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E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Serial No. KN-48-5 Copy No. 1 S', NEWARK PLANT PIGMENT COLOR RESEARCH REPORT \ RH-4I7-D, RS-482-D, and RM-484-D PLANT DEVELOPMENT AND STANDARDIZATION OF THE DIRECT LAKING PROCESSES FOR EXTENDED WATCHUNG* BED COLORS. Period Covered: February 1945 - September 19*7 ^ ,, ri FILE: DATE: 5/20/48 N42154 5orial Mo. KB*485 copy * X Copy tot #1 Jfrworioal JFil* 2 * Research Offioo (222.24) 3 * Lih*a*F m# (222,24) 4 - #10 Building Filo 5 - V. Chaiupaki, Plant filos 6 - Xnperial Charaieal Industries* Ltd. 1 m a g * a 9 * * F* Spengeoan, Hewark 10 * Ixtra wmmtum p ig me n t c o l o r r e s e ar c h r b pc s it Final deport Titlo* RM-417-D, RE-482-D, and RM-484-D Plant development and Standardisation of the Direot Xaking processes for Extended "latehung? Rod Colors. Period Covered* February 1945 * Beptestoer Xf47# Charge* 1100*12*33 (4-10*33) 3U3MIT3SD BY* B. J. Boon DATE STOMimD* 4/28/48 DUP050066929 Concurrent with the development work on the RT-428-D diroot Inking prooeee in the plant (non Export KH-47-21) a similar study wa started on tho extended pigments derived from thin toner, namely, RM-484-D, RE-482-D, ami RM-417-D* Tboro has been no laboratory or Semi-Borks Study on tho diroot Xakiag prooeaeeo for tbeoe oxtondod *atehung* red color** .................. h m-c s c -d Tho early plant production! RM-484-D waa baaed on the K-2089 tolar formula (diroot coupling, l*a, diaco into BOS aolution) In lino with experience on tho toner tho suctorial waa wary dal! in naaatono and blue and doll in tint eraua tho RM-484-D "isolated dye* otandard, lot 32639, and waa unsatisfactory. Use of tho reverse ooupling variable (BOH aolution into tho diaso) inoreaaed masatone Intensity but depth waa aleo increased* Strength and intensity of tint were inprorod, A proposed otandard, lot 44778, bloadod from two of thoao batahoa adjusted with whiting to standard atrangth by rubout waa rejected beoauae of a alight atrangth deficiency by linoleum composition grind* 4 second proposed otandard bated on this preoese, lot 48157, (a blend of eight batahoa) was rejected as being too dark and dull in aaaatono. Lot 48X57 waa out-of-line dark versus a board mix of the now diroot Xaking atandard for RT-428-D, lot 47X85, adjwatod to RM-484-D atrangth with Siting, Application of tho inereassd ooupling folutca variable at used in the 202235 toner formula to lighten maaatoaa gave fairly satisfactory parforwenea and a proposed standard bland, let 48624, baetd on material of this typo waa sdmlttad for evaluation* Preliminary teste indieatad that this mix was a trifl# too atrong end tinting atrangth waa adjusted (lot 49090) to give tho following rubout cosparisonrssult* versus tho "isolatod dyo* standards Lot 49090 vs lot 32639s dark, dull - OK * * strong * bine* This material was in-line in aasatone and tint with the RT-428-D direct Inking otandard, lot 47185* Based on the acceptance of lot 49090 a* tho RM-484-B atandard by Bales a standard diraot Inking formula* K-2264, waa written and ilia Production Division assumed supervision of manufaotur* In January, 1947* Meanwhile, aocoptanoo of this otandard was with-drawn because of a very alight deficiency in alkali rosiatanea in linoleum. Sales was reluctant to request one of our major customers to accept this deficiency beoauae of their rejection of a proposed otandard on another color under dollar eireumstaneos* The Production Division lmedlatsly returned manufacture of Rlf-484-D to Ohcadoal Division supervision but shipments wore continued on tho bads of th# let 49090 typo material* DUP050066930 4....'..'";~ i 1 2- Curing the development study and during tit* period subsequent to the rejection of the proposed standard a number of problems oosneoted with production rote, quality and yield control, end the filtration operation, wore encountered* The problems and the correotir# measures taken are listed below* 1* The possibility of using rat washing with the direct laking fcrania was considered*' This was ends neoeeeary by the ebrenie bottls-seek resulting froa tho non-availability of wash presses at the tins* Because of tho high concentration of the standard 1*5 mol bateh in tha 10,000 gallon etrika rate eatiafaotory rat washing was practically impossible* 1st washing was only praetioabla at a bateh sits of 0*75 nolo* da this was economically the rat washing study was 2. As in tha eaao of RT-428-D, deficiencies in the amount of Rid 2B acid used per bateh resulting from tha uae of erroneous supplier* a analyses were corrected by analysis and adjuetSiia&ei of the Rod 2B aeid sodium salt solution in tin rat prior to diaiotisation* Those rat analytes indicated that the supplier's figures wore approximately % too high* Available data do not Show any notabla yield improvement with tho ooarrected batches. 3* Masstons control was established by tho use of an acidification etep after heat development of thetoner far light aasstone and tho uao of Inoroaeod caustic coda in the *08 solution for dark masatone# 4* Abnormally long filtration time, resulting from the difficulty of cut the hoary foam from the development rat, were Corrected by the use Oetanol as an anti-foaming agent* 5* Considerable diffieulty with plate and frame breakage resulted from attempts to press the standard 1*5 mol bateh in a full press volume of $0 eubio feet* A filtration study indicated that a pressing relume of 68 eubio feet atuap prase loads] was needed for the standard 1*5 mol bateh else* On the basis of tha above study a new standard formula, K-2425, was written to rapines K-22&4, incorporating the Red 2B acid sodium salt analysis, tha use of the aeid after heat dsrslspmeat| the s$dttpref foaming agent, and the inereased pressing volume An alternate ibrvlla,;K*2426, to fit a 50 eubio feet press wee alee written. r Subsequently, la order to make mere efficient uae of the 50 eubio feet presses, the batch else was inereased to approximately 2*2 mol# to fill two full prose loads (lOQ oublc feet relume), this new press**, K-2506, differs from K-2425 primarily in that the batch sis# is increased by approxismtely 1,5 times, the BOR volume before coupling is decreased by approximately 30 and the large diase volume necessitates that diasetisatien be accomplished in the coupling rat* Finally, in July, 1547, let 49090 was re-submitted to Sales as a standard for HM-484-D and after contact with the easterner the material waa accepted* The Production Division accepted supervision of RM-484-D manufeoture in September, 1947* DUP050066931 -3* The first flint production of 88*417*9 mo oloo bated cm tin K2089 toner formula (direct coupling, i*o, diaso into BOB solution), Difficulties with dull masstonss and tints similar to the* experienced with RH-484-D ooro eorreeted By application of'ths retort* coupling variable* A proposed RB-41T-D standard, lot 48l50| was properod By mixing throe batches aado on the reverse coupling formula* At first tltlo lot woo rejected for otnndnrd because of ito dark, dull masstone cooperad to tba "isolated dye* RM-417-D standard* lot 29113* However, whoa it was shorn that lot 48150 mo o oloso meatono match to an extencioa Of tho BT*428-D diroot Inking otnndnrd* lot 47185* the materiel me otthedtted to oelooted customers end mo finally accepted as tho RH-41T-D otnndnrd in August* 1948* A formal* based noon that used for the eoraaoaant hatehes of tho new standard ms sst % ns ths S1I-417-D standnrd formula, K-2266* during February, 1946* Meanwhile, while smiting aeoeptnnoe of tho nor otnndnrd* n mrinhlt etudy similar to thnt outlined for RM-404-D ms run. A return! of the romilto ohtnined follows* 1* As ms ths case with B8*484*D manufacture, analysis of tho Bod 2B sold odium ealt solution ohowod that tho suppliere analyses on this intemedlats averaged shout Sf bighor then tho aetunl figure* Oorreotion of this deficiency apparently gar# an approximate *lf> yield improvement, 2* Slightly lighter msostenei were obtained by inoreaclng the diaso wolmss before coupling by about 3QJC* Uee of the sold treatment after host development m n mob more effective meant of obtaining light msetone ^material* liaeetone depth is increased by a 2-3)1 lnersnss in tho caustic soda used for dissolving ths BOB* 3* Difficulties with foaming during hsnt development which reeultsd laextsndsd tat wash-out tiass worn eorreetsd by ths addition of Ootnnol ss an anti* feasing agent* 4* Vat washing mo not practicable because of tho high eonocntratlon of the toner slurry and ths consequent poor settling characteristics* 5* Tho pressing volume far ths 1*5 ml bstsb ms increased from 5 to 88 cubic feet in lino with experience with RK-484-S* , Muoh of the above information ms ustd In revising ths K-2266 fornula to put it on a mere practical basis* Analysis of the Bod 2B sold oolutloa* addition of aoid after host development* use of Oetanel no an antl-fonn&ng agent* and inoroaso in tha filtration relume were all incorporated in the now standard 1*2483 formula sot op in December* 1946, K-2424, an alternate formula, doolgncd to fit a 50 cubic foot pressing voluas* ms sot up at the seme time* tho Production Division aeoepted supervision of HH-417-D manufacture in January, 1947* DUP050066932 The loir asles velum and potentially large batch aie of ibis BjL extension of RT-428-B for paper made it difficult to Ha# up o development tudy floi this color because of the co*g>aratively few batches undo* Bated on the reculte obtained on too batches manufactured during this period the following conclusions any bo drams 1. it a batch sise of approximately 3/3 ml (2043#) either revere* or direct coupling nay bo uood* the ditto volume io low enough in the eaoo of the dirsot coupling to permit addition of the diaso in 15 miautoe or less. Bat caching nay aloe bo uood at thia batch site* 2. it the regular 1.5 solar batch oiso (8819#) the regular reverie coupling procedure oust be used. The nettling rate is poor oo that press washing it noeeioary* Both of the betoho wore dote obsess to one mother and were graded dull - 305 otrong * blue by bruehout versus the "isolated dye" RI-482-D standard, lot 27822. After strength adjustment, theoe batches were dose in onsetone and strength but blue in tint versus the otmdard. i new dirsot Inking standard RE-482- formula, K-2267, mo sot 19 in February, 1946, to rcplaee the "isolated aye" typo proeodur*, K-9349. Thi# ... process me of tho 1.5 ml else using a toner formulation similar to RT-420-, X-2235. An alternate formula, cne-half tho K-226? batoh else, to fit in a 5000 gallon vat mo cot up at the cane time and designated K-22T7 * Revised HE-482-D formulations baaed enthe now toner formula, JC-2422, were net up in December, 1946# The variable* used were the Rod 2B add anal/sis, use of Octanol, etc., ohangss previously disouoood. K-2427 mo not at the i* normal 1.5 mol (8643#) *ico The K-2428 alternate procedure me cot up on * 0.75 atol (4321#) dee to permit rat washing if desired. Because of the low production velum tho "isolated dye" RK-482- standard, lot 27822, mo retained* The Production Division accepted supervision of RE-482* manufacture in January, 1947# There ie no patent restriction in the manufacture of Rod 2B colors. It io not believed that this study lues resulted In any patentable developments. g|ggggggg RM-484-P A 45J( extension of RT-428- on Vhiting. aosmemampeeaa^w ^m w RM-417-D A 42< extension of RT-428-D on an equal parti mixture of Alumina hydrate and lane fixe. DUP050066933 *5' BE-482-D An 8-l/# extension of RT-428-D on a 90-10 mixture of Barytee and Afcudaa hydrate* The caleiua-atrontiun a&lt of the coupling of Red 2B sold dlaxo and Beta hydroxy naphthoic acid. All Galelua Rad SSI dyeatuff pigment*. Rod 2B Aoid Orthoohlor meta tolaidine para eulfonie acid* Bata hydro*? naphthoic acid* Preparation of the finished pigseat from the haaio intermediate* without laolation or removal of the aether-liquor free the dystuff. JUI-484-D C8R-48-1 Parte I * U RM-41J-D and RS-482-D* 088-48-2. DUP050066934