Document wgJmaMM38mXOZ9jojG1nynjD

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Sori.1 Now KM-4a-29 Copy No. X Numerical File NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report SEMI-10RKS AND PLANT DEVELOPMENT AND STANDARDIZATION OF ALKALI RESISTANT RED TONER, RT-531-D, Poriod Covorod, *** 1944 - APRIL 1948 221.32 FILE: DATE* 1/3/49 V N42176 DUP050067066 Copy to* #1 - Numerical File 2 - Research Office (221.32) 3 * library file (221.32) 4 - #10 Building File 5 - V. Chalupski, Plant Files 6 - W. F. Spangeman, Newark 7 - Extra. Serial No. KN-48-29 NEWARK PLANS PIQUES? COLON RESEARCH REPORT Final Report SEMI-WORKS AND PLANT DEVELOPMENT AND STANDARDIZATION OF ALKALI RESISTANT RED TONER, RTw 531-D. MAT 1944 - APRIL 1948. Charged to* 1100-12-40 (AIC-40) S "TED BY* J. Rasa C-J-U*4 APPROVED BY* DATE SUBMITTED* 1V18/48 DATS ISSUED* I/3/49 DUP050067067 mwmmmi tom sales volume on the light shed# alkali resistant red toner, RT-531-D* made it des Irakis to continue manufacture in the semi-works for a considerable period (April,1941 through Apr11.19425 see KH-42-248). RT-531-D production was then inactive until Hay, 1944- when a plant trial batch was made- This was followed by a return to semi-works production (May - June, 1944). Finally, it was decided to dis continue the practice of manufacturing low sales voluss colors in the semi-works and plant developmant work was resumed in June, 1944* SUMMARY 4k COSCLUSIONSi An extended prototype of Iff* 531-&-designated BL-544-D, had been atandardised in the plant in April, 1944. On the basis of a decision to rsstandardlse RT-531-D to conform tlmctorially to the toner component of the lake standard (light, strong and yellow versus the Rt-531-D standard semi works lot 5239) a revised Jt-1447 procsss (lower coupling temperature) was used for first plant manufacture. Ths product obtained was similar to that obtained In toner control samples obtained from plant lake production. After the plant trial, semi-works production was resumed to supply material for stock- Seven batches made using the low coupling temperature variable (90F instead of 113F) were all of ths light, dull masstone, strong, yellow tint type- Reproducibility of the formula appeared to be excellent but a change in the lot of rtHaphthanll" AS used had a noticeable effect on masstone and tint- A blend, lot 43471, of these seven semi-works batches with two of the early plant batches was in use as an unofficial standard for HT-531-0 from July, 1944. Lot 43471 was not accepted by Sales as ths official RT-531-0 standard, however, until December, 1945. A new standard RT-531-0 formula, K-2429, based on the revised K-1447 process used in the manufacture of the component batches of lot 43471 was used ae the basis of all plant manufacture during 1945, 1946 and 1947. Plant manufacture continued at a slow rats during this period, with considerable variation in masstone and tint quality. On the basis of previous process duplieability data available it would appear that tinctorial variation was principally due to changes in intermediate quality from shipment to shipment, An attempt to set up an RT-531-D standard during this period which would be based entirely on plant manufacture was unsuccessfulThe proposed standard, lot 49298, was rejected by Rales Service because of unsatisfactory light stability and bleed resistance. An increased amount of Para soap was used in subsequent pro duction in an attempt to improve light stability. So significant improvement resulted, indicating that Para-nltro-ortho toluidlna (the first component) quality deficiency might be responsible for the light-fastness disadvantage (based on laboratory data). DUP050067068 2 Finally, late in 1947, it was decided to set up a plant standard based on current quality, and lot 83950, a blend of eight plant batches, was submitted for evaluation and was accepted as standard in March, 1948# A comparison of lot 83950 and lot 43471, the previous standard, follows! Varnish dryer reboot* Lot 83950 vs lot 43471* dark - OK - ws strong - vs blue Light stability* inferior Bleed resistance (soap)* a.superior A new formula based on the revised process was issued as RT-531-0 (B) and the Production Division accepted supervision of plant Rf-531-0 manufacture In April, 1948. mmmm The procedure used for the first plant batch of BT-531-0 (Kay, 1944) was based on a modified K-1310 process in use for plant manufacture of RL-544-D (extended RT-531-D). The formula used was desigued to give a lighter, stronger, yellower product and differed from the laboratory toner process, K-I447, as follows1 1. The coupling temperature was lowered from 113F to 90F. This is the effective variable* 2. The dlaso volume was decreased 15$, and the stirring time after coupling and the heating time to reach development temperature were lengthened in accordance with the RL-544-D process which had been previously reduced to practice* The resultant product was slightly light, dull In masstone, about 20$ strong and yallow in tint varans ths RT-531-D semi-works standard, lot 5239 Cbasad on the K-1447 process). Control samples indicated that the product obtained was a fairly close match in strength and tint to toner control samples from current lake manufacture but that masstones differed over a fairly wide range* This had been a problem with lake production and apparently was a function of variation in intermediate quality. In an attempt to prove this and at the same time build up stocks of RT-531-0, a series cf seven batches wars made in the semi-works. A series of four batches made from the same lots of Para-nitro-ortho toluidine end "Haphthanil" A3 were lighter, stronger and yellower than the standard, lot 5239, and close checks to each other. A change in the lot of BAB used gave a darker, ' duller and bluer product* A revision of the diazotization pro cedure (omit heating of the PHOT to solution in dilute acid) appeared to give a somewhat lighter and more intense masstone, slightly yellower tint product* DUP050067069 3 Plant production was resumed in June, 1944 using the modified K-1447 process* Two hatches were made during the remainder of the year* quality was variable, particularly masstone* apparently due to a change in the lot of HAS used* Four plant hatches (1356 pounds) were made during 1945* AH of the manufacture was dark and dull versus the new RT-531-D standard- lot 43471. hot 43471 is s blend of the seven semi-works and the two plant batches mads during May, June and July of 1944 adjusted to the desired strength with about 5% Blanc Fixe. A rubout comparison of lot 43471 and the semi-works standard follows> hot 43471 vs lot 5239* It., dull - yellow, intense - 10j$ strong - yellow, intense* Production rate was increased during 1946, twenty*three hatches were made. Quality varied over e wide range in tinctorial characteristics with manufacture averaging very slightly dark in maastone. OK in strength, end slightly blue and dull in tint versus the standard, lot 43471. Tinctorial variation was, apparently, principally a result of fluctuation in quality of the intermediates, PHOT and HAS. * A new RT-531-3D standard formula, K-2429 (subsequently the "A* process) based on the procedure in use in the plant, was issued in October, 1946. The principal variation from the laboratory process, K-1447, was* 1. The bateh size was out from 1.0 mol to 0.8 mol. 2* The coupling temperature was lowered from 113F to 90F* An attempt to set up a plant standard from batches mads during 1946 (July - September) was unsuccessful. A blend of five plant batches, lot 49298, submitted for evaluation in October, 1946, was rejected because of poor light stability end a deficiency in bleed resistance by the American Bank Rote test (reported in January, 1947)* Twenty-five plant batches were made during 1947. Many of these batches were mads with an increased amount of Para soap* (36 pounds per batch), in an attempt to improve light stability, laboratory information indicates that the amount of soap formulated for the "A" process (24 pounds per batch or 30 pounds par mol) is the minimum para soap amount that will give satisfactory light resistance* There was, apparently, no significant improvement in light stability obtained with the increased soap variable* Tinctorial quality continued to vary over a considerable range with the average performance being similar to that obtained in 1946, that is, dark, slightly dull masstone,equal strength and slightly blue, dull tint tarsus standard lot 43471* DUP050067070 -4- Laboratory raw material teats on both the PHOT and HAS show that both ingredients play a part in the considerable mass tone and tint variation from standard, There are no sufficiently powerful light, intense masstone or yellow, intense tint variable* available for correcting the dark, dull masstone and blue, dull tint effect obtained with sub-standard raw materials. Available laboratory information indicates that sub-standard PHOT is also responsible for poor light resistance* Finally it was decided to set up a plant standard basad on currant manufacture* Accordingly, a blend of eight plaht batches, lot 03950, was submitted for evaluation as a new RT-531-D standard in December, 194?. A comparison of lot 83950 with lot 43471 follows* Varnish Dryer rubout* Lot 83950 vs lot 434?ljt dark - OK - 2-1/2# strong - vs blue Light stability* inferior Bleed test (soap)t slightly superior* Lot 83950 was finally accepted as standard in March, 1948* A new standard formula, 81-531-0(8), based on the process used in the manufacture of the components of lot 83950, was issued in April, 1948. The "8" process differs from the "A" process (K-2429) as follows1 1. The formula is set up on a stepwise basis* 2. The usage of sulfamlo acid in the diazo is doubled to insure removal of the excess nitrous sold* Failure to remove this excess gives dark, duH masstones. 3. The Para soap was increased 50# <369 Instead of 24#) to insure maintenance of light resistance* The Production Division acceptsd supervision of plant RT-531-D manufacture in April, 1948. iamiimi There is no patent restriction on the manufacture of RT-531-D. It is not believed that this study has resulted in any patentable developments. GLOSSARY* RT-531-P - a buffered acid coupling of PHOT and HAS. BL..544-D - a 25# extension of RT-531-D on whiting* PHOT - Para nltro ortho toluldlne. , BAS - "Haphtbanil" AS$ the anilide of beta hydroxy - naphthoic acid. DUP050067071 Semi-works Plant DSN-48-27 DSN-48-27 Part I Parts I ami II DUP050067072