Document QXQVYpeb760z1QmgmBgqZw2Y4

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Serial No. KN-49-21 Copy No. i NEWARK PLANT PIGMENT COLOR RESEARCH REPORT TOLUIDINE BED, MEDIUM SHADE: RT-620-D LABORATORY AMD PLANT DEVELOPMENT AND STANDARDIZATION OP IMPROVED TQLUIDJME TONER Period Covered; October 25, 1948 - March 15, 1949 PILE; DATE; April 1, 1949 N42205 Hi9*n ---------- ------- CttIM nw.t :H Numerical File ' 2 * Reeearch Office (22U31) 2 * Libr&iy Hie (221*21) 4 - #10 MUgfe? IUi 2 * V* CholMPgki * tQml Filet 6 - D. B* KiUlm Serial Ko. i4$4 Cojy So* i itpjagy ftfflT prmmf cm/M HS8MRGH Pinal Report TitleI Toluidino Red, Medium Mbit RT*62(W) laboratory and Plant Development and StandardiaatloR of Sb^eoved Tolnddliie Period Covered* Oetdfaer 25, 1943 - K&reh 15* 1949 Charsoi Dinlamffli mwi Kvaluattonl U0EU31M4 (Pit. t 5 mmmm m* Kaieoi* 8* for Soar APPROVED ST A. am &wmmmt Kerch 15,1949 MTS ISSUES* April 1, 1949 DUP050067253 MSE&ii fa>ii4M>tii mri. mm develoDed In to atbenut to ooiiroxl&fttt cn improved competitive toluidtoe toner, Bamao** WWL (C-5U59). totoh to superior to toe old jrtandard Rf-386B in depth and intensity, lot 893x9 ha* bam set 09 as the official standard for B?~62CM>* It is lighter and mere Intense than ito39M>, bat on the dark side of 83V1. jgfgggg| dfbor a monthfs laboratory work* o ^c so mio s "nw tshcft Into the piwot on Roveober 23, 1948* which ferae toe basis Of too present formula* Eleven K39Q# tifttrhim vam a^ inriM &&*&&&* and tkmdwK* im tojg fatsaalA* A KOI *iae tii made iron 100# each of five plant batches as too now standard (lot 89319)* Since Jaauaiy 1. 1949* 17 more batches have been ran eatiofactorily 00 both the 1090# and 2180# batch else* Meanwhile work continued in too laboratory toward further improvement in too color* too variables, use of Sotax C end enesse sodium bicarbonate, look ` premising but tine did not penult their evaluation in plant development batehea* piSflP&pgp Against Rtol, Rt-386-O appears definitely dark and dull* Investigation if .all the old atmdarde for 87-386-D from 1934 to date Indicated toot tooro was* gradual trend toward end dullness* mwwMiiQ^in* to toe doveloxnmst ofam* ssnABi^^MAi Ae-^Ae** *W'"P* ^b ipbbba bbbB'B^aw a^b^b w ^* b ^ma b vMvM^M**iV '^b *a tow econcuy fonwla (RLH #48*38)* SeNevsr, none compare in both depth end intensity with IET-1# A laboratory fiafflcroa mo instituted to tanks the necessary dM*ii in too process to give tow desired depth and intensity* Proa four eerios of expertosnii on a 0*2 awl male was darlved a formula tolch gave a product equal to 8T*i to masatone. this formula m scaled up to a 3.6 pound-md plant batch which was first made on Rot^berS23>1948* tbs -result was darker than too laboratory product and anA S&lo kit AiwQditti!]3r ftfami l intii^ilra It vax MiitlkP to MMtoLa iit' 14 diiaMMMi a*j istauiur. but 108 weak and bine In of tow total of ton b*t#weoeHwa^aewAwKe^eA bamba enBB**weeBBB*AW|, 00 bba**b wepp ^^a c *a ^b a v s ^^a .*a w a we***F^ v b ^b b %b v b b o b a o v b a a a a a *ae^M^,eBeeaeeie undo prior to January, l%9, fivo nor# alaller to too first one* too ethor four suffered from effects of operating difficulties or variable studies. too process used in these batches, coded $$} RT-386-D at first* town (A)8!I*62EM>, differs from tow previous Rf*386*D standard formula in the following vpep.gowus ewea 1* toe HhPf to elurried directly into the aj^imtoately 3*48 hydrochloric add. ' instead of to sater* 2* toe sodium nitrite excess to increased from 1*4/2 to 3& % tooB8 to reduced from 529#, a 48 excess, to 522#, a 2$ excess. It to fe^reeipto i*w fjMn On caostle I wito aceticacid ! ***< of with eulfurto acid.m mmaB|^A*AA,e* BOA ew* *M" BWHArBIBW UPBAWBAPW 1 * *f ^MPBPb AWB^^B AA1 "A a b b ABA**BA "IP* ^AWWBSlA 4. toe 190# soda ash to replaced with 14# (1*8 aoM oodito^ asetatei toe 304# sooiiw DzcarDonato rwsaans unoiwngea* as a reeuxe oonsiueraoxe room xoww oursng flzwt *Atr of wmnHn.AAb W*Bf BBaAPAWF A*B* Br*rlB#IAABiA^B vi theAPB eaBrBlWie* rfowwlatoe dtouo ,** B acid to^^B*Aneutra^lAiaAWe*dBafcs*rB* the soda ash with the formation first of eodtom bicarbonate, end foam does not build up until tow end of toe coupling. With no soda ash prtsent, ths $8 drops rapidly and the bicerbewsto to decomposed ty -tow -acid to -fosst carbon DUP050067254  Mftfiyft produce the m feiea bnsks About hlf the has % The pi! drop quickly a* the dins* it added to the BH elurey, Th* pBE, with half the dlaeo added, it appcoxSaatoly 6.3. The final pa it around 5*3* $** final pg ef ET*3g&*D (8) it approMnately 7. 6* The coupling temperature has been reduced froa 111-113*? to f&mf&T* ' Oiharwiea no special tecb&l^s as m ysgp$y*s |a the conijpGl $ lh|| ttr&eena than lit th* ftteMLP #Gy*wla if* **t* radtiirad in taattk*fil2i* ftv*a4*ur^ grinding, or standardisation, The cost penalty at a result of these change l th jawwata ii approximately 2*6 cent# a pound. ftm hundred "< |M flee at these batches were oehimid tfa> a 'IQll Mat to fon the new standard. Since then twelve more 1090# batches have bees ran in the pleat, eight at which were satisfactory* The other four were affected in variable todies on the process* On rfg fOjmk batches variables were run to determine their effect on the color. The variables were &e follows* ip Use of para soap. Five pounds para soap added prior to coupling had only a elicit darkening effect on the color. Ten pounds gave darts esasstaa with no logins* in intensity tut a alight decrease in strength. 2. Eeplaoemant of 300# sodium bicarbonate with 190# soda ash and 30# sodium blear* tomato. The use of soda ash la both plant sad laboratory gave a lighter bit duller product, 8 - 10 stronger mid yellower is tint. 3. lower coupling temperature, The pretent coupling iUnperafnre, 96 * 98*F* is a low ae ean be <ariW used, and cannot be lowered further. A' 3* decrease in cot^ling teiapemture gave a lightir but duller product with no change In strength. 4, Use of lower coupling temperature and para cap. The intent use to eaepeneats fey the light, dull product at a coupling teoperaturo of 90 92* with tbs dai'kening, brightening affect of 10# para soap. The result was dash ami 3$ strong mad yellow. 5, Use of soda ash and a higher coupling temperature. Tbs Intent wee tocanjwnsats for the light dull product produced by 190# soda ash with the mxkmdxm*" . ' intensifying effect of a 101-1Q3* coupling tanpersture# 2h this milt higher ftfluWliwn tieoAfatKii* td h i* * ttttsttfc Sffrfllfflfa ay** til* t*dtoflt Mi *M11l light, dull, l$ strong end yellow. Meanwhile, other variable were being investigated in the laboratoiy. It was found that an increase in aaonnt of sodiua acetate would decrease death md 'inareass intensity, but a 109C#'batch would roquiro 147# acre eodiun aoHaN for any appreciable effect cm the color. An increase in the asuumt of hydrochloric add used to ninny the IHFT is the beginning iron 2,2 ool to 2.5 ad per nd of JHW had a sli#it dulling effact on the color. DUP050067255 Tw the nVsnt ftgatftti la r*aAm w casabininct the oMiMr crooextlons of caustic soda and acetic add in ah iron vat, An attempt was sad* to el Ininato thia.atep by adding excess caustic whan dissolving up th* BN and repreoipitating the BK with excess acid) bat thle produced a duller product. Replacement of sodium bicarbonate aith vaiying amounts of eode aft from 4j^ to on fltjTiwWolOir g&Vtt ifooulto ff4tq4 fWy- ^0 ihoo# in tiio ^^W^StiiOWP JJ3P6(JS0C^^tdi In feet, any experiment in which aoda aft wa* awed in any. proportion gave a dull product. Decrease in the concentration of the BK slurry had little effect. * AImiu Hmt seriig van wm tAIKdn. different deterCflUtS *t agents, in 2# and $S amounts baaed on pigMat, ahich were added to the BN Blurry before or to the ntsment slurry after ftwwwaiwg^ % following twatiag agents acre tried* Kaiser 3CW, Nopcowet A* N, C| SotexJg, P, C, NC,CN| urea, para soap, Alkanol B, Hone of theao gave any ii^rovapt., Sn lightness and Intensity In pre-coupling treatment. Only Sotex C .was beneficial in poet-coupling treatment, but has yet to be tried on a plant scale. it would increase the coat . i, ;-:wa>wtt1tf *rwtri riFFaKlig. . 'P. , < ' " An increase in the amount of sodium bicarbonate need from one to 1.5 mole had a beneficial effect on the odor. In fact, laboratory e^rlmimte smeaed to indicate that the preparation and addition of sodium aeetate could be eliminated . in experiments involving exceee sodium biewbonate, It night bvenhapossibls to '''-go tgdftft c modified RT-386-D formula, in Which soda ash was eliminated in favor of a--ro increase in sodium bicarbonate, and with a.lower coupling teajmrathre. ThblSlfttag# of this would be that the present RT-62M) could be matched at a . nuch less coat penalty than at present. Thee experiments have never been tried on a plant scale, but should be investigated. The result of all this pleat and laboratory investigation was a formula on which the pleat could standardise, RT-620-D (C), which replaced (A) RT-dSSO. and . differed fromit in the following respects* i) Bh has beat Increased 5$ from 522# to 127# to insure soslmst any oefttbllo dlaso excess. A i$ excess, $29#, is used in the BT-3S6-D (b ) proceea. Laboratory work ftoWSd that reduction in the BN to 522$t a excess, gave ' eomMhet batter Intedaitr. but this satruln was too close for aaaitttitsn. attd nottlt^M ^ e*ee iwnpev w p* ri^tilfiiifl ttoift Mifiii Tnfhrtfttit to $271 lOjlttlnAtiul tlai ''BBBBrwe wfvpweev ef^va'SF ^rewwm^wwiBe^F^r^rWF w p o pu b- difficulty with excess dlaso. " : '' * 2) The aise of ^e orifice has barn set <i#ft|Wi4ytf tisio ^ronndd fta hfttifr to foor lifibi 1& <wto to this ten nf #Aft]a imrf dHht<aia thi flK8tl&t teiiteteii#: 'Pi^BF *B^B PBBf ^^^PP Bw B ^^F ^FJF^F PB*P ^F W jBBB iflH4nnl ift r*4d^le^A -B F^)F ^PBpPndBPPPgB^F^^SB the fnAg. vbe three eten Gcniolinv nrocedure. eauolla, renldlv for 'tFi--wtep . , i.Mi fog. waa heavy, stirrins over 20 **"** imt<i the' foan broke. then alow coupling until the^ end, wae carried over from the Rf-38643 (B) proeeM into the (A) RT-620-D process. This proved unaatisfaefcory in tim nee fawwtttlfl. ittiit Mt bMa ft&Lftfiid tor a hittiv eauolint A , ilfiiyi nfli.a.PFeeaimaBpBm^etF p^^pOVpf B^^Fvmpe ^a ^e^PBe^^Fme w o m i w ipb^^p ^eppeem^ v^^^rB^MpBBP.p.B<BjHe sePB^^FP^paB^.'^^Fm) ^BaB.ShUFaa saaj^a^ctF* 4pBaFPF require constant aupervisicn by an operator. DUP050067256 3) Sodiua bicarbonate m* inoraaaad ttm 300# to 33G# in *dar to raiao tha final pH attar coupling 1S*o final pH oith tha (A) RT*62(W) proocea tint approximately 53 Tha BT*62Q*B (D) fonsOn it an altaniato to HT-620-Q (C) and la baaod on an increase In batch aiae from 109(3# to 2180#. fho and (0) forssula ware accepted by tho plant on Surah 9, 1%$. Bofcaboak 1217# Bapta. 25-52 Sottootfc 133t# Sxpta. 2# 3 KH-49-14, ' ` " DUP050067257