Document MMKNEmgDXEYrmwZYezK0jZGry

E. I. DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT 256 YANDERPOOL STREET NEWARK, NEW JERSEY Copy No. / Ah i copy <9- / A r/V / ~ Period Covered: NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Red Dark RT~432**D laboratory & Fleet Development &f Cheaper Process. Sovember 1943 - March 1945 FILE: DATE, 222 HI H-29-45 NJ8SP9 a". / / / Serial Bo. KM-45-91 Copy Mo. / Copy tot #1 - Burner!cal File , 2 - Research Office (222.111) 3 - Library File (222.111) 4 - #10 Building File 5 - Imperial Chemical Industries, Ltd. 6- " n 7_ ft h 8-0. H. Lawson, Mewark MBffARK PLANI PICBIEBT COLOR RESEARCH REPORT Final Report Titles flJDuol8 Bed Dark RT-432-D Laboratory & Plant Development of Cheaper Process, Period Covered: Movember 1943 - March 1945 SOEMITTED BYs . Chalupski APPROVED BY: ^y&r.. . Chalupski DATE SUBMITTED: 11-20-45 DATE ISSUED: 11-29-45 DU P050150751 2* ffllffffflffgfll A short study was carried out in the Development Laboratory to modify the RT-432-0 formula in order to reduce costs. A few simple modifications were found which gave acceptable pigment? these changes were gives plant trial, and a new standard was set up. The new standard, darker, stronger and bluer than the old, was a good match for a number of outstanding competitive products. In the laboratory it was found that savings of about 8/10 of a cent per pound could be achieved by reduction of excesses of materials used in the Coupling. The old RT-432-D formula used higher amounts of caustic soda, sodium nitrite, hydrochloric acid and beta naphthol than did the other Cuol^ red formulas? it was foundthat a reduction In the amount of hydrochloric acid used in the diaao and an equivalent reduction in the sodium hydroxide is the beta naphthol, resulted in somewhat bluer tint. Reduction in the amount of sodium nitrite and beta naphthol had no appreciable effect. Attempts were also mad to reduce the temperature of development end strike, but this had a detrimental effect resulting in lightness of aasstone, weakness end blueness of tint. Plant batches were made using the acceptable changes indicated above. These modifications are tabulated below:- HaOH for Tobias Acid RaROo in diaso HC1 BaOH for beta naohthol amt. beta naphthol to.ggaai*. 31.5 lbs. 52.5 w 68.5 52.5 110.5 M aM.toiLt.aa, 34 lbs. 58 H 96 It 84 112 If (for 0.75 mol batch) After five plant batches were made this way, a mix of two of these batches was made and proposed as a new standard (lot 7247). This mix was slightly darker in masstone, bluer in undertone and tint, and approximately 556 stronger than the then current standard? properties were satisfactory. For a short period after this standard was set up, a few ok straight* batches were made in the plant. However, when later shipments of Tobias Acid were used, dark and blue products were pro duced. It was found that this material was readily shadeable to the new standard, using the light calcium "Duolw RT-431-0 for blending purposes. On this basis, supervision of the new process was turned over to the plant in March 1915. The new standard formula, K-2113, represents an ingredient savings of 92//100 lb. of pigment. EiprnMmm,.r e t a il s Laboratory work see Research B.B. 1063, exp. 15, 16, 19, 20 Plant development work see Development Section Data Book DSB-45-35. DUP050150752 K-2113 is representative of the new lower ingredient cor-t Berk Cr.lv.iwa ' 'Bwc3.!* toner designed to replace K~l63& A email cavings of appKocimately *5 ce?" jsr li ; pounds of product results fro alight cuts in igrd3 sni weeflsis,. Th variations from K-I636 used in.K-2113 follows ' .11 caustic soda used for dissolving the Tobias Acid is cat from 34 tt -;:, cr v (f iuivalent to about 4^/mol). ? i'li-- sodiVM nitrite for diasotieetlon is lowered from 58 to 53 pounds (erivr.H < to about fO^/mol) Shis, corresponds to decreasing the nitrite excess fs-cm lit to approximately 2$. 3* Th muriatic acid, in tbs diazo is cut from 96 to 68 prund-a (equivalent to a-.-vi 9#/mol).- This, cuts the acid excess in the diaxo from 1 l/2 so?. to l/l. mo? < 4. By reason of the decreased acid In the diaxo fie esustlc 00da in the D.is ssazt be lowered from 84 to 52 pounds (equivalent to about 7Q$/bo !*) ,'<x% 5 The Beta naphtha! is cut from 120 pounds to 3.?.?. pounds (equiYcXoat to .nlrut mol) This corresponds to decreasing the second coesponent exfoas 'fron 11% v; -' 1/2-. * Tbi; -pigment slurry volume before the strike is cut from 537& gallons to 320 % Vlor s, i, Tlx use of the "Noiseless* heater type etesa-line.for boiling during t.Je strl^ ; period'Ik specified in the as* formula* The combined effect of the Ingredient weight variations x>eed in K-2113 is a giw slightly lighter, very slightly weaker, and slightly ,)Xuer products. A ru'ocut comparison of the new RT-432-D standard,' lot 7247 (rspreseat-vsi v-> of mas&rial made on the K~2H3 formula) and the previous standard, lot 229-1-7 folio-t i f247 vs* 229478 dull bl, e. dirty - setr- bl. Tide sr.--.ddy maeetone, blue tint result is representative of tha type a&teri .! boias obtaiii-cd recently with the previous standard formula, K~l$36, There has been little, if any, experience with the use el variables in t-x< r-ew foi aula because of the limited production to date* The diecuosion of ra-inbl:r.ppendri is based on experience with X~163&. It may be .mentioned that the rsult 1 discus: td here are based on oversell trends rather than on definite result.* isvou? i i the 5r.re.tic nature of plant performance. Many of the 'difficulties have bven ` orreot r-d, however, end it is to be ejected that RT-432-B production'will a 101/ bo octroi than heretofore* :* Xntrrmeiiate Qualitya As is tho cane vith meat '*DuoIs" the qvsili'j 0.' < litio.-.-l' ex id TK (Tobias Acid) has a nctab?.o effect on tin ori; L prepgri .3* T.Tceri-*. ->.ee fea indicated that both mass-tor, and tint ere affo3ted by chon.j s i.. 1 cbi?e '-.cid quality* Jfa of nAihi-.r^J'- Asia TQEEft The substitution of 5~" 0% c? TOM f r TU tie 'lTicTgives dark, muddy nmostone, weak, dirty tint prc&uctr. ___ A DUP050150753 N41587.01  'Sefrft Haohthol Excseei 1'he present standard 2-1/^C enossc is the iiinit us. that 3.*-. is ssfe to use* It is believed that the lowering of the Beta Hapten .1 f.'.:'0',a tiw original 11$ to the present figure has resulted in a very ellghtlj '-'v;cr product;,, :;? Ooualing Aikalinitvs In general, increasing the alkalinity of eorp'JLrg result' in iar.--aBed -depth of maestone end strength end yellowness of tint, O'owversf iv, I : : r-e; , . v,ak' ,-nd. bluer products are obtained with decreased coupling alkalinity. I.oue-.v.j r ihi. caustic soda excess corresponding to the present alkali amount (5S pounds per 2./'' s-'t .-hatch) is believed to be clegs to' the optima* for depth and yellowness! Ksporisrc*with tho alkali variable on the K~X636 type formula indicates that caustic sc da nx juts? oorresp ending to'a rang of 41 to 60 pounds on the present foramla, my be ur sd. X.v3r horn been soma indication .that alkali amounts at the extremes of this range tend 1-r give cuddy maostoaee and dirty tints* It should be understood, of cures, that the coupling alkali variable sort as preposrly combined with other variables i order to be effective. Amount and Type of Roeini The present standard amount of S rosir. (IijC$) ii- bsXSeved to be close to the optimum for death of msstono end strength sud ysllo meat of tint. Some advantage ia strength at tbs expense of Kaastocs depth Bay ba obtaia nby lowering the rosin amount to l0 pounds. This variable should -rat be carried t? ; extrerasS .because of the danger -of securing an "unturned?* light, dull, m*k or ?d tet, Substitution of X Wood roela for the B Wood grade resulta in light 'me very yellow tints. - U Gun rosin has been substituted for B Wood rosin in both -Sejai^Wgr'is a id plant production and has given variable results versus standard. .The usual eff t appears to fee lighter dad brighter masstonea and bluer and cleaner tints* Use of t;Du-ponor* 3 She addition of "DupoaoX** results ia darker aaeatasoe a: a strongs? and bluer tints. She standard' amount (12)4 per 3/4 mol batch) is believe! ; be close to the optimum for depth and strength. ' She results obtained vith' "Buponol" is believed to be due to its 1 is renal.v, ih nBuclisting" effect of tfea rosin used. The standard formula calls for aidit:.03s - f ~.he "Duponol" immediately after the rosiest* solution is added prior to the dsvsl'yi wont of ths Liihol soda salt. If the "BupoBol*' is added after the development of -sh* soda <3e.lt just before the strike a lighter maestone product rerultss. Ammonium. Chlorides The presence of the ammonium chloride ia neces/ary fu.~ curiny depth and strength. Omission of the ammonium chloride results ia c. '.i,~5v .. lvuet wick product. A considerable increase (100/Q, however, t..ay also give a fcr.MS, 7/ '..k, lev brotue product and for this reason aasaoniisa chloride vari&t: s:is .' > colder., if ever, used In the plant. Sffsct of Strike Volume* Variation in strike volume 1*: one of the j linci; .; ?'lions of standard formula.used in the plant for controlling nssetons-. vs.3 Tie pren-nt standard volume (4320 gallons) is the minimum that may be used and is cptiaras. .'or depth of masstons and yellowness of tint. An appreciable decrees in t:-.y result in an "untuned* light, weak, yellow product. Increasing 'V.o c: i clone r .i 5376 gallons gives a lighter, bluer product. DUP050150754 I ***** to facilitate maaufactur a ten minute strike time has been selected aa stanc-nd. it the im time, however, it is necessary to eiiadaate to as great a degree a? post 5vis the fe:'nsvtio i of high local precipitant exoeecee during-the striking peric J vKs. would ;.tv undesirable light? weak* blue products. This is accomplished b.rt 1, Striking through & spray tube. . Good agitation* 3 1 noreasing surface agitation by brisk boiling using a "!?oiael3s,-jtt ctev.; sparger which accomplishes the desired effect,at the cost of acne v.i - of steam. In order to keep steam waste to a minimum regular belling. using the ordinary steam sparger is used during the twenty radswie dev ilop* mtot period subsequent to the strike. I'hfi boiling strife and developnent is necessary to obtain a ccapletsly "Buolired" product. The-use of modifications of the striking end developing procedure as u mba* of varying masetone and tint is not recommended because of poor control. RwoimNDED vmiAB'm cQmimMQE&.im^mMSK.Gomsi^ For OK Straiadht t The Standard K-2113 formula should give passable j.srftvr :.ao*. For garb. mellow nroductst The aoet consistent results should be ebtrir.'K by uaing the previous standard) K>1&36, formula togother with the 4320 gallon voitr.s before -strike and special cars during the strike .(uae of the "Noiseless* rfcarm 8p*.3T.?sr) - For dark, blue nroductai The standard K-2113 formula gives a fair preport.inn of dark? blue batches. If production is tending to run dark in oasstone but yells,* in tint increasing the volume before strike to 500G=-540 gallons with hot water imy the desired effect. For light, yellow..produfltnt Usable material of this typ is difficult %; obtain. Variables that have been used on occasion? l.e. substitution of K Wood fer B TSood rosin or elimination of the small rosinate addition before the devel op-oent s' the Lithoi sodium salt tends to give weak "unturned* products. In spit oi the tjh. cost involved it is usually recommended that when light, yellou shading material :U needed the Medium Calcium "Duol" toner , RT-431-D, bs used. For light - blue products* The following variable combination ie rcooat-s.v.'iU 1* Decrease the second roodnate addition to l60,-: B ^'ood rosin * 32< ; -cusi Seda. 2. Increase the volume before the strike to 537$ gallons with .He* ..s\ 3. Do not use th "Noiseless" steam sparger during the strife;*. Ilai.r -v la a fairly brisk boiling temperature with regular steam eparg-r. DUP050150755 4- % Brviae T&3&>eratuget Although the standard drying tt-ajar-itura ha;- ' -SbU ,jt &< 48. hours at 140*? a small asaouat of pleat .experience has indicate;'. 'ast : fioge drying cycle (15 hour a at 200*F* * 5 hear* at 140".?.) or von 10i hcor. drying at 200F ay be used without undue elfoot on quality. Xfctiil* fields to data have been fairly satisfactory and saactmt to figure will oh wem basad on the K-163& fornsule. t< tie w :t M8iSJ >s. j. hi*.ns 2l3~4 DUP050150756