Document B56680k1qYqbGdLLKwrKwjM8J

* E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY S'rial No. KU-48-31 Copy No. j Kumar leal Fila NEWARK PLANT PIGMENT COLOR RESEARCH REPORT FINAL REPORT ( Poriod Covered: LABORATORY STUDY AND PLANT DEVELOPMENT OF RL-582-D. (Alumina Hydrata Laka of RT-533-D. tha Mn Salt of PCAMBA BON) OCTOBER, 1947 to NOVEMBER, 1948. S A T S FILE: DATE: 222.23 3* / ' P ( ''/ ` p m .^-3 N42177 Njtxra --------------- Copy to* 1. Somerical File 2* Research Offto# (222.23) 3. Library File 4. f. Chalupski * Plant Files 5. 0. B. Killian Serial Bo. KH-48-31 Copy Bo. 1 HEWAHK PLABT pmwm c o l o r r es ear c h r epo r t FIHAL REPORT rats* LABORATORY STUDY AHD PLAHT DEVEEOPliSST OF RL-582-D. (Aluiaina Hydrate Lake of RT-533-0, the Ma Balt of PGASiS* BOS) per io d? CHARGES Oc t o ber , 1947 to mmmm, 1948. A-IC-37, A-IIC-37 SdBlfflB BY* F. S. Hath APPROVED VSt A. A. BrlaTzOlara BATE SUBMITTED5 11/24/46 DATS ISSUED* 8/30/49 DUP050067074 Early in the study of reds for vinyls, a rather thorough study of lakes of organic red toners was undertaken* Fro mis study of lakes on modified HT-533-D, It was concluded that the alsaiaa hydrate lake gave the most promising results Ca 50/50 alumina hydrate/toner ratio being as god as a 25/75 ratio}* A semi-works batch on the 50/50 ratio using plant timer slurry mas prepared. This material was treated with 5p mineral oil emulsion which reduced dusting. : On the basis of this one seal-works batch, lot 9558* Sales decided that the lake be developed in the plant and standardised* II 1 The lakes of RT-533-0 prepared in the laboratory wares Alimins Hydrate, Blanc Fire, Alumina Hydrate/Blanc Fixe, China Clay, Asbestine, basic lead carbonate, Kalvan, fhlting, end manganous hydrate* As stated in the Introduction, the alumina hydrate lake <50/50 alumina hydrate/toner ratio) was considered most desirable. This early work involved paste miring so when interest was shown in the resulting products, slurry mixing was compared with paste miring and differences in vinyl dispersion were found to be negligible* Slurry mixing is preferred to paste mixing in the plant because it eliminates the use of the Abbe* lenart mixer* Better dispersion in vinyls was obtained by high speed pulverisation# Alumina hydrate lakes so pulverised presented a dusting problem. This problem was not solved tout reduced by mineral oil treatment - mineral oil being a substance which had no effect ou tinctorial properties of the pigment. In the plant Fractol A was substituted for lujol used in earlier work. Following the semi-works preparation of lot 9558 of HL-582-B (the code assigned to the mineral oil treated, alumina hydrate lake of RT-533-D), three plant batches, lots 59812, 59831. and 59856, were made. So difficulty was encountered in their development end all warm very close to lot 9558 In properties. hot 59812 was Set up as standard and HL-5S2-DCB) was set up as standard formula. in. **. 17. 1. Vinyls In tinctorial properties the dry addition of HL-5S2-D to vinyl composition equals the pre-dispersed addition of the toner control (comparison on equal toner basis). Vinyls show no signs of migration or crocking* DUP050067075 2 2. Brvlng Stnfrr Drying between temperatures of 140df and 200% did not affect dispersion of BL-582-0 in vinyls bat did effect yield because the aolstore content wee lowered noticeably. 3* ytnancaa - 1.35$ - 1.65 on $25 meeh screen* 4* Oil Absorption - 35.6 lbs* vehiele/100 lbs* pigment. 6- aMte.gaaitf...at .tmiafa - t&*t 7. SMOlflE OTOTlty - 1.74? 8* Combustion sparks were very pronounced at 330%. 9* Panting - lake better than toner control. mm&hjmm&t Notebook 3L27d - Experiments 1, 48, 51* Hotebook 1307 - Experiments 5, 6, 7* 118 14. Detailed tabulations of results of plant batches. VI. HgmmCBSa DSH-48-28. DUP050067076 FCKTOvA H0T3S I. xmoBOOTIOI: idMi KL-532-I5 Is a mineral oil troatod, alualaa hydrate laic of modified BTH3'33'~D {modified insofar as It la not glyceritm treated), BT-~S$3-I> does not .disperse noli in vinyla, so in the laboratory a group of lakes was propored fey paste mixing BT-533HD untreated plant presscake and vari<ms extenders Alumina hydrate gave the most promising results <& 30# laic being as good as a 75# laic} so a Semi-works batch of the 50# lake using plant toner slurry was pro** pared# This material was treated with 5# minors! oil omuls ion which decreases dusting# On the basis, of the one semi-works batch, lot 533, Sales decided that the lake fee developed in the plant and standardised. / II. BOTES% 1* The wBn .proeeoo replaces uhe previous formula., ML-5S2-D, and differs as follows r> th volume for slurrying the alumina hydrate is increased from' 16 inches <2726) to 28 inches (3748) in Tat 521 and the volume for the emulsion is .decreased .from 55 to 20 gallons* 8. lotos on HT-.55S-D (B) hold for the first 57 steps as the tinctorial properties of ja5r5S2-& vary directly as the aassfcon .and extension of the toner control* 5. The mineral oil emulsion does not affect the tinctorial properties of EL-382-Dj neither dcoc it eliminate dusting but It does decrease the dusting tendency of the pigment* 4, eying at temperature a higher than 140F up to 200F did not affoot vinyl dispersion but did affect yield because the higher the drying temperatlire, the lower tho water content end con sequently, the lower the yield* 5. The .moisture content on the first three plant batches varied from 14.5# to 14..75#$mciature content of standard lot $2612 is 14.5#. 6.. The fineness on the firofc three plant batches varied from lo55# to 1*65# pigment remaining on a 325 mesh screen, 7. The presscake was firm and contained approximately 40# dry color. XXI, TESTIHG t 1, Eubout - same as for B.T-533-D. 2, Bry Fineness ~ TF-31-7. DUP050067077 --2*" TV * GMiGVltkT'BD' OOUPCBXglQg At, GOAL TIE I# i Oalciilatad CoHjx^ltlcia w m tom* of ?mm - BOis i-Xmlma layoffat }&mval oil 4vx> 56 *3 .6 .535 1I>S. 303 50 w r"jmrw%* Goal 1060 lbs* nas is** 030 55 ftshydff-cus molstaffj 14,5$ H feffs.no i 1507-15 Ol^noi: F* S* Klein - 9**2S"43 .Xrpvovocl? A*&lb?isaolM?a 9-28-48 DUP050067078 3 3 /AT ' P:=P 1 D,V. z U.S. Pat, 2,225,665 Cost Group * 37 (B) RL-5S2-D K#_ -Ets am 1090 s>zl~MmK DIAZO VAT: 3QI ^33 ^3 I COUPLING VAT: 206,207 213 APPROVED BY: HA! CWO: AAB: m/iw NAME: (3012) Std, Hrs, 6.^0N-8LEE d in g ___ INSTRUCTIONS USE LBS. CODE AU/0/4Y ACCT. LBS. 1. Ob t a in an d p l a c e a t s c a l e f o r u s e in d ia z o v a t in s t e p ft 350 2* w(2l*iQ.) w at er in t o d ia z o v at 3. We l s h in d r u m "a n d p o u r M- ft. We ig h an d s h o v e l o b t a in ed in s t e p 1. Fr o m #n e t l o t Fr o m #n e t Lo t Fr o m #n e t Lo t v, St ir l*) min u t e s o r l o n g er t o d is s o l v e . 97 350 167 4 350 % -35-0* .. 350. Mi sc, 3 Df* 6. We ig h an d h o l d a t v a t 302 f o r s t e p 15 7. Te s t d is z o v a t an d r ec o r d : BY , mu s t be +. 8. Wh en s t e p 5 s t ir r in g c o mp l e t e d , t a k e 8 oz s a mpl e f o r ANALYSIS. 9. St o p a g it a t o r . 10, Ch e c k an d r ec o r d s ", II. De l iv e r s a mpl e t o l a b o r a t o r y . 163 82 163 ) 302 12. Ru n 9" Oo Bg .) w at er in t o v at 302. 5 13. We ig h in d r u m an d po u r in M 14. Tu r n o n a g it a t o r an d St e a m. I1). Ad d in 3-10 min u t es N-82 w eig h ed in s t e p 6. 16. Heat t o I30-IW4F, 17. St ir 10 min u t e s o r l o n g er t o d is s o l v e . 4 c.v. 6 ~l8. In s t a l l c h a r t in t e mp e r a t u r e r ec o r d er o n c o u p l in g v a t . 19. Ru n v a t 302 in t o c o u p l in g v a t . 20, Ad j u s t t o "(92%) at 6ft-70F. 21. Wh en u s in g v a t 207 o h 213. s e t a g it a t o r a t 20 RPM. W____ _ ii___I 1 ' Mi'-. -57-- + Re p o r t t o Gr o u p Su p e r v is o r f o r c a l c u l a t io n s bas ed o n an al y t ic al r es u l t s. __ Ga Lo x #/Ga l = : I&1-350 D.V. 7 22. Ad j u s t f r om d iazo v at bas ed o n an al y t ic al r es u l t s #n e t Lo t OR REMOVING GALLONS. by ad d in g 4 23. We ig h , ->is s o l v e in 30 g a l l o n s w at er in d r u m, a n d h o l d AT DIAZO VAT FOR STEP 27 2ft. We ig h im d r u m an d h o l d a t d ia z o v a t f o r s t e p 29 MT 4 25. We ig h s l u r r y w it h 30 g a l l o n s h o t w at er im d r u m. AND HOLD AT COUPLING VAT FOR STEP 33 60 ft5 0 IT or _5___ 28 60 7 39 , ft5 , / .. c o nt inued o n pag e z. DUP050067079 34 ........ VAT Pag e: 2 * Co d e:3^RL-582"DLb s : EST 3BHS In s t r u c t io n s : >s ' 1090 . . USE LBS. NCODE ACCT. LBS. D.V. 26. Ad j u s t *1410 vtT to at 2o-32*F, 57 * $00 9 27. PaUR IN H-fi PREPARES IN STEP 23. 2$. St ir 2-3 mimu t e s * V *. 29. P-UR OH M-28 VEiGHEB IN STEP 24. TO. St ir 10-15 min u t es ma in t a in in g + Kl t e s t . ............ Rec o r d s Kl t e s t ' T ' "* ' MlSC. 31. WEIGH. DISSOLVE IN 30 GALLONS HOT NATES IN BRUM, AND 10 KOLB AT COUPLING VAT FOR STEP 51 66 3 66 \ D.V, 32..Ch ec k b ia z v a t an d r ec o r d : II n o r ma l *(5558) c.v, 33. Po u r in t o c o u p l in g v a t N-39 pr epar es in s t e p 25. 12 36. Co u pl e o ia zo v a t in t o c o u p l in g v a t a t 64-70F u mber THE SURFACE TNR0U6H THE BlSTRIBUTOR IN 18-22 MINUTES. MAINTAIN COUPLING VAT AT 64-70T THROUGHOUT COUPLING. 35. St ir 20 min u t e s . "W 13 36. Ru n 15" f270S.) w at er in t o v a t 37. Tu r k o n a g it a t o r an b s t e a m. 38. We ig h an d bu mp in 39. Ad j u s t t o 184-1l8"F. 40. STIR TO DISSOLVE, 321. 354 336 354 .... \4lT Wh en s t e p 35 s t ir r in g c o mp l e t e s , t e s t c o u p l in g - v a t a n b 14 Rec o r d : Dia To . mu s t b e . 42. Tpst an b aEc o RB: BON , MUST BE +. 49. Test ANB REcoRfit pH NORMAL 5f>"7*Q* 45. Hc at to ll4-ll8F in 8-12 MINUTES. 45.' St r ik e v a t 321 in t o c o u pl in g v a t o n t h e s u r f a c e in 5-8 min u t es " 46. St ir 1-2 min u t e s . 47. Te s t an b r ec o r n : pH . NORMAL 3*5-4.8. 302 48. Ru n II" (1326.) w at er t o v at 302 . 5 49. We ig h in br u m an d po u r in M, 50. STIR 1-2 MINUTES. i 7 ___50 IX 51. Po u r in t o c o u pl in g VAT K-3 PREPARES IN STEP 31. 52. Ru n v a t 302 in t o c o u p l in g v a t in 5-8 min u t e s . 53. St ir 1-2 min u t e s . $4. Te s t an b r ec o r d : pH , n o r mal 8.4-8.7.__ ___ 55. h eat t o l79-lj3F in 10-12 MINUTES. 56. Ch e c k an d r ec o r d a c c u r a c y o f r e c o r d e r . Low: t h er mo met er #F Rec o r d er F. Hig h : t h e r mo me t e r 'F Rec o r d er T. 57. St ir 30 min u t es at I79-Io 3*F. ""W 58. Ru m Htf (tlBI) WATER INTO VAT 321* IT 59. We ig h an b s if t .in v )\ ' - e.v , 60. Wh en s t e p 57 s t ir r in g c o mp l e t e d , r u m v a t 321 In t o 18 COUPLING VAT. 61. St ir 30 min u t e s . 529 isr 5i9 DUP050067080 VAT Pag e: ^ Co d e ,gfig.p Lb s : In s t r u c t io n s ' USE LBS. N- COPE ACCT. LBS. Dr u m *9 62. In s t a l l Hi Speeo "Lig h t n in " mix e r in d r u m. 3863. Ru n c a l l o u s w a t er in t o d r u m. 64. Hzat ^o 70-90"f fF>- k:?QH IN PAIL AND POUR IN 66. We i OR IN PAIL AND POUR IN 67. WEIGH IN PAIL AND POUR IN M 68. St ir '*5 min u t e s t o s mo o t h e mu l s io n . c.v. 6<J. Wh en s t e p 6l s t ir r in g c o mpl et ed po u r e mu l s io n 20 PREPARED IN STEPS 62-68 INTO COUPLING VAT. 70. St ir 30 min u t e s . .71 Pr es s w it h a g it a t io n . V 2# % "64c 51 "641 2 7 3.6 m m 311 315 323 6a u 2 W 9" it" 6" 0" 215 - gjji? gp? 33M |4" TP 452 -- ^ gr5 24* 37" 16" [6* 555 206 207 213 Ga l . 20 13" 13* 52 13" 925 TIME START ....... if IT....* - 1 ! ' "' -- fi TIME f iw II n If ' n '' OPTR IZ ' '1 P -------------------- " ' ' `1' : .. . . DUP050067081