*100 vs blue, vs dull 98*100 s dull 97*100 s blue, vs dull 101:100 duH 91*100 v blue, s dull 93*100 v blue, dull 100 *100 dull 100*100 blue, dull 102*100 dull DUP050068974 DUP050068980 BBritartutefc N62'h- - 718 - 719 S6Sfe ~ 720 721 Month N''ov e mber December * n H R R It tt It ft It It It ft tt ft ft It n it it it R ft ft It H mmuLm <****, mmsurnJmzTmi^M^ma^ 100*100 s blue, doll 104*100 v dull 101*100 dull 101*100 a dUU 101*100 dull 108*100 a yellow, dull l$f*100 vs yellow, dull 109*100 yellow, dull K&*100 v dull 101*100 a dull-dull 102*100 dull 101*100 dUU 97*100 v dull 100*100 duH 100*100 vs blue, a dull-dull 103*100 dull 104-*100 dull 103*100 dull 103*100 s dull-dull 104*100 s dull-dull 103*100 vs yellow, vs dull 101*100 ws blue, vs dUU 103*100 dUU 103*100 dull 100*100 vs blue, s dull 102*100 dull 101*100 dull 103*100 dull 101*100 dull 103*100 dull 103*100 dull * .. r 103 *100 dull *v 101*100 dull * Jr 102*100 dull 100*100 ws blue, vs dUU, 99*100 vs blue, dUU ^ 100*100 s blue, dull 97*100 blue 96*100 blue, vs Intense 97*100 vs blt*e, vs dull 96*100 vs blue, s intense DUP050069012 28 mmmMX NEWPORT STANDARD CHLORINATION PROCEDURE AS. To the 400 gallon nickel-clad autoclave adds 3400 lbs# sulfur chloride containing 6?#5 ~ 69.5JC chlorine When temperature of sulfur chloride is 30C or lower, adds 268 lbs# chlorine-free Bliss CPC rosene content 27 lbs* anhydrous copper chloride (Hawshaw). 15 lbs. anhydrous aluminum trichloride (Ohio Apex). Bolt manhole cower. Start water through Andale condenser. Heat with hot water (65-68C) slowly to 50C, shat off water and allow reaction to occur. When pressure is under control, heat with steam to 175C Hold at 175C and 265 psig for 4 hours. Cool charge to 130C, want pressure to 40 psig and drop charge to rotating dryer, 100-213# Hush autoclave with 500 lbs# sulfur chloride and drain to rotating dryer# / - 29 - masuxi m*htms o l v e s t o f "h o n a s t h a l " To a 1227 gallon steal jacketed tall mill, 6* x 6** loaded with 21,000 lbs. cast 1/8" shot, add* hOO lbs # dry crude Green CPC (maximum volatiles content of ijO bo lbs* sodium nitrite* bO lbs. trisodium phosphate. 360 gallons acetone (minimum purity - 98.5$) Hill slurry for 2b hours. Pump charge to acetone still. Add* 100 gallons acetone to mill, rotate 5 minutes and pump flush to acetone still* DUP050069014 ~ 30 mmm,ssa EXTRACTION OF SOLVENT-MILLED "MONASTHAL" GREEN To two Green CPC mill charges slurried in water in the alkaline extraction, 100*231, add: 150 lbs * sodium hydroxide solution (5050 . Dilute tank volume to @M with water, heat charge to 95C with steam and told temperature at 95C Tor two hours. Filter at 90C or above, press wash to 3000 ohms or 8 hours on "A" wash and 1 hour on "B" wash. Discharge press to ribbon mixer* DUP050069015 October, 1951 November,1951 December,1951 31 nmjMmMmm urn Average Goal Average Actual Weight Actual 456. 470.4* 471.7# 427*8# ej.e 442.6# 93*67* 92.58* n.m f (10i (1) Green Batch No* ,,, 830 831 833 834 835 836 837 .839 Avg. TABLE B - SOLVEST MILLING LABORATORY YIELD - "t^HASTEAL" QWm (2) Ext. Solids of crude 97*24* 96.43 96.43 95*95 95*61 94.18 94.44 97.02 Crude Wt. as 100* CPC 12 x (2) 11*67 g. 11*57 11.57 11*51 11.47 11.30 11.33 11.64 (4) Recovery ffoa 12 g. > 11.57 g. 11.59 11.51 11.43 11.47 11.43 11.48 jl.45 (5) Extracted Solids Fin ished Green -104 54 98.41 0.81 98.45 98.40 98.02 9$.$t 99.12 (6) <7) finished Actual Wt.as 100* lield on CPC (4)x<5) 100* CPC basis. XfeUJi 11.40 97.69 11.41 0.62 11.37 11.25 11.29 98.27 97.74 98.43 11.20 99.12 11.35 100.18 11.35 97.51 95*91 98.57 98.45 TABT.E C COMPARISON OF GK15KII FINISHING YIELDS WItB AMD WItEOOT JJASALliK MTRACTION 895AA 895A 925AA 925A 927AA 927A 929AA 929A 94.75 94.75 96.41 96.41 95.95 95*95 95*85 95.85 11.37 11.37 11.57 11.57 II.52 11.52 11.50 11.50 11.48 11.48 U.45 11.53 11.51 11.64 11.47 11.64 AA Alkaline and Acid extraceed A * Acid extraction only. 98.70 0.03 98.03 98.01 98.57 0.25 98.75 98.09 33*32 11.25 11*22 11.30 11.35 U.31 11.32 11.41 99.6 99.0 97.X 97.7 98*7 98.4 98.5 99.3 DUP050069016