Document vVQn1jo3YX6YQNn49rm3GGD26

E. I. DU PONT DE NEMOURS & COMPANY KREPS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial No. , Copy No. 1 Numerical File ( Period Covered NEWARK PLANT PIGMENT COLOR RESEARCH REPORT T:cL mm. iia s s ? $Ro<mmi ZB$ X9S.3 V 213 FILE: Ffil)o X2p 1951 DATE: 3 A Serial No. KN-51-12 Copy No. 1* Numerical Pile Copy tot #1 Numeri cal File 2 * Researoh Office (213) 3 * Library File (213) 4 - V. Chalupsfci * Plant Filea 5 * 0. B* Killian 6 - W, P. Spengeman/J. B. Callaway/PJM 7 - Extra 8- NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report "SEALED-VAT." MILORI BLUES PLANT PROCESSES 1843 - 1950 CHARGESt A-I10-189 A-IIC-195 A-IC-5 SUBMITTED BY: J. 0. MORRISON APPROVED BY t DATERUBMITTED: Fan. 12, 1951 DATE ISSUED* & Feb. 12, 1951 DUP050068556 I^TROKrCTIOHs. This report briefly summarizes intermittent; plant develop ment study and standardization programs* A standard stepwise formula for making pigment of toe desired quality is included* An evociicofr of progress through tbo laboratory and' of the project ie to be found in Plant development studies wars active intermittently throughout the period 1942-45. Pigment of goal quality in slurry fora mo produced regularly but severe quality deterioration t invariably encountered duri 1944* however* a plant working standard of 'satisfactory quality (lot 7303) was preparod from pleat pignent manufactured at sing! prose batch size by the K-2161 process. Standardisation emphaaJ was then placed on the companion double-press batch size K-2162 seas for economy reasons* The concentration increase had little'If any adverse effect on slurry quality* but deterioration daring processing remained a serious problem* Unfortunately* it was esta blished that the inert atmosphere products were inherentlj from 2 to 2-1/2 percent costlier, ingredient-wise, than conventional pri* This penalty difference was determined to be real* by ohemioal analysis of various experimental samples* and was traced beyond doubt to the sealed vat technique itself, the higher complex nitrogen content of the sealed vat products may well be an indication of greater chemical purity* i.e* less absorbed Impurities, since tbs products are noticeably superior to conventional products in color purity as well as texture. Recognition of the cost penalty resulted in abandonment of plans to release the improved product as a conventional pulverized pigment* but it was agreed to continue with standardisation of sealed vat processes for the iron blue component of "super-soft" Chrome Greens < Project A-IIC-195) and also to standardise the blue in dustfree granular farm (Project 214)* in whioh "super-soft" texture is rto roll*r *- Rone of the contemplated applications of the sealed-vat process have actually materialized to date* The attached formula embodies all of the features to date* Directions for manufacturing a granular form are given in the (B) B jraLftBMSsp A patent application, Morrison and Perkins Case 1077X* h8 been filed covering the combination of vigorous agitation with con trolled oxidation at the shite precipitate stage* DUP050068557 REFERENCES* Project files A-IIC-189 - 195 * 214* KN Reports - 42*50* 65* 155* Laboratory, Development, end Plant Assistance Group monthly summary reports* DSN-46-27 Sealed Vat Iron Bines Semi-Works Studies DSN-46-28 " " " w Plant Studies (Includes DSN-46-32 tt * " * B-2162-D. JOMslg Att* DUP050068558 sxu&a&a This process describes preparation of milorl blue by the sealedvat process* for use as the blue component of IfuenCh-mixed Chrome Greens, Its mo for this purpose was very limited* since a bins of tbs desired properties for this particular purpose was developed with out nee of sealed vat technique (see (C)B-269-D* or B-300-D(A) ) The sealed-vat making prooess baa been written on a step-wise instruction basis. It embodies tbe significant control features of previous experimental formulas of this type (K-2162* iC-2161* K-1681, etc), via striking with vigorous agitation in a oarbon dioxide atmosphere to prevent premature oxidation of tbe slurry beyond an op timum level (controlled by peroxide preoxldatlon of approximately l of Idle copperas) * and use of bichromate as sole oxidant* Additional plant study is necessary to confirm satisfactory reproducibility of texture as well as to attempt to achieve economies through elimination of tbe oarbon dioxide and peroxide (thus substituting controlled air oxidation for the latter) and substituting chlorate for a major portion of tbe bichromate* Provision for tbe latter study bee been incorporated in the formula (steps 15* 16* 17 and 54). A special temperature con troller cam is employed to provide a continual temperature increase and positive pressure in the vat throughout the preoxidation steps* Tlnctorially, tbe prooess responds to normal iron blue control variables* She quantity of 5-540 may require adjustment to produce the desired masstone color* PRESSING AW WASHING Maintenance of the soft texture attained by tbe sealed vat strike demands thorough oid uniform washing* which baa never been con sistently attained in past plant manufacture* The press burden of tbe K-2162 process has been reduced by approximately 6% In an effort to improve washing? further reduction may be neoeasary* although it is hoped that this may be avoided by effective use of electrical resistance end point measurements of the wash water. The specified end point (2800 ohms) is subject to revision based on experience. uaau Past experience with plant drying of sealod vat blue has like wise been unsatisfactory. Encouraging results bate however bom recently Obtained with other blues using the specified reduced time of 10 hours at 200p without increase in the standard 19 hour overall cycle. Pans must be uniformly loaded* deformed pans which prevent uni form air circulation must be avoided* and overdrying of any portion of the lump color must be absolutely avoided. DUP05006S559 -e* Same as K-2162# 317 lbs# anhydrous per mol, of ??$* (SB 113.$ -p 27)* $17 at $308 ~ 484 * 3477 lbs* anhydrous 3651 lbs* at 47g Ha. SX3BMITTED BTj J. 0. MORHISOH JMTJAHY 12, 1851 DUP050068560 '/AT 38<r i i CODE:. GOAL;. M DIAZOVAT:. COUPLING VAT: STRIKE VAT: k aSEALED VAT .SIZE: .__ ,, >8l ,280,2^2 APPROVED BY: JOM: 12-3-48 . HA: \2-\-W~~ CWQ: - 12-6-48 JD: 12-748 NAME: MI LOR I BLUE INSTRUCTIONS USE LBS. NCODE ACCT, LBS,. i. Pu mp in t o s c a l e t a n k 36O CNx* CNxs Al k a l in it y Al k a l in it y 4> T * T M to- OR - . . ....................... k. St a r t w a t e r in t o s c a l e t a n k $G -- , - B. Tu r n o n a g it a t o r a n d s t e a m. Cl, We ig h a n d d u mp in - CL Ad j u s t t o 77" (30530.) a t 704-l06F. Ef STIR ?0 MINUTES OR LONGER TO DISSOLVE.TM S S .. 594 5308 594 4 * Wise. 2. We ig h a n d h o l d a t v a t 383 f o r s t e p 5 1670 *40 1670 33 3 3. Ru m 15-20"(+ 2450.) w a t e r in t o v a t 383* 4. Tu r n o n a g it a t o r a n d s t e a m* >=5: Du mp in N-340 w e ig h e d in s t e p 2. 6. a d j u s t t o :40" (490G.V a t 70-75F. . 7. St ir 20 min u t e s o r l o n g e r -t o d is s o l v e . V"', ' S.V.. 4 , * - ..8^,REM0WE,STEAM-VENT. SEAL , IN .STRIKE. VAT,.AND ..CLE AJL*....__.... 9. Se t a g it a t o r a t 12 RPM. 10. GET INSIDE STMKE VAT AND HOSE TOP, WALL, AGITATOR ETC. II. Th o r o u g h l y c l e a n * 12. Ru n 20-25"7+ 26250.) w at er in t o s t r ik e v at v it h .. AGITATION. IT. Bl o w s t e a m l in es . 14. Ru n w a s h h a t e r t o s e w e r w it h a g it a t io n . "r~" >V; ---- .... ..... "1W~ 15. We ig h a n d d u mp in t o v a t 5 16. Ad j u s t it 24" (400,), 17. He a t t o I2Q-140T t o o is s o l v e . ' . ... s- i w ^_ ,$7 18. Ru n In t o s c a l e t a n k j87 f r o m v a t 343 . * . ... 6' ; ; m 19. Ad j u s t t o 24" (400.). 20, St ir t u n if o r m s o l u t io n . 1w ` 'h - I '*** * ': H1i' .. ..... , , .. nil 1. . ... r.. ... ' ~J **' " ** -* ........... ` 12 i 8 < *" *' '* * * 545 > " 38BT 21. We ig h a n d p o u r in t o v a t 386 . 7 " 22. St a r t a g it a t o r . 23. Ad j u s t t o 30" (860.) b y a d d in g w a t e r s l o w l y * .. 24, St ir 3-5 MiNiitES t o e mu l s if y . . t^\ WEIGH AND POUR IN IN 2"3 M1NUTE8 V .-,1 ,_ 26. St ir 5 min u t e s . 27. Ch e c k a n d r e c o r d : s o l u t io n -*: s . mu s t b e o a r k .-a n d -- .197 1 58.. w 197 i1 ; 122 5* ;* 56' H:.. 1;! -1" \ Dr u m "8 Misc VI 9 CLEAR. : - 28. Ch o p t o 3" l u mp s o r s ma l l e r in b a r r e l STRIKE VAT Fft STEP 48 - 29. We ig h c a r e f u l l y in ,p a il o n -o y e . s c a l e . '* ,< - - v ' v". and ho l d at . .. ; CONTINUED ^ P^GE ...................... .......^.1^ + 150 ; 4i 1 ... i-. 48) " 150 5Q3-. 4 U -------- !I DUP050068561 ,, VAT Pag e: 2 .Co d e :i^)*2694D Les:- 3651 . SEALED VAT ' In s t r u c t io n s ' USE LBS. ~ NCODE ACCT. l bs . ^0. Dl LOTEf T T aAfc.^N$.WITH M^Ter ANB HOLO *T S.V. FOR ' . _, 5. STE-P- 4-0' .--- ' - - .: -.. --- ----- ' '----1-T* 1r-S-- Mf . . .- SiVi io `Vi.. * *' . . 31. Wh en s t r ik e v a t r u n s 'e mpt y . h o s e t o p.w a l l .a g it a t o r et c FROM OUTSIDE OF VAT AND RUN TO SEWER. 32. Ru n 5-15" (+ I050G.} w at er in t o s t r t k e^s l at . . 33. Pu mp in t o s t r ik e v a t w it h o u t a g it a t io n f r o m v a t 3o 2 pH Fe M <6 pH Fe M * 34. Wh en s t e p 7 s t ir r in g c o mp l et ed , r u n v a t .383 in t o s t r ik e VAT THROUGH SCREEN. 3*5. Ca l c u l a t e an d r u n in t o s t r ik e v a t f r o m s c a l e t a n k - M . T ... . * (Us e l bs N-594 )X'(^Al k ..:. )= 'Ac c t .Lbs N2] 36. In s t a l l , s eal ed v at t emp c o n t r o l l er c am rop s t ep 52 1 * Leav e a ir s u p p l y o f f . -h - .37, In s t a l l .c h ar t in t emper at u r e r ec o r d er . ------ , 24 3475 24 27 ' * itr .' > ' ' 1 1 `.,1 ' r .r l. 3S0 IS s.v. 12' ( 39. Ch ec k aWd : r ec o r d 'ac c u r ac y o f c o n t r o l l er : . Lo w :'t h e,r Mo met er . FvCON'Tr WLl er J . .... ./ 4*' 4.0i Ad d . N-509 PREeARio s t ep 30. 41. St ir -3 iirNUTff ^ "i/v -*-.* ---- i" - ' . 4 42, . STOP ACffTAT" ^"">>*JJL *! .- ?u.- -"7.. - " ? .... '_r__ ' ./ . - ` : \ . . ..... ' 43: Ad j u s t s c al e:. t aR* 3JS0 xB. :>77,,.(3053Qn at I04~I06F. ^ i j ' . ^ v: * ' ' i 44. Pl ac e s t eam v es t ^Al,;i.NifaTR:i!KE v a t .- V. 1 45-. Seal r ear t r ap oooR^:^... . 46. Ad j u s t a s it a t o r `f6j 46JPH. Do n o t s t ir . * iJ! ij. > 47.. FIVL WATER s Eal s an d l eav e w at er r u n n in g . -* ,4t5.. WIMP IN N-481 PREPARED. IN STEP 28. . -1 49. `Sea l - f r o n t t r ap d o o r . 50. Wa it 3-5 min u t es , t h en s t a r t a g it a t o r . 51. St r ik e v aV -360 At iD4-I066F in t o s t r ik e v at at 74-76F. :lV: w. o n t h e s u r f ac e'in 40-45 min u t e s . * 52. Tu r n o n a ir to t e mp e r at u r e'c o n t r o l l er an d IMMEDIATELY s t a r t au t o mat ic h e a t in g c y c l Y: ' H'1-4 ..... .4 ' ' -7 . (A) 90T t o IOd6F ik 5& min u t es . ~' (8} IOOT t o I96F, iir^rMNUTES. ' Pe c o r d : t ime s t a r t ed " At U .. " ' 53. Wh en s t r ik e v a t is e x a c t l y a t tfo'F, Pu n in f r o m s c al e \ - . .1 . . . TANK IN 5*10 MI NUTES - ,M v- k T - \ <fX . ' A*, - > 2377 ' 54. Ex a c t l y 90 min u t e s af t er s t a r t o f h Ia t in g (s t e p 52) r u n v at 387 IN IN 2-4 MINUTES ; : V......! ir ..-.-S _;'.j -1T'_ Rec o r d : t ime s t ar t e d ., . 1 . . - OR. If N-12 is u s ed : A. Ru n v at 389 in at e x a c t l y 90 min u t e s . B, St ir 15 min u t e s . C. Ru n v at 3tf7 in in 2-4 min u t es . 55. St ir 15 min u t es . 56. St o p a g it at o r . Rec o r d : t ime 57. Sh u t o f f w at er s u p p l y t o s e a l s . 5o. Sh u t o f f s t e a m. 59. Re mo v e s t e a m v e n t s e a l . -.1 \ 'C*X'C ; \ <0NTi*|!W^OWv(PAgr "T " AM ..h .i-C"'?": . , ________ ----_------ -- -------------------------- ---------- .----*---------- 4- DUP050068562 Pag e: - Co d e: (B)B-269-D l b s : *651 3 SEALED VAT J 60. Ad j u s t a g it at o r t o 12 RPM. in s t r u c t io n s ' 61. Open t r ap d o o r s . 62. St ar t a g it a t o r . Rec o r o ; t ime 63. Tes t an d r ec o r d : Co pper as XS . mu s t be +. 64. Ch ec k an d r ec o r d ac c u r ac y o f c o n t r o l l er Hig h : Th er mo met er F,C o n t r o l l er F . 65. Fif t ee n min u t e s a f t er s t e p 56, r u n v a t 3o o in t o STRIKE VAT. 66. St ir 1 h o u r . Rec o r d : t ime s t a r t e d - USE LBS. a__H&L___ Ji N- CODE ACCT. LBS. 67. Sh u t o f f a g it at o r . 68. Air c o o l f o r 8 h o u r s o r l es s t o i4o -I45bF, Re c o r d : t ime s t ar t e d . Rec o r d : t ime s t o pped . Rec o r d : b F. 69. 3 HOURS a f t e r s t a r t o f a ir c o o l in g , t u r n o n a g it a t o r FOR 3-5 MINUTES. 70. 6 HOURS AFTER START OF AIR COOLING, TURN ON AGITATOR FOR 3-5 MINUTES. 71. Bef o r e r ec o r d in g f in a l t emper at u r e in s t e p 49, STIR 3-5 MINUTES. 72. Ch ec k an d r ec o r d : ", n o r mal 77" (80S5G.). 73. If n ec es s ar y , f l o o d t o 140-145'F. Rec o r d : b F. Rec o r d ; ". - 74. Pr es s w it h a g it a t io n . _____ TIME START II If a1 TIME FJN If ll ~~ n 1 ~!-T SPTR *1 ....... *..... ; .......... * DUP050068563