Document MJBdeYrYRO9ReD7XjrY3ewBOy

E. I. DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Copy No. /* NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Bsport K$-425-D Cost Reduction Study s s. Period Covered: February 1944 - ^uly 1945 J and Plant J- { <: < FILE 222.11 DATE: 21-30-45 NJ3SB9 Xi*l&J, / / v Merisi Bo. KB-45V77 Copy So. / onvj s.^**VaSJvS* Copy tos - America! File = lesesrch Office 1222.11) - Uiteary File (222.ll) - -riO Building File -i6 * y - iraperial Gaeraical Industries, Ltd. _, n8 ,,8 8 ~ l>. It. Dawson, Kwarfe- / a - / o - Vi ffll FLAET PIOUS T COLOR EESriECH BEPOGRT Final Report v-t;-? Ef-425-0 COST HEDOCTIOS BTUKf - iS&Sl-i MXJ k j :/ -: ol Covered* Fefcruery l?i4 - tfui- 17/5. v . 31 i CTisXups&I ^ ^ /* '.t V, ChaLupsLl V 75.5 DUP050150793 % 2- A laboratory process, - K-2042, teas developed 1b order to . the cost of the standard calcium lithol red RT-425HD. This process xeqt.f i-as- dry shading of the struck product with 0ol red dark in order to obtain the blue tint of RT-423-D. The bac?: f*;~ produces '& strong- lithol, which is diluted and Cheapened by aiUSitln" of rshinate; This process was studied in the semi-works end then tele;.! to the p^ant; after an experimental program was completed there;, a plant standard area set up. The -new. formula is K-2059, - which :.s of K~ 205$ (the actual struck pigment) shaded with ;1T~43'2~D'. ; *&,SSSM All of the semi-works study was done on the same basic laher ; . formula, X-204.2* . In this process, the diaso is made by dissolving * tobias acid in hydrated lime, to which is added sodium nitrite &.:i hydrochloric acid\ lime sad beta-napbtool are slurried together \;x: then s.oidified with acetic and hydrochloric acid* The diaso.ent bc*t- * naphthol suspension are mixed and. the Material coupled by adding; ckv < -. soda* Sodium rcsinate solution is then added and the material cove:?by heating. A series of 26 semi-works batches was sado over a peri;-. I about 5 months'in which numerous chemical and operating details of. tv. process: were investigated* Early results Indicated that mater it 1 simile.;:- to the laboratory product could be ma&ej such pigaeat ij S $;. and. yellow compared with the RT-525-P standard and requires shaclr &* with dork calcium wOuolw (ET-432-Dj to produce a replacement for ;'5>. Apparently the most Important point is obtaining satlaff cles.; quailtv using the new process is the proper control of pa thruxut t,; process| much of the semi-works investigation was c j q coined wi U- -A: particularly 1die amount and quality of lime used wi th the tool is. . c and bata-aaphtbol, the amount of caustic soda used in the coup li ; -> . the pS after coupling and-before development;, Both agricultur >1 ,x: chemical grades of lime were tried| satisfactory results were >tc-.-i; with both when the correct quantities were used; but there app... . be soft;; r-.>n-uni.foraity la both grades,, so that unexpected vari .!.t *;. occur from time to time. The mechanical conditions'*in rec.ctir . 1. :, lime vith tobiat- acid and beta-naphtfaol also appear to be impc .i - 1. la the ce.:-' of the beta-naphthcl some difficulty ua-.> vcouatex ..{ - .. the be in-naphthc-1 collecting &s a solid unr.r-c.ctcc] 1 op under agitel; r. Optimum pH after coupling ras deterrdnod. lti lav c-ox - -- - i cation of the formula dose: Ibsl zbo.-?n .In hLSx var.In/ te solution is added to the T a'oh.t- "1 Mon t:.v di&EC, was'given two ixxrd -v j?y, trials. i.r the' ;,j -; H -s.v;s :t .;ight that this prcced'jre sJ /h*- .' -- 'r: 'v"'"' f - ' -- 'I-yt '* 'q - seni-v..-..`kx results ware undesirable b..CiV^ oi ivr.I . x-: -i-ciio, 1 : as col variables tried in the ..-2r.*-`~- : rl:e vox r r - 5 of n v sold -;icrccEoc strength rave h'rk a-or ; > .:t -. : r-;::: rtrspr:fcttrri eg the tobies acid wi th s ; r..fici-23s rl like, x! later - o.E the r^st of the Xim -i?s.v X; '':io -x. . oj. es: : of !hr- to give lower ink showed no 3' :ct m ; : DUP050150794 Representative seal-works batches of satisfactory quality were 2vs.lu.i-.tefi in ink; compared with the ia* standard they had. so*erht. logger mixing time* slightly heavier body but with more ink lezmth. -Atisfactory liveriog and litho resistance properties, sand exccl'e;- t-r,;ture. These batches were also tested .for Dulux hle^d and *ev->d sue* tory-.r's,' /. m '. # In the first plant batch, a development temperature higher than that used in the semi-works was employed in order to get & liyV. masst-one. This hatch was light and weak, flu not only to the hixV development temperature bit also t the fact that the beta~naph.li,xi was stirred with the lime for an excessively long time; in the s- 20..:; plant hatch this long time of stirring was reduced and the develop!; . t temperature - was lower, resulting in a product similar to the aeuri-r: v material in quality except for slight dullness of masstone. A tempo" \ working standard, lot 7219, was prepared from a Check hatch (92 part lot 15969, $ parts dark "Duol RT-432-D). During the next few month; attempts were made to correct dullness of masstone hy various mevmt ? including Increasing the amount of rosin used, increasing the amour.. :v of lime in the tohl&s acid, the use of chemical grade lime (with ad justment' in the amount to correct for higher available alkali) .&ix! mi:;* talning the alkalinity during development hy adding caustic sc da as needed. Very slight improvements were obtained at optimum alkalinity, as discussed in the semi-works section above. TJse. of a deficiency o,f' lime with the tobias acid, followed by a later addition to make up if. 3 deficiency, as discussed in the semi-works section, resulted in weak material in the plant. Reduction in coupling volume also gave weak ness. A mix of 11 normally prepared plant batches shaded with 0 of RT-432-D was, therefore, made up and recommended as a new standard. Compared with the old type of RT-425-D, this mix (lot 43807) was dart, 8% strong and blue in tint. This mix was made up in September 1944was used as a working standard until it was finally set up officially in July 1945. 4 new standard formula for the main component of P.T-42"-! was written; this is -2058, which Is standardized to RT-425-D by mixing with HT-432-D. This mix is designated -2059. The new process for RT-425-D represents a twelve percent reduction of ingredients cost; the differential is less in out-ox-pc; and total cost. The following data, from the second quarter reyXxcumeat costs are not completely comparable because of revisions ar.C-x the methods of costings- Y'f " lew process -2059 Old Process -1550 lRg*31X3M 32.75 37.01 50.83 52.53 IX, 73.. 75. A. more detailed discussion 'of the variables which effect quality it ry be found is the operating notes- for -2158, a copy c.C 'which la Included under Bxpcrimeni&l 3 of thireport. hee Development Section Data ?-odks D3-A5-2\. Shu t 4-''-25: for plant work. !?' i - A- DUP050150795 ..c p RT-425-P Component ,K-2058 is representative of th nm low ingreldsnt cost Calcium Miiiol toner designed to replace E-1559. As tbs aw product is lighter yJ.)oir:r than the original RT~425-& it is neoessary to two RT~432-3 it i t'fci.i mstarial to approximate the RT~425-& standard tinetordally. The principal reasons for the approximate $6,19 ingredient c>&% savings per 10# color obtained with. the new formula are iha following cr 'nri fie*! K-1559* 1. The substitution of hydrated lime for -the calcium chi >rde and mos% c.f t:; caustic soda. 2. Omission of the "Ltthoeol0 Mono Acid W, 3* The use of 8Qj? of rosin per mol in the strike to give increased yi'>3/e 4* The filial dry mixing is of about 8j of the oomparatlv aly low ingredient cost pigment* RT-432-B. S Some experience Ms been had ia the plant with tbo following cersrrr-'. variables* lat.^rtyl lata Quality* - he is the 'case with most lithols the quality o.< :>'r. "LithoBol1' held TIC (Tobias Aoid) has a definite effect on .tinctorial paop-ju-. tie. lasstone is most affected by slight variation*! is ingredient pui it,*. Awwnt af. Hydrated..Maw - ar as ia bes'ti plant results are obtained by controlling the pH of'the Tobias Ac; d partial solution within the specified pH range of i05-ll=5 The pres .rr?' standard amount of chemical grade hydrated lime (44 pounds per moll eheuld g." the decided result. If agricultural grade lime is used the initial am; urt should be inoreased to 46 pounds per mol, Xn cases where too xsneh lime has been added (re -ulting in pi-5 t in the srder of 12.0 for the Tobias Acid solution} a definite tendency tew; rd the production of dark, week material has been noted. Wh*n pH tests are u>norrsJJL.f high it say be possible to adjust pH before di&zotieation with */,v 1; eoit- in .-wder to eeeurs a satisfactory product, Thor ha:< been as eaeptfiar- xn ia -.la plant with this, however. A low initial pH on the Tobias Aoid solution (i < the range ' '-V 3 ^.Lt ;3 r.?.re couplet solution but a lighter* weaker pigment is usually Mv.z: . Ons or t-ro pounds of Xim should be added to. adjust pH in & case of th. a ; la Beta tfanhthol Slurry* There should be so difficulty in c V... pH -f th* Bata Haphthol slurry within the doslrrd range (11,0-11.5} uslaj.: ''4 pourds pr mol of chaadoal grad hydrated lime or 55 pounds? of the agrf gra-:-&. DUP050150796 N41597.01 Ai,vi.H fag^SouoMjMtt * Tb standard amount of 60 pr.;c? per mol is hr rr-. to h .log to the optisms, lowering the amount in t! f *Bl~5?rka to >y .. p{'--r...a per ffloX gave low coupling; pH teat and slight i**o oxcg'sa. " :5,; tin- yugh tiie dvelhpmt under ibeee condition g&va l.igfert, dv.ll' rar.-jr 8jai;; -.ss 'X tint e Increasing the coupling allcsli mount give* hirt coupling pE % ' ; -%k:-m ,-eqiiiree additional acetic aeld to carry through tivo pH ad^uetaes/rt so; filing* If the adjustment is net s&d high devolop?5s.nt pSi 'conditior* ' to giv--- <iark, hull, weak products. - n IflAfe-2"h pressat standevd addition rati- M the sovpiJ.ig alkali of 4~6 minutes is believed to be doe* to. the is?*. Thera i e no plant esperiftttce with variation iu iity of edition. OsmUjngS" 4S-S pH after coupling* pH testa oa the souplisg aftor the 15 si stirrix-g 'period usually range between 10,0 am 11*0 and are adjusted, nefeaeftary, .to a pB of 9*8-10*2 before tha addition of the nodiwa roeic-.,.,-, h'hea pH tests are bel.ow 9*0 & dieso sxosas nmy show up which ufeoui-rt di wfcteh. tie- proper pH adjustment is made. Ma.er and .Beta; Jjachthol.Bxoe.ee .After, .floaolirtgi The norm! e -nit* a testa for iShi# coupling are a strong excess of Beta Sfepfct.-.oi ad a tee-'; for. free diaao* Occasionally, however, a slight tea- fer excess i-i;tog-ether with a faint test for Beta Haphthol are obtained uve* though t.fc. - i test i* normal.. Mo definite laatioa can ha sad for this pheewtPH thrugh it lift' believed that the conditions under nMob the Beta laphtiw'" Is; precipitated are reeponafbXe* la any caee, as a very dull bis safere is ; vif the pigment is heat developed in the presence of'free iiaso, it is ' : ' ? to .rtaBCva the excess diaxo by eoup'tisg with Beta Kapbihsl., This is be-it accomplished by adding 2 or 3 pounds of Beta Faphtfcol rliiiolvsra in arj .*, with about 3/4 pound of caustic sods, normally, this fir.yU addition es' i-s?t* ffephihcl should raw# the diare excess hut in eosie cases ae much a I'i vt-an'l; of Betii Naptothol are needed to give the desired effect* batches of tbJ.e i*-..t ; ? tyr-; ars usually of poor quality but when only mall arsovete of the Ir1-ic '- -- or*? needed the batch usually is close to ttoi normal quail'.y. Yeaaarature of Pevelonaenti The standard dovei-iptrettf tesspar-\i.. ? {1*. itJf) gives opticim depth end strength, Inorecsing the development tyr;- it. VI$*F. gives lifter, eiSnewhat voskef product3. r%ii ft-r T^eveiogBsenti The norm! pH drop during i: dgvolopiaer: i ' ' i ' ite orf-ler of 0.4-0,8 unite. Scms of ti batches, V.^ever, as mc-h %r ?/ ux;its ' ` reReon unknown) with the result that a lighter, j \ivcer tsasefeOK. s '- -. 15;,-;-! e$'<r product is ewcured* This can bo controlled, to w.w extort, ty 0 : -1- DUP050150797 -3*- p5 at intervales duping the boating cycle bx A adjusting tho pH if necessary with 2 ar 3 pouadB of caustic eodft. This Should fee done' feeforo the tipar*~ tur reaches 130F id order to obtain the desired effect. A very small amount of experience with this tre&tsmjnt indicates that the tendsnoy tc-r.."-< lass of strength is eliminated but m improvement in mestone is obtained,, Manufacture on the X-2058 are\C a has been controlled s both the light and dark side of the original RT-425-D standard, lot 25956. Howsver, all masufaoture with the new formula ha* fee;* deflnAt'sly yellower than the desired shade which makes it necessary to dry mix light masstone material made ca the K-2058 formula with approximately Z% RT-432~J) to give the required zoasetone .and tint. Attempts to use an accessory agent with the new forcjola in tie manner of the original RI-42JHD (Mono Acid W used) .ware unsuoceogful, Xx; most cases dark, yallow products were securedj where blue tints were ov.t^-f m& the products were wary dull in sweeten and weak in tint. At the present time the only possibility for setting up an "OK Straight* formula is to slurry mix with the proper amount of RT-432-D cither in slurry or re slurried press cake for. Vide- procedure chcrnld be tested then more experience with the K-205S formula has been obtained and bettor established. XaM* field:? hava varied over a fairly wide rssgo (17^-) but the average (4f? po-iads par mol) is very aloes to the original estimato of 490 pmr.ia par moi, A goal yield has been calculated and amountb to 498 pounds per arl. S. J. HSSS 9-26-44 A... . DUP050150798