Document Rj8Qq2NDLgXee26Y9RMzQLOeV

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPQOL STREET NEWARK. NEW JERSEY Soria! No. KN-48-41 Copy No. 1 NEWARK PLANT PIGMENT COLOR RESEARCH REPORT cykm. mar o o n SEMI-WORKS DEVELOPMENT Period Covered! June 1948 - September 1948. FILE; DATE; April 1, 1949 NJS379 N42187 ~ ' ----- Kumx'loal ytii# Reoearch Office (210) Library file (SO0) m V, ChalapaJd, PlaatFUt j Serial No. 1 mm pl an t Title* Copper Hereon SBslJtfoi* Cerralopoint Period Covered! Jme 1948 - Septenber DUP050067139 aliffilifam** **,*&&** iiA 4uii*> *Bw Mn^ndeai Corooration thnnuh antnl muft of irtudv i<i<< tsftb&l^it if producing & w*>'roflw copper fwfocufsoldt p^|pnm%.i PeteiDt teetlon was applied for and the product fees marketed ae the RBH 3900 maroon. rTun* 1948 the du Pont Company esquired theprivilege to manufacture Copper Karoon on a nsnlt? soaraont feaWiw wik inttOfehemical <*%e*t to awwiiir p*ip5pi P "'p ip w w pp w ^PflglP ^^p pPw^*"<P|g wPpWOOWwfKlw^^O* wt<i & saai-works procesa fr***"* ytymty <>tvii 4 , smm m mcmiam ,* Upon o&aplatisn of necessary alterations -to saBi^works i^iijnssti antiifwatmp of Conner Rp592D vas tBdtrtokn **1^* tfai tp^wn* f *1 Doreonnel fin Mtr^ailiu* A Aiz of tha first ton t<fc 0713. p^ppppp^^p ijjp^p^F p ^p p p pp *p*p 'P"* p^"p "pa ppfpp^pp^poo tw ^jppa p p p p pvpjB4B prp pppi^ap .air^^^^^ppoompaafl^ .omapTr p p*<w^jp^s wu evaluated and established ag standard. A formula with <mwxy<w motes '^p ^ppp*pppp ppppipp^Bpp ep^ppwppp '^"O p p pp'W'^^wpPHi^^p p p ip *w ^oRoa,pp^i^aai^^^Mip ueesi^B.' ssafsese^awss .aa# established as standard syuiufft^turing procedure and supervision of aasfpVQrka * manufacture i*wti e#**#*1^ ly th# Production n^pi yt<^t ?>: *> '- ' . 1. , $t*-. '' : Production of Copper Karocn on a *aaiwork* scale ia anticipated until *"PTM' twfttittttKt PoPf A&t mP^^PwP jg&kifi it dftlirfPtb*PlsP to lH6llftOftOPI^PP.^PP PPPP tPoP & "" wtflBfjlKw^PPP goaliePP^PPPppPP^p ., L vi *<-> * d!kto&3w~ ' / . 2n the manufacture of B5920 acidified sulfate is mm lata-a near tiling solution of poiaasitBS ferrot^yanlde solaytonaith _ The nrocess ahtait from MenaiiaiPi^ pp ^pw-pp^p* atolladp^WVP^PPP tar Intsrchemlcal pp p p pfpwppppi ^PPPPP diredtjy ,in oamipvorks dwelopaont studies. CuS0*.5Ha0 Water .Interchemical ---------------- mL 16 lbs. x 48 <9*8 pi.) du Pont' 160 lbs. 480 (58 gal.) imv*. 5J^?it 352) 0.12 Strike ia 60 minutes late K*F <CH)6.3H0 29*5 Water 0 118 (34.2 gal.) Valasts field (Set.) Stir 30 minutes '` 4 20 4*4 cu. ft* 135 3.2 9CI6I 1180(U2 gal.) 6<52 ^t. ft* , '30 ^ 2800 240) 10 m ft* am ;r The following eoiismaat ehang^a wsre essential before B*592>>0 oeuld be aada in our iMsdamabei 1. the copptr tad ferrooyanide solution eats ware fitted li&b beating ooils to present froei epon steam whlfh airfit result la off duds oroduets*^^*'jgppP^ POTp p PPP PPp^PHF Pr^PP.*PSWSp^ DUP050067140 ,.;S': 4 "Lishtnin" v es iueteti fa ths u*Mwg yat to ppovl4t the necessary vortex type agitation, $ Facilities were ts&de to safely dispose of the cyanide gag idinB off durian tin nooMoi a<i to tha avanid* la the filtrate tram, the press (is m Homo Report on Copper Hereon dated July 26, X94R). r* All of the batches ware mmto on the formula given above. Washing ituMfi pirtnnlil tlmi< mt44iiMit ai| h mMu c fitiiltid u$m& tin W ^^p'P^^p ^p ^pSW^W;^^P^Pim^e ~yWp ^*eeMmfcWwmOgy '^P *0*^woo^OPO 0*00 OMSt h M^MppiO^p . f' wastied fox* three hour with water at 140*F follond tWi awid water *<*^p*iwfa^p .pv# p*a# pwp^pjp p p t v ^^p p p ' pp'ppp mi^yvp w o *o|ppoaWF"^^p ^wwesppo p p w w p h io F^vmswpn ^^pp*^JfcQpwOOj^O'..- for shout IF hours. Later In the development two batches were struck eonweatlvely end tressed as oisa. Mi is now conwtt standard orootice.j^p*p ^ppip *^^w p 'Pp *p " p wfpw ppw ip p p^^^p ^P ^pppp pi^^p <^aap^p.^p^o Although most of the material was close to the KBB*3900 maroon (C#5012) to color sees iMffimdfaf as?|wf4,i;ftp<i Iw Aafllwitinp rubOttt results* "The CSUSS a^^^pp p^^^ppp^pp ^^ppapapi^p ^p.f p u m"Siy ^p ^p w f w w ^^p s s p f ^, ^p j ^p p p TMp ^p p ^p p p p f p^^mc t p mp.p f f p wF|^p^.pes ,p p p pp p pp p j e. pa ^b f iMf w h o , aawe b s s b s o p wswwespfliF of this was probably the absorbtion of Moisture by the pulverized pigment which oausee the cob* to beeeme lifter. He variables wore developed to produce material but laboratory experiments landieete the possibility of producing dark M^torl by the addition of IBS end liaht mtrt#l hr the addisimi of eotasaiwa #f>-M# * Considerabla difficult? mo experienced In filterdns Cooper wap**** In the laboratory. waMwp it imsosslbls to establish *ho ^ yield in aime wpdp ^pppp^^p^*^^a.aper^y jy *^^*^^**^| ee M*m^p^aM^weF^eae^^ai^p p pSf e^^^OF'^ppsei^pe e*ae ^Qjpp^^iMd dy'^ea^wjjMeM Opes ssewlS ee|aWi^^Sp|a ey the proposed standard was analysed for copper and by aseming all the copper to bo precipitated a theoretical yield of 464 pounds (tm strikes) was found. ftdJ figure aeeaed aueh too hi^i eoa^arod with aotnsl yields. IHo goal yield of 436 jxwinds was therefore established by averaging tho yields of six batches* Further experimental details may be found in DSH-4&>40 and 8.B, 1220. mterehaolcal has awlied for natsnt wotestlon for tha orocau far^f 1.a^*^^eee^F^^soe aw^^se ^w w p^. ^p^pa^^o^mieeso ewe ^wee^w ewe e^^F^o-O^sip e *f p producing Copper Storoon. DUP050067141  */ ?Af.A'< Ft. r. u Ibur-idiur Y0 i I. C '/? Vi, ..:r. io > .. '.Mi ZO pigment. ore -.fM frcp 3 .t)-TMiir:h t ErYv^r? fir.- and coupled to aeefcoacpt'vrrfuotolui'S Ida and & cornet 1 bive **ifch Harmon?s B~2 and Imnsrialf a Sumatra idiot X-Oto^tl, fhe YT true of issmidine Taller Yo svetr-ior in li ivtfartrso or l is more stable in certain ao.pXlc stdorr than the A'U.. C'cn r-rt' ' : 'cceci by ''"P-^YQ^D* AtT.-^oi(K-.-YChi; ,<:>?. icueXooed in the laboratory to correct a strength Ynf > o? one*/ >n >:' .. original orpdnct, Anv>64"'l givos ateroximately 10 v-'rear strength and has lower anuaenurin* cc c-tt- than *C~J?:K4 * Van rield nrc increased from OQ,,i$ to of theory> Yronos.3v73.se Yf]Y.' rY y ;} differs from -.-2194 in the following: 1; Ircre-v.sc4 batch si-se from 41** -a flO-f, 2. karvnt of sulfjrlo a Yd ir t*;- r.tv.-oseo raiu-cod from 3.5 mo Is to 2.,5 mols oar 1 ,0 -mol bCb.<, "y folur'i Acctata (,vf vir i c so ; *. : .< etic acidf reduced in amount from ?,,*? rnolr. to 5.0 ncls ere 1 .0 -ol DC;3., 4. forcoeronm-s of 2GC \fAf) ,, tr Ira `cased from 13C (59P) to 5c f: ; 5;?. ocra of cov-lY v-; i rev nr. of from 15G {59F) to 3Q0C <G60f), 6. tuenrViiTit war elicii?nted. 'i'he follu'./lng control opines and variables for the process were observed n the laboratory- !,, DuPont BOB an! V.cursor. DCS ore irtnrchan^cRble, 2. AaOT from ESI and C & 0 are interchangeable* 3. , Clarification of the tetraso is necessary to maintain light massbone and intensity- cf tint , 4. elimination of oxcoss nitrous, acid by meant of sulfamic 'acid' tended to -give s 0Tf.su ;hat lighter ' tootone.. 5. Prolonged stirring of the caustic soda solution of AAOT should be avoided because of the resultir;* adverse effect on masstone. 6* Seduction In the amount of sodium acetate. i.e* caustic soda and acetic acid, baler' the formula amount (apcroxlmately 5,0 rr.ols cer mol of DOB) uill result in darker FT and' lower strength, Increase in the sodium acetate tends to give lighter masstone, however with increased cost DUP050067142 7, The .nest important variable -`or octroi o.f rrassfone depth and strength is befeoerabtre of ooi-olir:;^ Increase from QQb (32P) to 30*% {6CF5 resulted in iar'Vsr >.i* and increased strength, B, Heat dsvelopwenc of the tenant slurry after coupling is necessary to obtain maximum Xightfv*viwn. Prolonged boiling is also necessary in order to obtain a leveling out of masStone depth . and hue of tint. STAhDAdDIZATIOh of this cons should be by the varnish driers rubout srsthod f?n,X3^TMll 0*5' r 1*5 3 x 50 Hoover Muller 1:200 Z?iQ extension CALCULATED COKPOSITIOK - Azo Pi.nm'% Dyestuff * 100$, YIELD Theoretical Bk5 lbs, (1*3# moIs) Estimated ' $10 lbs, (9^ of theory) !?as is18 and anhydrous, SHOES KH-4.<?~3 (laboratory bvudy} - AAS:CC ,st? >/>/Vy A, A, 'SafemAEA CHEMICAL DIVISION DUP050067143