Document O39agVbzXxnb9pvbbKBeyoMNw

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 YANDERPOOL STREET NEWARK, NEW JERSEY Serial No. KN-48-32 Copy No. 1 Numerical File NEWARK PLANT PIGMENT COLOR RESEARCH REPORT FINAL REPORT LABORATORY STUDY AND PLANT DEVELOPMENT OF BL-586-D. (Alumina Hydrate Lake of RT-525-D, the Mn Salt of 2B Acid BON) Period Covered: JANUARY, 1948 to OCTOBER, 1948. FILE. DATE: 222.24 N42178 ----------------------------------------------------------- Copy tos 1 - Hoaerieal Pile 2 Research Office (222.24) 3 * Library File 4 - t* Chalupski - Float Files % - 0. B, Killiaa Serial Ho. KN-48-32 Copy So. i SgWARK PtJkW* PXGMBIT COLOR RESEARCH REPORT F3HAL REPORT TWMt LABORATORY STUDY AHD PLA8Y DEVSLOPHEHT OF HL-536-D. (Alania* Hydrate lake of BT-525-D, the Ha Salt of 2B Acid BOB). PERIOD* JANUARY, 1948 to OCTOBER, 1948. CHAROlt A-IC-37, A-IIC-37 SUBMITTED BY* F. S. Hiein mmom b y * a . a . Br BAYS SUBMITTEDs 11/24/48. BATE ISSUED* 8/30/49 DUP050067083 The development of BL-586-D coincided with the development of RL-582-D (recorded in XH-48-31) end followed the same pattern* RL-586-D is the mineral oil treated, aluBtina hydrate lake of BT-525-B (a 50/50 alumina hydrate/toner ratio} and was chosen as the most desirable of mine lakes made on BT-525-D. A seal-works batch of RL-586-D was prepared and on the basis of this batch, lot 9576, Sales . decided that the lake be developed in the plant and standardised. II. m The lakes of BT-525-0 prepared in the laboratory wares alumina hydrate, Blanc Fine, alumina hydrate/Elanc Fiat, China Clay, Asbestine, basic lead carbonate, Kalvan, whiting, end manganous hydrate. As stated in the introduction, the alumina hydrate lake was considered the most desirable. Early work involved paste mixing but when paste mining of HL-586-D was compared with slurry mixing, the differences of the resulting products in vinyl dispersion were negligible. Slurry mixing is preferred to paste mixing in the plant because it eliminates the use of the Abbe* Lenart mixer. High speed pulverisation aids vinyl dispersion. To reduce dusting of this pulverised lake, mineral oil was added because mineral oil had no effect on tinctorial properties of the pigment. In the plant Fractal A was substituted for the Hujol used in earlier work. Following the semi-works preparation of lot 9576 of SL-586-B, throe plant batches, lots 59900, 59926, and 59954, wera made. Bo difficulty was encountered in their development and all were close to lot 9576 in properties. Lot 59926 was sst up as standard and HL-586-D(B) was set up as standard formula. III. iv. SiWL3Wm.t Sous d is c u s s io n o f wumsm* 1* Fiuvls In tinctorial properties the dry addition of HL-586-D to vinyl composition equals the pro-dispersed addition of the toner control (comparison on equal toner basis}. Vinyls show no signs of migration or crocking. 2. Drying Study Dryingbetween temperatures of 140F and 200F did not affect dispersion of m-586-D in vinyls but did affect yield because the moisture content was lowered noticeably. * DUP050067084 2 3* Fineness 1.9 Z*$% on 325 noon screen. *. ^LJtooSAaa - 38.5 lbs. vehlcle/100 lbs. plgneat. 5* ai3imi.Spjaisafe * 12.95 - 14.05. %U$.Smbm%..pOmagaka - 385. ? rnmmsLMmrn - um 8. Combustion - sparks were rory pronounced at 320C. 9. Busting - lake better than toner control. v. MmmmimMmm* notebook X2?6 * Experiments 18, 44, 53. Notebook 1307 - * 8* 9, 10, 11, 13 detailed tabulations of results of plant batches. 71. MiTOgNCgS* DSH-48-29 DUP050067085  X , `p FREP 1 OTT user 313 4 sTvT -5 1 6 U.S. Bat, 2,225,665 Cost Group - 37 (3054) RL-566-D (B) - 1.5 Mol*, AAB: 6r4-r49 , 315, 323 HA:.. 9-1-49 206 CWD; 9-2-49 1055 106. Std, Hours NCN-BLEEDING ES: 11-21-49 - ! i BON RED LAKE STRIKE 1* Obtain and hold at scale for use in diazo vat in step | its Hun 24" . (8030*) .water into diazo vat ,3*.,,, Weigh in chtua ^ud pour in . _ . ......... M ..4* Turn.co agitator and,steam. . 5*. Weigh and shovel in in 5-10 minutes , , obtained^ijistepl* ,, , > ...... ..... From............. # Met Lot Fronr .......#Net~ lot. From" Net Lot, From* Net Lot" From Net Lot_ X % ,.,,6,.. Heat,, to .95 j . 100F. .....,.,... ................... ........ ..........,., , 1... _ 7*.. Stir 10 minutes... to dissolve*...... .. ^ ........| ,7&7.Test"...and .records. B*Y . ', must ,be +, .......,, ,. ,9* If N-467 dQes not compietely dissolve, raise temperature ___,,.,.ia^5*...?tP? to,a maximum of 120F* . .,..., io,_ Stir 5 minutes, . .., ... v , .. ,........... ........... . ........ . JL^'.7'Ta|s?! 1 quart sample for analysis, 2. 7' .,. ........2... 1.. 7~X1 IT J.467 .1,467. 467 Il.. .,.13.*Check and, .recordi^. , , Normal 29"(963 G.). 14. ^ Check and record: . "..F..,."....`..............~..2................. "'"T" 15* Deliver sample to laboratory* *''&*' Wei^h, dissolve in 40 gallons water in drum and Sold 72217f'IL ?^?9*y4t .for^step 44....... .......... ........ ,.7..L ..17*,, Obtain.and.hold at.scale for,.use in Vat 313 in.stepJ22.1. 16* ,,. Weigh and hold at Vat 313 for step 25. Assume + 106% 4 f ............... x `' ,i --* r .. 19. ,Hun.20" (300 .iimW into Vat .313. . ,. ....... .... .,.,^1 .20* Weigh in.drum and pour.in....... ....... M...... ........ ..... .......... J ,,2l* ,. Turn on . agitator and* steam. ......... ...........: . ___ .___t 22*. Wei$* and add in 3 - 10 mnutes..... ...... _ ................. ... _ | obtained in step 17* I ' .'M#.7.K to" i304Q!f7'777772.7.! 1.'2777 17 11.711 '71 ...24*. Stir 5.minutes.._______ ______ __..___________ ,,.,,.2...__ J .,25., I^p in N-ft weigfrpd in step !& ;_.....,,................ ........... ^ { . 126*7.sXlia.mi^ ....., LX... 112721 61 '300' II 62 6 27, Install chart in temperature recorder on strike vat, 26*7 jtoixl9?7iCid^b. Jwfc*1 217111 _29, ... Turn on, agitator amd steam*..... 3p/Jk Weigh and dump in , 31..Heat to 340-160 F. 7.,..... '.... .... ............ 32, . Stir to dissolve* 33. ^ Weigh and .hold at-.diazp vat for step'36^ # Net Lot_ ' 2.177 ." IMIiIf u \\ (71 ib;ir J1L? f I 'll .(C ont Id, -on page. 2) ......,.. DUP050067086 VAT > D.V. 7 206 8 D.V. 9 206 10 S.V. 11 3 Pa g e : % Co d e: KL-586-D Lb s : i $60# In s t r u c t io n s 34- Weigh in drums and hold a,t diazo vat for step 46 M T' to Z:ro\-.:-. Supervisor f*-: 3:. l^uiailong. Report to Group Supervisor for Calculations Based on Analytical Results, t USE LBS. N- C0DE 28 i ACCT. LBS. 133 _ Gal.X #/Gal. # N-467. 35. Tf ueftesnaryj adjust diazo vat hasari on analjrt.ioal results by adding from # Net Lot ' OR Removing Gallons. 36. Dump in N-58k weighed in step 33. 37. Stir 10 minutes or longer to dissolve. % 38. Install chart in temperature recorder on Vat 206. 39. When step 26 stirring completed, run Vat 313 into Vat 206. 40. Weigh, slurry with 20 gallons hot water in drum, and pour in 41. Ad.iust to 13" (923 G.) at 6&-72F. 42. Stir 10 minutes or longer. 54 When ster> 37 stirring comnleted. adiust diazo vat to id.1 (1501 G.) at 32-36F. 44. Pour in N-5 prepared in step 16. 45. Stir 3-5 minutes. 46, Pour in as quickly as possible N-28 weighed in step 34. 47. Stir 2 minutes at 32-36F, 48. Test and record; KI test , Must be +KI test. 49, Check and record: ", 467 39 5L 57 +900 57 +4050 50. When step 42 stirring completed, couple diazo vat into vat 206 at 68-72*F, under the surface through the distributor in 30-36 minutes: Maintain Vat 206 at 68-72* F. during coupling. Record: Time started Record; Total Minutes 51. Check and record accuracy of recorder: Thermometer 52, Stir 15 minutes. ' T?,,nnrd.,r "V, 53. Heat strike vat to boil. 54. Check and record accuracy of recorder: Lows Thermometer F Recorder High: Thermometer *F Recorder F. F, 55, When step 52 stirring completed, strike Vat 206 into strike vat at boil oh the"surface in 28-32 minutes: Maintain strike vat at brisk boil during strike. Record* Tims started Record i To+.n1 mi*rirhs 56. Stir 20 minutes at brisk boil. 57. Flood to 78" (7488 G.) (Continued on Page 2) DUP050067087 VAT 321 12 S.V. 13 DRUM 14 S.V. 15 Pa<s e : 3 Co o es EL-586-D Lb s : 1660# *>8. Run 30" (*510 is.Y water into vat 321 . 59* Weigh and dnmn in In s t r u c t io n s ' USE LBS. NCODE ACCT. LBS 819 551 &9 60. Run Vat 321 into strike vat. 61. Stir 30 minutes Record: Time started 62. Weigh in ltCi gallons donm 61- To r tan tIT.i ghtoi oil Mi t t > 1 64. Weigh in Daxl and tour in 65. Weigh in nail and nour in H 66. Adlust to 60 gallons at 70-90*F. 67. Stir *> minutes to smooth emulsion. 79 3 % 640 7<3 641 3 7 5.5 68. When step 61 stirring completed, pour drum through Vat 321 into"strike vatl 69. Stir 30 minutes Record: Time Started 70. Press with agitation. TBffi STARTED ii M " ii TIME FIN n ii it n 0PTR it ti a ', . DUP050067088 II COD:*: HL-586-D B ESSis (ir ~ eoas 1660# OATS: HA: 9-1-49 jf. Laafe 'PlSSIi '^st }_ J^' wMwAVK^XVN : :''.l-a. .-ss^<!M;i>-`'.'.`-'' :**> MAKBG ARM . . , Lte* 'is_*_.__1_1_-_30-4.9. HlSSfKG AR3A WS'jSlWTXCilS ,.*.^ vt'>s-i:v.'W.'',-v>--'--W-`.,-v.,^w.svs>..,A`>-w#>.'V/iY,('?w.S"t'Ss*-.''yi'':'-,*i'^iciN'.'-^,>-i>.'-v:i'.>Yv.-<ViYy;-.-vsf.'i:';1 "*)ai-a fxsii ^ ,,>,, St, > w ^ * toePife/ IIs^^ t'j's ,,<* '*.&> A^ivii&r*5'* ,FtIPV iW' % ylpliate Free - ,, XXX l>' r, 'ii ,, , jjiV*-. ,,*,.- ;? \\ , ,, 6 Cars. SsjoewM. 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DUP050067089 iSc!SrMEI X. imOMCTIOl: RH55~JD is a mineral oil treated, alumina hydrate lake of K^-S^S-D* To improve the dispersion of ?.T~S2S-.1> in vinyls, a group of lakes was prepans d by paste mixing ET-oCd-D plant pros soak and various exbcadora-. alumina hydraio gave the most promising results (a 50$ lake being as good as a. 78$ Idle) so 'a semi-series batch of the $0% lake using slant tone;-? slurry ?;as prepared. bi material wm treated with '&mineral oil emrloicn to docr-oas dusting of the lake* Os the basis of the c:i sc&i %ro:?l;s batch, lot 8576, .Sales decided that the ltd o to dovelcpsc! In the plant and standardised* II. .HOPES* *hm 1. ill MB3f procoss replace a tin previous formula, AEL-SSS-I), and differs, as follows;- the tenor 1c flooded to 73 inches (74086) instead of 85 inches (&R'5o&) 5r Rtri'-o met to permit totter .agitation of hydrate"toner slurry? the Ncluao for clurryleg the alumlm hydrate is increased from 22 inches (tfdC) to $0 inches TdlOS) in V&t 581 and the volume for tfco caulsion is decreased from 72 to 40 gallonse 2, Botes cm af ~525*'I{S) hold for the first 57 steps as the tinctorial properties of EirBSG-p vary directly as the mass tome and extension of the toner control* 5* The iir,er.al oil emulsion doss not -affect the tinctorial properties of lUj-S-SC-'X?? neither doo-a it eliminate dusting but it does decrease -dusting:. 4* 'laying at temperatures higher than 140 up t-e 20GF did not affect irlnyl disparsi cm but did affect yield because the. higher the drying temperature, the loner the viator content and eon**' sequent ly, the lower the yield* 8* The moisture coxvbont on the first three plant hatches varied from 13.0$ to 14*03* 6* The fineness on the first three plant batches varied from 1,9% to 2.83 pigment remaining -on a 525 mesh screen. 7 The presses!: was firm and was about 38$ solids. XIU TESfllGt 1* Hubdut - cam as for ST~523~I>. 8* Pry fineness by TF-51-7. DUP050067090 OAtCUIAfSD O0If??OSJSXOI & GOAL YIELD: 'ffityni/1 ifrrf nwrwtn'irririrr trr iWrtrrnn-rM irT'--rM`n'n- iW*. *>*< Calculated Gasposli!Ion Ha tones* o? 3*J ilc$4 Alumina Hyiraivo sliaj?al Oil BOH y?,<3 "> ?< tw:% 800 Xbs 780 80 Bolj ms* cal Xisld 1880 lbs. ,:a.3 .is,: 1400 lbs* 5fiiydi*ows molstm' " 12# 8$ Hof03?no 1807 -IS ? Ba Klein $m22~4& &P'p:/'-Wo ill A* A #Ej?ls35ola3?. 9~22"48 DUP050067091