Document 5jgXkN5mGg88ny6NzDKeeBMR

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT \ 256 YANDERPOOL STREET NEWARK, NEW JERSEY Serial No. KK-52-4 Copy No. 1 M :V NEWARK PLANT PIGMENT COLOR RESEARCH REPORT RT-423-D BLEED IS SOLVENTS Period Covered June 14 - 21, 1951 FILE: DATE: 4/9/52 Copy tot X -- Huassrlcal File 2 - Research Office (222.24) 5 - Libras? File (222.24) 4 * H. Arnoul - Plant Files $ - J. X. Tully/A. Siegel/Library 6 - fi f Spengeaan/iibrary Serial Ho. 18-52-4 Copjr Ho. 1 NEWARK PLANT FIGMENT COLOR RESEARCH REPORT Final Report Title! RT-42S-D BLEEP IN SOLVENTS Period Covered! June 14 - 21, 1951 Charge! 1101-11-32 SUBMITTED BTi X. B. VET HOOT PATS SUBMITTEDi 3/10/52 DATS ISSUED! 4/9/52 DUP050068924 IBTRODDCTIOS 41tbough tbs "Watchung" pigment*, when dispersed in vinyl on printing ink, are claimedto show no bleed in enter or in the commonly need organic solvents and plasticizers, customers have occasionally reported bleed by their testing methods. Moreover, it has been observed in the laboratory that a alight bleed oen be obtained by mixing the pigment directly with the solvent* The purpose of this study was to determine the nature and extent of this bleed in various solvents, end to determine whether the bleed is due to the method of^mnufaoture or variables in the processing* Specifically, the objectives were as follows* (1) Extent of bleed of RT-428-0 standard, lot 91195, in toluene, MBE-TCP, mineral spirits, alcohol, and hot water* (2) Comparison of present standard, made by direct strike procedure, with an earlier standard made on the isolated dye process* (3) Comparison of bleed of current standard with current production* (4) Comparison of bleed of ET-423-D with competitive reds of tbs "Watchung" type* (5) Effect on bleed of the following* (a) omitting para soap (8-424)9 [b) Patronate substituted for para soap* 0) omitting rosin, 'd) omitting strontium from toner, e) increasing BOB excess from current 2% to former 65*, f) pressoake washed until wash water is colorless, g) recrystallized 2B Acid (8-467) for the diazo* (6) Extent of bleed of sodium salt and acid form of 22 Acid -* B08/(Eed 22)* (7) Analysis of bleed of RT-428-D. .I. RT-428-D, lot 9H95 2* BT-428-D, lot 47706 3 3390-244 4. 3390-242 5* 3390-240 6* 3390-274 7. 1390-272 3. 3390-270 9. 3390-270 10* 3390-272 II. 1390-27F 12. 0-54173 13* C-52209 14. BT-420-D, lot 26220 15. RT-423-D, lot 22067 16. BT-42S-D, lot 28062 17. RT-428-D, lot 28102 12. Bed 22, Sodium Salt 19. Bed 22* laid form Current standard. Earlier standard mads on isolated dye process, laboratory control. Bara soap omitted. Petronate substituted for para soap, laboratory control. Bara soap and rosin omitted. Eosin omitted. BOB success increased to 6jf. Pressoake washed bleed free. Made from recrystallized 22 4cid. Rincon Bed B-616O (Harmon). Citation Bed #1054 (Kentucky). 411 Ca toner, Sr omitted. "OK Straight" plant lot. n n tt ft ft OH DUP050068925 All Maples were tested In toluene* a 1:1 Mature of methyl ethyl ketone and tricresyl phosphate* mineral spirits* alcohol (23A), and hot water according toTF-7201. nrara.riftTnBg ET-423-D shows some bleed in every solvent. Material made on the direct strike procedure currently used in the plant ahowsless bleed than that made from the isolated dye* Current production is running better than standard in bleed* probably indicating there has been seme improvement in diazotization and strike procedures* or in ths quality of the intermediates* since the standard was prepared* The amount of bleed is small* and cannot be attributed to tho use of para soap* rosin or strontium salts in the manufacture of the toner* or to ths reduction in the BOS excess. Although some of the bleed msy be the sodium salt of ths dys* most of It appears to be a mixture of decomposed diazo and treating agent* The bleed is not affected fay the use of reoxystallizsd 2B Acid or by washing the presscaks more thoroughly. The bleed msy be inherent in this type pigment) in any case the competitive samples are no better in bleed than current HT-428-D production. 1, BT-428-D standard* lot 91195, shows considerable bleed in toluol* H8K-T0P, alcohol* and hot water* but only slight bleed in mineral spirits* 2. The current standard* lot 91195* made by the direct strike produoedure, shows lass bleed in all the solvents than the older standard* lot 47705* made from isolated dye* 3* lots selected from current production show less bleed than standard in toluol* HEK-TCP, and mineral spirits* but are equal to somaefcat better than standard in alcohol and hot water* 4* The competitive sample* show less bleed than lot 94195# better than current production in that respect* are no 5* The cause of the bleed is not due to any of the following: a) omitting para soap* b) substituting Petronate for para soap* c) omitting rosin* d) omittingJ** 9) current use of 2 BOH emcees* f) normal washing procedure! in which the preesoake is washed until the waahwater is chloride free* but not necessarily colorless* g) use of 25 Acid as received from Qrchem, without further purification* 6* Although 8T-42S-D may containdye (or free acid depending on the final pH), the bleed of "BT-426-1J cannot be entirely attributed to this* Both the soda salt and the sold form of the dye show less bleed than BT-428-B in toluene and mineral spirits. It would be expected that both forms would show considerable solubility in alcohol and hot water. DUP050068926  7. Lot 9119$ was extracted with hot toluene, the extract concentrated and analysed* the aaouut of the toluene bleed was of the order of 1$ end bid the following composition* 5%/2 naphthol 7% mixture of 808 and Bed 2B acid tarry, resinous residue believed to be a stature of deccespoeed diazo, diazo amine, and treating agent* N.B. 1390* Expts. 2k> 27 H*B* 1379, Kxpt. 38 TP-7201 DUP050068927 s s na &n *2 So3 n3 2o DUP050068928