Document VodJ52kGOGgrzG8ky1RbOQxo

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Serial No. Copy No. X Numerical File /f//' A // NEWARK PLANT ^ PIGMENT COLOR RESEARCH REPORT Period Covered; Final Report ALKALI RESISTANT REJ> LAKE, RL-544-D SEMI-WORKS AND PLANT DEVELOPMENT AND STANDARD12ATION JANUARY - OCTOBER, 1944. 2/22/49 FILE: 221 DATE; NJjMTB N42199 " Copy to* 1 - numerical File 2 - Research Office (221) !: Library File #10 Building (221) File 1: V. D. Chalupskl, Plant Files B. Killian, Newark 7 - Extra Serial Ho, KH-49-15 Copy Ho. 1 NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report ALKALI RESISTANT RED LAKE, RL-?44-P SEMI-WORKS AND PLANT DEVELOPMENT AND STANDARDIZATION. JKANUARX - OCTOBER, 1944. CHARGE* 12-40 SOTipED BXi i. J. Hess APPROVED BX* y, 0. Morris DATE SUBMITTED* 2A4/49 DATE ISSUED* 2/22/49 DUP050067191 Serial So. KH-49-1? mm. Copy Ho* HL-544-D Is ail alkali resistant light red lake tor linoleum which found considerable use as a replacement for Molybdate Orange daring the war-time lead shortage* It is equivalent to a 25$ extension on Whiting of the RT-531-D toner iPHOT --^ NAS). This study was started about two years after the first Semi-Works trial of this color, then designated K-1310 (see KN-42-248). Upon satisfactory conclusion or the Semi-Works study and as sales volume expanded, the process was taken to the plant* mmjUmsmsmL The early Semi-Works lake manufacture using the K-1447 toner process had been on the dark, blue side of the laboratory standard, K-1310. For this reason it was decided to use the reduced coupling temperature variable in order to obtain a lighter, yellower product. Results on the Semi-Works production using the modified formula Indicated that process duplicability was satisfactory but that a noticeable quality variation was obtained with a change in the lot of "Raphthanil" AS (the second component) used* The f irst Semi-Works batch in this campaign was set up as the HL-544-D standard, lot 6989* The remainder of the Semi-Works material was blended to give a fairly satisfactory match to this standard and was shipped to fill existing orders* Plant manufacture was then started using the modified process* The first five plant batches ground out on the dark, dull masstone, strong, slightly yellow tint side of the Semi-Works standard* However, even though a number of different shipments of both of the intermediates PHOT and HAS, were used, results within the series were fairly con sistent. On this basis it was decided to set up a blend of this material, lot 42876, as the first RL-544-D plant standard* Subsequent plant manufacture varied over a fairly wide range* Attempts to develop an H0K straight" procedure were nullified by raw material variation. Blendable material was made by the use of a number of variables as required. These included* 1. Coupling temperature variation to control depth of masstone and strength and hue of tint* 2* Settling of the dlazo prior to coupling to obtain a very slight improvement In masstone Intensity* 3. Control of the nitrous acid excess in the diazo before coupling to vary depth and intensity of masstone. ---- - - - , . ............. DUP050067192 -2- 4. Increasing the agitation time after the diazo addition to insure completion of the coupling reaction prior to heat development. Shis is done to insure maximum masstone intensity. 5. Change in the supplier of the "Haphthanil" a s . General Dyestuffs1 counterpart for this inter mediate, "Sephtisdr' AS, gave light, intense masstons products* She successful production of light, intense shading material from the General Dyestuffs HAS mas one of the principal factors involved in the blending of much of this manufacture* Upon completion of the plant variable study; a new standard mJ544p formula, K-2018, (subsequently designated RL*544-D(A)) was issued and tha Production Division accepted supervision of manufacture in October, 1944* DISCUSS ION Semi-Works production of HL-544-D was started in January, ' 1944. Bight batches were made during the period January - February, 1944, using the low coupling temperature modification (90F instead of ll3F ) of the K-1447 toner formula. The first of these hatches, lot 6989, was set up as the BL-544-D Semi-Works standard in February, 1944. A rubout comparison of lot 6939 with the laboratory standard, K-1310, and the first Semi-Works trial hatch, lot 4599 (made in 1942), follows; Lot 6989 vs K-13101 s.dark - 10-15# strong - yellow* Lot 6989 vs lot 4599* light - 8-10# strong - yellow, intense* Subsequent Semi-Works manufacture made using a different lot of *Haphthanil* AS were slightly dull in masstons and slightly blue in tint versus the new standard but ware blended and shipped to fill existing orders from Armstrong and Sloane-Blabon. c Plant production using the modified process was started during the latter part of February, 1944. Two different lots of PHOT and three lots of HAS were used in the manufacture of the first five batches. Although all of this material ground out on the dark, dull masstons, strong, slightly yellow tint side of the Semi-Works standard, these batches were fairly close tinctorialiy despite the introduction of the raw material variable. In view of this, a blend (adjusted for strength) of these five plant batches, lot 42876. was set up as the plant B1-544-D standard in April, 1944, A rubout comparison of lot 42876 versus the Semi-Works standard, lot 6989, follows* Lot 42876 vs lot 6989* dark, dull - 2# weak - s.yellow, vs.intense* DUP050067193 -3* Meanwhile, plant manufacture was being continued* Results again started to vary somewhat with change in the raw material ship ments, particularly in the case of the ^ptataall" AS. A Humber of variables were used during the period March - July, 1944, in an attempt to control quality performance. Although the ultimate goal of developing a satisfactory "OK Straight" process was not reached (apparently due to raw material variation), practically all of the production was blended satisfactorily* The variables used In the plant manufacture and the results obtained follows* 1* Coupling at 100? and 105? Instead of 90P was resorted to in order to obtain darker mas stone and bluer tint products as needed* 2* Use of a 20-30 minute settling period for the dlaso before coupling in an attempt to increase masstone Intensity* A very slight Improvement resulted but the products were still on the dull masstone side of standard* 3* Control of the nitrous acid excess In the dlaso (before coupling) to vary masstone depth and intensity* Complete removal of the excess with sulfamic acid (negative test on KX - starch paper) gives maximum lightness and intensity of masstone and is the normal procedure* Attempts to adjust the intensity of the test on the KX - starch test paper for control of masstone quality is compli cated by the fact that the dlaso alone affects the test paper to some extent* 4* Agitation of the coupled slurry for 45-60 minutes instead of 15 minutes in order to insure completion of the coupling reaction prior to heat development appeared to give a slight advantage in masstone intensity* 5. The use of "Hapbtbl*3 48 Fine (supplied by General Dyestuffs) to replace the Dupont "Naphthanll1' AS was the single most effective variable for obtain ing desirable light, intense masstone shading material* Soma of xhev"Haphthl!f AS shipments gave slightly dark masstones but all material was at lesit equal in intensity to the BL-544-D plant standard* The light, intense masstone material made with the General "HAS" was one of the principal factors assisting in the satisfactory blending of the plant manufacture* DUP050067194 A new standard formula, X-2018, based on tbs process then in nee, was issued in July, 1944. K-2018 (subsequently designated HL-544-D(A) differed from the modified K-1310 process (based on K-1447 toner instead of K-1260) as follows* 1* The batch alee is decreased frees 1.0 mol to 0.8 mol to fit available plant equipment. 2* the sodium nitrite amount has been increased from 56 pounds to 56-1/2 pounds to insure the presence of an adequate excess of nitrous acid throughout the diazo stirring period. 3. It has been found possible to destroy the excess nitrous acid with 3 pounds instead of 5 pounds of sulfamic acid on a plant scale. 4. The diazo volume is maintained *as is** after dlazotizatlon and is not adjusted to volume. The. net result is an approximate 18# out in diazo volume before coupling. 5. The diazo is settled 20-30 minutes before coupling, 6. The acetic acid used for precipitating the Haphthaniltt AS is increased from 96 pounds to 98 pounds to obtain the desired very slight acidity before coupling. 7. A coupling temperature of 100P instead of 113F is used. 8. The toner slurry is stirred 45 minutes instead of 15 minutes in order to Insure the completion of the coupling reaction prior to heat development. The Production Division accepted supervision of RL-544-D plant manufacture in October, 1944. nmM'Mmmm There is no patent restriction in the manufacture of Ri544-D. It is not believed that this study has resulted in any patentable developments* GLOSSARY* BL-$44-D - An alkali resistant red l*ke equivalent to the approximate composition* 25#HT-53I-1> 75# Thiting (calcium carbonate) BT-531-D - An alkali resistant red toner, a product of the coupling of PHOT and HAS* DUP050067195 5 PHOT - Para nitro ortho toluidlne* HAS - ',Haphthanil,* AS - the anilide of beta hydroxy naphthoic acid* EH-BHIKEHIAl DETAILS. DSH-49-15. DUP050067196