Document 70NeyBXQqpD3G29OxZ9YY0nwB

E. J. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Copy No. 1 Numerical Pile NEWARK PLANT \ PIGMENT COLOR RESEARCH REPORT FINAL REPORT DEVELOPMENT OP A PRIMROSE YELLOW TO MATCH THE #90 YELLOW OF W. P. FULLER COMPANY Period Covered, FEBRUARY ,194$ - MAY, 1949. P`LE: 211.1 DATE, 9/29/49 Njearo N42219 Copy tos 1. Sumerical File 2. Research Office (211.1) 3. Library file <211.1) 4. V. Chalupskl Plant Pile 5. D. B. Killian, Hewark I. Extra 7. Extra Serial So. KN-49-38 Copy Ho. 1 HEWARK PLANT PIOHSST COLOR RESEARCH REPORT FINAL REPORT TITLE* DEVELOPMENT OP A PRIMROSE YELLOW TO MATCH THE #90 YELLOW OF W. P. FULLER COMPANY PERIOD COVERED: FEBRUARY 1949 - MAY - 1949 8/30/49 9/29/49 DUP050067416 mmmm* For some time the plant had been experiencing considerable difficulty in manufacturing light, intense, green masstons Y-488-D suitable for sale to the W.P.Fuller Company. She Chemical Division was ashed to develop a match for this customer's #90 Primrose Yellow standard; 1. A batch process was developed which, in the laboratoi gave products superior to the Fuller standard* Semi-Works attempts to manufacture this material yielded unsatisfactory results, the products being extremely dark, green and dull in raasstone. 2. Plant development of this product resulted in products which were considerably lighter and greener in masstone than thine made by the standard process for Y-488-D. Such products were difficult to handle in the press room due to thixotropy. Several variations of this process were run in attempts to correct this situation* 3* A mix of several plant batches coded Y-488-D - 90860, was made Up and submitted to the customer* this mix compared by ruhout as follows with the Fuller standard (C$51214 - T.F.247-6). fertuauBt Mai 8%Tm Tjnt 90860 vs dk*ared,intense OK Y-488-D,SD-48377 dk., v.red red * 90860 vs Y-488-D it.,intense 105*100 s.red The mix was ultimately rejected by the customer because of excessive redness of masstom, despite the intensity advantage* H^COMMSHDAYIOHgFOB MEL 1* Plant evaluation of the leads suggested in the letter J. J. -- VHC - 7/21/49 (see copy attached) may correct this situation* 2, A single source of vehicle ( Archer-Daniel-Midland Pale Orinders acid refined linseed oil) be kept for all laboratories* mm 1 nothing of a patentable nature was discovered in this work. .; . DUP050067417 -2- timM&KUmWU Simultaneously with a sick list study to improve the quality of Y-488-D (see KH-49-24), the Chemical Division was asked to produce "Super-s tandard" material (lighter and greener In mas stone) for possible sale to the W* P* Puller Company. A review of recent production was carried out, and several attempts were made to produce lighter - greener material, by decreasing the quantity of chromate used in Y-488-D manufacture and applying certain of the techniques used in the above mentioned study. These techniques had given Y-488-D lighter in mas stone than standard. Two batches were manufactured simultaneously) one batch in the plant green unit, and a second batch in the yellow unit. A definite superiority was shown by the material made in the green unit (probably due to better agitation). All products, although greener than Y-488-D, were excessively dark and dull compared to the Fuller standard (C#51214). Other variables, such as changes In the amount of soda ash utilised in white base, lead excess changes, variations in sodium chromate, strike temperature changes end variations in agitation, were studied in the laboratory without success* It was apparent, therefore, that a new process would have to be developed to produce pigment to match this competitive sample. Several years ago. the writer had studied the possibility of manufacturing Y-488-D continuously. During the course of these studies, a continuous process had been developed which gave pigments which were lighter and greener than Y-488-D. (See H.B. 1121). Laboratory studies were made on this process and compared with those prepared by the Y-488-D method. A marked advantage of the new process, as compared to the standard method, was quite evident. This process utilised sodium fluoride for masatone intensity, and was essentially a phosphatestabilized, heat developed rhombic phase yellow. The heat development step was quite unusual for a primrose yellow as light as Y-488-D. The process was modified to make it suitable for batch manufacture without difficulty. After several laboratory runs had been made, two attempts were made to manufacture similar material in the semi-works. These attempts were unsatisfactory, yielding dark, green, dull pigment without any apparent reason for failure. Because of the very limited experience with Y-488-D In the semi-works, it was decided to attempt the manufacture of this material in the plant (Y-488-D - 65554). The process behaved very satisfactorily in the plant. However, the press cakes were extremely thixotropic. DUP05Q067418 3 Laboratory investigation revealed that the thixotropy was a fanstion of the amount of tetra sodium pyrophosphate used in the process and a second batch was made* decreasing the quantity of this material (Y-488-D - 659943 by elimination f the final portion. Unfortunately, as the amount of pyrophosphate was decreased, a tendency toward greater masstone redness has observed in the plant* and a com promise in quantity of pyrophosphate had to be made. Several attempts were made to correct this situation by decreasing the amount of initial sodium carbonate used in white base preparation for greener masstones and by giving the press cate an aluminum sulfate wash after the regular press washing. By these means, products were obtained which ,were net overly thixotropic despite the large amount of pyrophosphate used (see Y-488-D, 66540). A mixture,coded 90860* of three plant lots (66lS5 66470. 66540) was submitted to the customer for evaluation and was rejected because of objectionable redness (see attached letters). A special testing method T.F.247-6 has been set up for testing pigments for the W.P. Fuller Company. Considerable variation in tinctorial effects were noted, when different laboratories rubbed out the same product using variously aged samples of the specified vehiele (Areher-Danlels-Midland Pale Grinders Acid Refined Linseed Oil). Investigation showed this variation was exclusively the result of differences in behavior of our pigments in different samples of this vehiele. Unfortunately, the competitive pigment wad not so sensitive to such change in the test vehicle. It is recommended that all such vehicle be kept in one can, and used by the various laboratories concerned when necessary, rather than being divided into individual supplies for each laboratory. fetters pertinent to the problem arc attached* summarizing the current status of the problem. ataw, A total mill cost penalty of $1.15/100# versus Y-488-D, was indicated primarily to'increased ingredient cost* and cost of heat development. A copy of a typical plant and laboratory formula is attached. REFERENCESi SsH-49-32 H.B. 1121 H.B. 1142 - . f. DUP050067419 'T 4 -- NEWARK, N.J. Jims 15, 1949. HR. J. W. CRONIH f WILMINGTON ML Shis letter will serve to summarize the status of this problem, which has been dropped frm the Inorganic Group program.. Products have been prepared at a cost penalty of $1.00/100 lbs*, which are very slightly red and intense versus the Fuller standard in masstone, as evaluated by standard Fuller testing procedure TF-247-6. They represent a definite improvement over Y-488-D in approaching the Fuller standard* All tints are very close to the 0# to strength and hue. After 3 days outdoor exposure to OB-2527 alkyd, our products are at least equal to the 0# (See exhibits 1-3-4 attached to Mr. Cronin's copy). After 7 days exposure {See exhibit 2) or after 24 hours to Weathor-8-Moter, our products are considerably redder than C#4. Y-488-D standard compares quite favorably with the C# by Weather-O-Meter evaluation (but is too dark and red by Fuller TF-247-6). These products, which have been prepared by slightly varying types of formulas are unstandardized at present but the Production Division has agreed that their manufacture should not present any serious difficulty* The following tables summarize our evaluations of these products} m as Y-488-D SD-< Mr v.si,red s.lt.,s.red, tot. ws.dk,, s.red, int. v.sl.lt., tot. dk*, .v.red/- m* s.strg. , i * ; : TIBT vs red vs red s .red vs red !t * L/Fastneas * '' v.si.better v.31. worse a * ws worse not available as yet due to slow drying characteristies Of Fuller rubout vehicle. m 66540 A. in.Jr.lQ.3 Op.igAMLMaMagJS depth, v red ws It. , vs red vs It.,vs red, vs tot. ws It. ,vs red,vs int. .f9fr9at.,f * after 3 Pays Outdoor ......... .... . s.lt.,s.rad, s.lnt. red, s.tot* s.lt.,s.red, a*tot. a.It.,s.red,s. tot. ,7'Iasa dk., red, tot? dk.,red v.dk. ,v.rad v.dk.,v.rad See eshibits 1 - 4,: 1* DUP050067420 5 Lots 66185, 66470, and 66540 totaling $200 lbs, were mixed under lot #90660, Rubouts of this product by Control Laboratory read as follows* JBL US* TINT Fuller TF 247-6 vs 0# vs dk*,rsd9lnt, OK red Lot vs Std, Y-488-D It., int. 105=* 100 s,red Ve hare also included (Cronin's copy only) two exhibits of some additional studies conducted during this investigation. It appears at this time, that retaking the around pigment is highly beneficial to stability and color retention as evaluated by outdoor exposure in alkyd* Two exhibits of this type material are shown. Exhibit #5 represents a rebaked portion of the grind of lot 65994 (different from previous types)* It is definitely superior to the competitive product in alkyd by outdoor exposure but is quite similar to our Y-488-D standard in tinctorial properties, as evaluated by the Fuller method (IF 247-6). Exhibit #6 shows the effect of rebaklmg the grind of lot 66185 (similar to components of mix} as evaluated in alkyd by Waather-0-JIeter and outdoor exposure* The effect of this rebaking procedure is new to us, sad we have not attempted any studies of this in the plant. We would appreciate your evaluation of the value of this llghtfastness improvement. Your comments as to the significance of tests in alkyd, in light of the use of acid-refined linseed oil in the customer's standard test, are also solicited. JDLIUS JACKSON ECAL DIVISION DUP050067421 -$* NEWARK, N.J. JULY 21, >949 MR. R. P. ENSLIK ROOM $22 111 SUTTER STREET SAW FRANCISCO 4, CALIF. W. P. FULLER 4 COMPANY Refer to Letter BPS to JWB * July 12, 1949. We regret that the customer has rejected our hew offering of Y-488-D - Lot 90860. In ay opinion, and also that of Mr* A.J. Hughes of the Newark Control Group, this lot represented a definite improvement in approaching the Fuller standard. It is much closer to their standard than Y-488-D SD-48377 or any recently submitted samples. We would not hare submitted this sample had we not believed this to be so. We were of the opinion that despite the redness of messtone, the greater masstone intensity and cleanliness would be of interest to the customer. Since the Chemical Division is no longer working on this problem, certain suggestions that may correct the masstone redness will be attached to Mr. Chalupskl's copy of this letter for possible plant trial. JULIUS JACKSON 3AL DIVISION DUP050067422 V. E. CHALUPSKI 7 HEWXRK, H.J. JULY 21, 1949. Since Mr. Enslin reports that the lot 90860 submitted was too red in masstone, X would like to make the following suggestions for possible plant trial by your group. Use Basic Process Y-488-D lot 66540* Apply following variables (1) To reduce redness of masstone (a) decrease initial H-3 added to H-41 and replace by equivalent amount at adjustment of pH Just before heat development* +25 lbs# ? (b) decrease M-8. Raise N-108 +10 - 15 lbs. (will probably sacrifice some masstone intensity). (2) To reduce thixotropy of presscake use 25 lbs. N-15/1000 gals, water for press washing. If Some thixotropy remains increase H-15 in 10 lb. steps. (3) Dry 12 hrs. at 140F. Bake 12 Hrs. at 220F. JULIUS JACKiSOS CHEMICAL DIUISIOH DUP050067423 LABORATORY 1 Mm. X-48B.P Lead nitrate 165.5 gr. in 3600 ml at 70? pi 5.0 Add in 3 minutes Sodiumcarbonate 14.0 gr. in 100 ml Stir 2 minutes Add in 10 minutes Sodium bichromate Sodium sulfate Sulfuric acid Aluminum sulfate Sodium fluoride , in at pi . *7.6 S*. 2.$ gr. 8.2 gr. 9*3 2.0 gr. 900 ml 70F 1.15 pH after strike 1.4 Add fetrasodium pyrophosphate Sodium carbonate 4 gr./io co 18.4 gr./200 ml . to pi 6.0 Seat to 190 in1 hour. Add with 2 minute Intervals Aluminum sulfate Tetra sodium pyrophosphate Sodium carbonate if necessary 9*3 gr./lOG ce 4 gr./200 co to a pH 6.0 Filter wash 804* free Dry 16 hrs./1400 Bake 5 hrs. at 220F. DUP050067424 I~408-*?3 for Fails? Based on 66540 Codas Y-433-D K/^ is i, Y isId .XSeakT l Size: Approved By: Coupling Fat Strifes Fats 5^12^1 TT^"HIsl2W Prep X JFAI4B: 3HSTEUCTI0US u s e ib s . CODE J ACCT* IBS Is Weigh and hold at Hogshead for step 18 '^r*tleTfin'^rissolW'l"4:Og5Tlc^'*wa:^er*ax^^T20^ ' i4d .1. j : ; .mo .7 It c T" 3 8 170 B c^rjs.-wsK't'irv'ia'SSS S*F $ "^e'Tel.gh aSS"l*<jftarJ'.atl 'E^iSTtead" 'Mr11 step 3f, '^;r``~7eTflT^H^Isl5oT5^Xrr'3^P'8rsT~iiTeFa^TMl2(5s'F''" ho ${m 805s{* 3SS 'So) water into strike Fat., Tri?u!rtrii?Q^i^^ If"4 Si" Adjii-st" t& 46" a.73"77F. I?* lISl'i&T to wf|T^7 .o?1$S5* Beeord; 5$ . 0 IDs *5et agitator sdT'SI, :BM$ ' Ho.g:S Head ..i$.9. C^nJ ..mfcsr^.i3rjto..j^ ........ ... ..r... 3 & &SU._ff*tJft'_fi2Li.tefliaQ....... .. '...,. - __ __________________ 13o Add &3 weighed in stew 1 in 2=3 minutes<> ifrieaT'ToHS^l^Fr . i,S.J...^..t..i.52...irt. _ . ...... ,....._.... __ 40 717^"'f' ' 40 8 "It f If a X 8' i u 1 . ' . : "* *~"*~-* ' L . .<-."?WE3w rsifc-rtw-.^efar j us c> OClieigh andTlioXrf at seale tank 35F ttr .step. 2l r77^eigl5 andTKSXSri^ .seals' tank 3S1 for "step 22 ~5r~ it It U--gf-J 93 H OoVo ^'"IWWrWTWTl^T'SMFWFJX'WfinMM^TMRMTK EfTS ?W ABIB.J______ _ 5 W.c 'Run .rt s.oltition......nisnar.e.d. in.ste'tas._H-i strife Fat on, the surface in 3~5minutes <> 19 .Stir 5 35i 201 iun 17^ 1'203""Ct ')1. wets? into scale tank 341* 6t. |?X*' Duitip in 3-1.5'$a IgEed in .s tep J.6a .'.. r Si 3i ' " is 77r'TJuHp"'IfT^UB' step 17 ,, ::.T... .t....... ;.. . _____ H. ... .........:.. SnVo 7, 24 0 Bun in (stir tank 355 he fore.) . .. fe.ly-W' *1V' *4. jWf/r?f,*3& X!S<a3<`WKW%' a "'IraJT^h'',^^,*,,,"^ lW... 'l"^,,^",.,.". ,."IJ,''",,l,"'kl',H*,,c'!B,avs"'K.>n.%*T'Wfi'.M"0'.".t>5erea,a,'e'rw*>-wM"w"/'"** ""sV'? --l*,!"*,l,'"l,"' ","!""- ^T*isKSftrrtr^^59^t97^--* 27r"T^f^M^eoWST^Br . 2frr7HtTH:TnnrT51B^..^ -- -- -V- k^top agitator 1 ... 11 I! 5.1 a....._...:..:., ti | SL^hj^step^ knS J4_ at 7377F without agitation into strike Fat ....... ... .~T35ru the under surface strifes line j ___ . as' Papiaijr as poss6le!* fiecord: iiiae started__ t it .... --o-.... i . b -. - 357 ST""'SMS ',20,r`%8hwVilmy^mf&F` Into" "vat1 3Sp" r ,1 .'.' ' "TTI '"" ... --...,,-...J - - - II ...._....... 8o and'.Steam*... ' '" ..... ..:"T 'mrr "'.... 330 Add $=i weighed in step 2 in 2=>3 minutes. ...1 .. J..... ....... 340 feat to 0O-1POo F ......... i' i l5.fi..Stifeto ..dlssolVo... .' ,,.. ____:....r... ........... ...... .......... Continues on page 2a ....... |....... i .. ----j--L-- DUP050067425 DUP050067426 CODES. Y-438-D PROCESSi Coals 1593 Dates MAKING AREA MOTES Est,, Loss Remarks Lbs . ____ ____, pSTRUCTJOBS Vat ,*Wn*yisa*to7H~ft.-.f.lt&lli KWinVTOIMOHWOWO^ Date Time Released by Press Hoo #2 .. . North #2 Souih , , ........... Press wifch~OUv agitation*iwrxiyft'jw^mcv< Hash to 8' hours... Record; . ohms Make first. test after___ ____ r&. SfpscisJ. Instructions-.:. fonBleedlns I After &a.sh.im notify making. to jpye>. .1 pare slum solution pump thru press I c^k^jjai-JMsis^,__ _______ Samples s.v ms w .s v ^v*mt o >Vw iiiiiib w imw o www*vif,<8a'<flsty>.'.<iii>>.iMtt^?i;w,A'-x:,y-g<y*y} Deliver to ---- - ------ -- -- -- .. I 'xs7SX'a*w*wiv DRYING AREA INSTRUCTIONS. n^MNwiti^vMw o^-wa: L1I(V BVo . Bum'leans Hours * WMMfc.mitMW,li lull 1 12 + 12'> P" &~~B~ Zj -M0__22LL | Lump e on tainer s chart? n-ly.>Hn.ol Special instructions tfon-Blasdlm J Drverso Use .. gK<a Samples j>!.x-i*rili?**'M.'.5 fci-V Deliver to Liners *?;a^ww<'iiw*=l .1 a GRINDING AREA IHSTRUCTIONS Grinder No 10 LSoP Special Instructions: Non-*Bleed.ingj. * Samples .1 -3 envelopes" ldt.1ilS.'LJulL^.S.Stl.Dl_.lis.t orat g j :>_ P&Cfe&jtinif * S*r5. Cj a3.Tv o -.-*SWkj<S*T 6frt*e*0 N-iwfcV'aptf'.Jwivflva'-:*-,.a I'STM'^^^T.-MWMUtnvcfyWsiHw;'''' # --s ^^1 PRESS IMG* AREA ROTES . DRYING AREA ROTES GRINDANG AREA-NOim DUP050067427 Y-488-D NOTES lo A decrease In the amount of sodium carbonate added in the white base, accompanied by a simultaneous and equal increase in the second sodium carbonate addition., makes for lightergreener masstones# 2P T:he thixotropy of the press cake increases with an increase in the amount of final, tetra sodium pyrophosphate. Removal of this step eliminates most of the thixotropic character of the press cake, but results in the production of darker and redder masstone products# 3o Increases in total alum quantity makes for the production of lighter aasatoae material# ' 49 "fashing the press cake with alum solution after pressing and washing materially decreased the thixotropy of the press cake# Some further increase in the volume of solution should be attempted to obtain batter distribution of the .alum# If this proves to be only partially satisfactory, an increase in quantity of. aluminum sulfate used should be attempted# Further studies on variations in the amount of sodium fluoride and of the quantity of sodium bichromate should be investigated as possible means of decreasing the masstone redness of the product# 60 the effect of higher strike temperature <90F) should be investigated# DUP050067428