Document 0gEjbjmqDv9xKxbZzwzbnrBJV

I. I. PU PONT PE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 25$ YANDERPOOL STREET NEWARK. NEW JERSEY Serial No. Copy No. K*-5fr-U / NEWARK PLANT PIGMENT COLOR RESEARCH REPORT IYq &iw k s Tteport 0 warn iy w^rtaiitB h mb b s in Poriod Covered ***. 1953 to JmSXOC, 2954 FILE, DATE, SM/Sk NJ 44ST Oofff lot iH - Nuaerioal file 2 - Retearofa File (223*4) 3 - Librwy File (223.4) 4 - B* P. Elenka, Jr., Newport 5 - j* S Tully/A. Siejel, Newark 6 - M. A* Perkins* Jackson Lab. 7 - W* J. 0La, Cbaafcere Works 8 - #U Buildini File 9 * J. B* Cooper 10 - P. J. Hbnahan (For X) U * mm 12 - Extra Serial So. KN-54~11 Cojy No. f NEWARK PLAN? PIGMENT COLOR RESEARCH REPORT TITLE* HP KILLING OF PHTHALOCIAHINE PIGMENTS III STUDIES IN PERIOD COVERED* JPSL, 1953 to JANUART, 1954 CHARGE* A-II-C-297, 298 80SKITTED BT* APPROVED BT* ASu-rv BATE SUBMITTED* 4/1/54 DATE ISSUED* 5/24/5$ DUP050069777 X* Introduotioa K# susaexy XXX# SteUst Statue IV. Description of Process jpA Eqtiipaenfc V. mental Hnmi| Ltbontoiy A. Agents B. tmbMSt With 0-diflhH,oynVaw##n# 0. Dry hotx v. borax sludge* sand 0. Bboogoditlta B. V. 0* colors VI. Plant Developamt A. Blue BT-352-P 9. Green GT-735-P VII. ChlorinoFr Blue VXXX# Experimental Detaile * Notebooks XX. Appendix A. BT-352-P Formula ^ '9^m 8. OT-735-P Formula A Operating Notes C. Beferenoes DUP050069778 -X- I* IHTRODUCTIQh It has toil! found possible to condition pbthalooyanine pipaents for pigmentary use by BP milling in water a mixture of tto pigiimnt, a finely di vided inorganic salt and a dispersing agent* Work carried out previously along these lines has been reported in Beaearch Report X8-53-12. XI* 3UHKART At present, tto Rework manufactured products of this process are two pastesi BT-352-P and GT-735-P, to^ch are later eomrerted to eeveral end products for sale, vise, BL-288-D, B^53-P, 8^358-0, WWIZ*P, GW-732-F, GP-74Q-D and 0W-749-P. The OT~735-P proosss ha* toon modified by the use of alkali-extraoted green erode sa a stinting material, and many of the difficulties recorded pre viously in the operation of this proems have been overcome thereby* Both the BT-352-P and GT-735-P prooeseee have been accepted by the Production Division. Formulae sad operating notes are included in the appendix of this report. III. PATOTCgfAIDS A patent application on aqueous HP ml],ling has been prepared and filed. (Case 1251ft, Ehrioh and Stratton, Serial Rubber 377*110, 8/3/53.) A patent application relating to the removal dispersing agent (sueh as HLancol), which is quite firmly bound to the pigment particle, by treatment with o-diohlorobenano, is under consideration. Research Reports KH-52-13 end KH-53-XSi describe the essential features of the prooess and the equipment used in considerable detail. Since there have been no major modifications in either process or ocpipnent, the description will not be' repeated in this report. On u iahoratonr seals, two nine were made with a leu cylindrical grinding agitator operating with relatively close cleaxunce within a cylindrical vessel. Xt hod been suggested that such a device might be more efficient in overall operation than a disc type agitator (ref* 1), and might to used in a Ctotlhhcus operation process, lie results obtained indicate that this type of mill i far lees efficient than the HP type as regards particle else reduction. Xt appears that a relatively lone reeidsnee 'period is reouired to acaaemlieh maximum reduction in particle else) consequently, this mill offers no advan tage over toe Cowles Dissolver. . v,y , . ,V.-1 v . M; DUP0S0069779 a- v* A* Pigpen Research Report 01-53-12 lists several dispersing agents used and evaluated for aqueous Iff1 Mllingand the work reported herein merely <mlirie previo---u-'--s--- observations regarding m Twaii in t .<u 3 . Qnlgr two new sere triLed* via* Atolene NR and Alrosa HK 1-66, neither of which appears 16 show any proedae Atolene HR Dexter^ettioal Corp. Alrosa ISC 1-66 Alrose Chemical Co. Type Completely sulfated special oleic acid fraction* Probably an imdmb substituted derivative of laurlo acid Various easbinatlans of BLsoool end Indulin XS-3 have been used with sons degree of success over other eoobinations of agents) but, in general* RLanool has been used most sldely in HP Billing* and with considerable success. It is currently specified ito both the BT**352P and OT-735-P processes. B. Although aqueous HF silling* as previously described* conditions phthalocyanine pigments for pigsenbary use in paste fbm, subsequent doling of these pastes does not lead to toners which are easily incorporated Into oil systems. The presence of the dispersing agent* which is quite firmly held on the eurfaoe of the pigment particle and cannot be removed by extensive wash* ing with water, apparently accounts for thU incompatibility with oil systems. It was discovered, in connection with the "green 25" process, (ref* 2) that electrolyte (A1C13) which could not readily be removed by washingwith water, could be displaced by o-diehlorobenzene and than be removed easily from the syetsm by filtration and washing with water* The ODCB could then be eli- sdnated by steam distillation. The success of this type of treatment in the removal of electrolyte led to the suggestion (ref* 3) that this technique be applicable to the problem of removing the dispersing agent from toner j pared by aqueous BP milling* * Experiments along these lines were carried out* and it was that Blanool (a condensation product of naphthalene sulfonic acid all could be removed with marked success f?hm the pigment by treating aftarvy of aqasous milled pigmentary QPC with ODCB and then steam distilling* Stoner thus obtained showed improved strength and intensity over an untreated product* and in the case of CPC Green, was equal in texture to GT-674-D SO 121* Intense and yellow* DUP050069780 3 laboratory grinds made to twit the efficiency of dry borax n* borax itrfiw iMieato that tho dry material la mere efficient as a sriadlna fttHtim than is tho sludge. However* itan sludge ia used la conjunction aith dry borax <4 parts eludge on a dry basis to 1 part trash dry borax)# tbs grinding effU oienoy is entirely adequate. Straml grliy^t ha** b**n iw&fr to thft labontoiy to coBqpfejrd f^y^y diiidid to bofiXa In nmitla tin results thov tha borax ndndi to tMi aora advantageous with raapaot to quality of flalahad product and easa of sepa~ ration of the pigment froa tha grinding osdi\a< Considerable success la tha oaa of aanl as a gHtt*^?g agont buy box achieved by Orehost at ilbehr'yi laboratory# D. Homogenisation The Kanton-Oaulln homoxenizer has been used successfully in ****** ***** Where deflooouL&tion baa been required. It was thought that this device night be useful in the production of a dry toner CPC; therefore* several laboratory experiments were carried out aa follows* High speed pulverised crude was HP silled* with no dlsperaina aaent present. The poressoabs obtained after removal of the borax and filtration was then homogenised in acetone* two passes through the hoaogenisor at 5000 pH, one minute recirculation on eaoh pass. Results of some promise strergtbwise and tinotorially ware obtained in the ease of CPC Blue; however* ouch a process does not appear economically attractive over present methods (ref* 44*15)* CPC Green did not exhibit the same response when no dispersing agent was preswat* Howovar, the addition of 5% Blanool to tbs HP grind yielded results cooparable to those obtained with the Blue* Both carbon tetrachloride and water proved to bo relatively poor media for home* genlsation* hf far* the best results were achieved with acetone. It won thought that perhaps homogenisation of HF or pebble milled presooake in a 50$ Blanool solution might yield dry color* which would be>aeily dispersed in water* Several experiments of tide type were carried out, but no results of promise wore obtained* The addition of a wetting agent (Triton X-1Q0) did not improve tbe results to any marked degree* The Production Division assumed responsibility for tho operation of this process on tferoh 2, 1953 (rUtf* 6), DUP050069781 -4 * 8* A campaign was initiated in September, 1954 at the request of Quality Control, in an effort to disprove the quality of this paste. Extremely poor grinding efficiently use apparent as evidenced by the pressase of a percentage of grit or hard aggregates in the final presscake which led to poor quality of the end products mads from this code) especially (W-749-P, designed speoifioally for mass pigmentation of vieeose. It ess quits obvious that some means of Sit* oressing the grinding efficiency had to be found. An inspection of the overail process indicated that several factors mere contributing to poor grinding efficiency resulting in lack of strength and quality of thia paste) vis., severe caking of the charge on the inner nail of the Coulee Dissolver, the two hour griiidiigg Cycle eaolosed mas not enough. the amount of dieDerains ament was insufficient and finally the CPC crude itself mbs exceedingly hard. It was felt that if some improvement could be effected in each of these factors, the product itself would show improved quality. In Research Report KN-53-12 (p. 12-13) it is indicated that considerable difficulty was encountered in preventing rise in temperature of the grinding mixture in the Cowles Dissolver and that caking of the charge on the inker wail of the vessel accompanied this temperature rise. Further investigation of thia problem showed that caking began at a temperature of 60*0., which is the transition tarn# perature of borax (the dscahydrate) to the pentahydrate. It was felt that, if the temperature of the grinding mixture could be hpld below this point, caking would be largely prevented, nth this in mind, an inspection the c^5c^Hbg jswiJcotf of the Cowles Dissolver was made, and it was found that a considerable amount of rust was present inside the jacket. This scotssulstion of rust was sufficient to reduce the heat transfer capacity of the cooling system, thus permitting a build-up of the temperature of the charge. It was recommended that the jacket be given a thorough cleaning and flushing* After this was done, a masked improvement in heat transfer was obtained. Subsequent charges run In the Ccwles Dissolver then shelled almost complete freedom from caking. Heat transfer calculations, however, indicate that the efficiency of the present cooling system on the Cowfl.es Unit is borderline. Future units of this type should be equipped with more efficient cooling jackets and the present unit should' be cleaned and flushed periodically for most efficient operation (ref. 7). The grinding cycle was Increased from two to throe hours, after particle else index measurements indioatsd that this was necessary for maxiem reduotign of particle else, nth increased reduction of particle else sad therefore increased surface ares presented, it was neosssaiy to ins***** the amount of dlmpmmlhg agent, Hlanool, from 10.0 to 12*5&> Finally the CPC crude itself was investigated, and it was found that an alkaline extraction prior to HF milling was advantageous (ref. 8). The use of aiwitTM. extracted crude was introduced into the process and subsequent lets of GT-735-P showed great improvement qualitywiee. DUP050069782 5 A31 these modifications of process (ref. 9) led to improved quality of GT-735-P and the Production Division assumed responsibility for future operation of the prooess on January 15, 1954 (ref. 10). Efforts to produce, in the laboratory, a counterpart for BT-297-D tar aeneous milling the "EF" type of crude with Indulin XS-3# Bismol, ocublnatlona thereof, or with other agents, have all led to products much redder and duller than is desirable. Through X-ray diffraction analysis, it has been shown that there is phase conversion effected by this prooess from 100* p in the case of the starting crude to approximately 30g oL in the finished product. Such conversion is ttadselrahle sines redness of the produot is a function of the amount of a(~ phase present* The addition of ft. crystallising solvents to the milling charge has been to no avail, and indeed has led to inferior products, largely as a result of decreased grlMing efficiency, attributable to the formation of an emulsion of the crystallising solvent in water and to reaggregation of the pigment partiolee. Although Wettstein (Ciba) (ref. 11) has reported that the presence of water or water vapor favors tie formation of the o nn < the case of aoueoua milllturi the hr emish conversion operates is not fully understood. It is thought that water alonl, however, is not sufficient in Itself to cause this phase modification and that sons additional force must operate in conjunction with the water, l.e* mechanical action or heat, to bring about such phase conversion. Orehsm has reported that aqueous silling, using sand as a grinding medium, does not lead to the formation of the oc modification (ref. 12) HF milling, with no dispersing agent present, followed by homogenisation gave interesting results* but such a process does not appear at all aitimetiv*. Or far, the mostintfresting results to Mate have been obtained by BP Milling OP CPC crude in acetone. These results will be reported in a later SB report. THi. The studies reposted herein are recorded in notebooks 1455# 1# and 1471. A. 20, 39, 43# 54# 59 8, 12, 13, 16, 17, 12, 20# 21, 26, 27# 33, 46 fi - 1-19, 34. 35# 42, 43# 49# 53# 54# 60 - 7, 13# 14 - 9, 12, 14# 17, 23, 24, 25, 26, 28, 29, 30, |1, 2, |5, 36, 37, q. q<J. AO. Al. A2. At. A7. A8. 50. 52. 53. 60. C. Bias BG 1455 - 27, 28, 29, 30, 31# 32, 40, 41, 44# 46, 47# 48, 50, 51, 55# 56, 57 1471 - 1, 2, 4, 5, 10, 15, 16, 34, 44, 45# 55, 56 DUP050069783 O BJ 4 BI-352-P Formula and Operating Notes GT-735-P teterxmss. rax (binding of CPC. (Letteri C, H. meter to J. 5. Tully, November 28, 1952) 2* "Green 25** Process and related experiments. (Notebook 1454, P. F. Bhrioh) 3. Application of "Creed 25" (GDCB) treatment to HP milled material. (Interoffice Cksasonloationi J. H. Cooper to V. J. McNally, Hay i, 1953) 4. Finishing CPC Crude by HP milling pin* homogenization. (Letter! V. 4. McNally to E. F. Klenke, September 2, 1953) 5. Cost An&lyeie, homogenised HF milled CPC crude. (Letter! I. F. Henke to J. H. Cooper, September 15, 6. AestBqptiim of operating responsibility - BT-352-P process. (Letter! H. Arnoul to J. H. Cooper, March 2, 1953) 7. Coirlea Halt, Heat transfer. (Letter! W.J. MoNally/O.J.C. Klein to R.B. Morton, November IS, 1953) 8. Rotating Drier Crude (keen Dispersion * Research Suggestion #612. (Letter! F. F. Ehrioh to J. H. Cooper, Septt.lt>er 4, 1953) 9, Suggestions for Ispwved Quality GT-735-P. (Letter! W. J. McNally to R. A. Hageaan, December 15, 1953) 10. Assumption of operating responsibility - Qt-735**P process. (Lstten H. Arnonl to W. J. McNally, January 15, 1954* 11. Patents - Wettetein (Ciba) French 1,035,730 German 844,757 French 1,042,424 German 84k,301 BHtish 485,582 British 487,387 12. Minutes * Orchen/Pigment Department fleeting (p. 7) November, 1953. DUP050069784 VAT MISC. 1 w iviWtfi: CODE:.-. . ........ ...... ic.s. CD). BT-352-P 'APPROVED m- GOAL:..... 600# ....... _ SIZE ......... RAH: 5-25-53 DISZO VAT: RBM: 6-9-53 COUPLING VAT:.............................. r t o k o ?: vav- COWLES DISSOLVER Std Hrs. KOH-BLEEDING NAME; "KONASTRAL" BLUE PASTE/C*G. 20 IMSTRUCTIOJ USE IBS. MCODE ac ct . IBS. 1. Weigh and hold at Cowles Dissolver for 3tep 8 12 m fl. sleigh borax sludge from previous charge in classified. Do pot dip out liquid on top of Borax.* Record # Sludge in table step 33. 3. Calculate and weigh Borax. K-73A to be added in step 11. 22k. 600#- (Borax Sludge welshed in step 2 X 62Tc# X 100 H-71L* Record in table step 33. L. Calculate and weigh water to be added In step 10. 290#- (#Borax Bludge~weighed in step 2 X 38 )= #water ___________________________________( 100 _______ . .5. Shovel N-73A sludge weighed., in. step. 2__into,,Gowles, X, maliof-MsfesrJLn_3&isi, step 1. RecoM_soiurd3._.ln 10. Damp in five 25# bass of N-735. Be sure that all material from each bag Is completely mixed in before the next baa is added. During addition of N-735 add water from step L as needed to maintain vigorous agitation when all pigment has been added,popr in,the, remainder of the water from step k. Record: # and . Lpt Noa. in table step 33..----- -------------------------- _ 11 Dump in all except 100# K-734 weighed in step 3. 12. Stir 30 minutes. ___________ . 13. Add 100# Borax. N-73A held out'in step 11 1L. Stir i-l/2 hours as follows. _________________ ____ (A) While stirring it is permissible to add water (no-- more than 1 gal.' at a time) as needed to maintain good mixing._________ (B) Record power In.tab.le bjjlow,.. fC) If power exceeds 35 amps, add 1 gallon water at a time to reduce power to 33 amps; if under 25 amps add Borax to raise it to 25 amps ? bl> If cake is formed on inside of Cowles scrape down to insure good mixing and good heat transfer urns' Total IMbU Amps Amps' 15 rIPS Started Minutes 1/2 Hr. 1 Hr. 1-1/A Hrs. l-l?2Hrs. 1st Charge 2nd " 3rd Ath ML 'g. 2Hrs. DUP050069785 fit ClSsSlER 3 2 XMM: (B) BT~352~P 600# ............................................ L,,,,. L^jyk-JSiajE^^--------- 1___ Uik~j*i&s3J^SM^^ j45U. BspJufc^ ..--........ -........ M ^m%. 2B* 4 :,.(, | 2f- | J|iQlt j *"* | OODRI JOBS. f l1 | CLASSIFIER 4 1,20*,,.............................................................. ........................................ mtmms.*.4 :.3#1tM.:!i^t.t!te ... | ....................... 1 t 21* liitot of ,3*5 4.?0 s^34-P^ .'.'--. . . . . .'/ '.-i'^^^^:.' - ...'.-'.' '.v,.~.- V ..' .ivv.v.' ^'.VL.; . . ... yyt.v.;.;r<.: '.yyrjyyyy.yy.y .yy.yyyy-.y..yyyyyyyyy.yyyv.y-.yyy.vy.. .......... ............................................................................. alwjig9,,..s^^ U3kJfta&JIJ8l4^^ fjfc*... .............................................................................................................. ,.. | 11 ...... . > < COWLES DISSOLVES 5 css*. ihsBMStoLJAjrtstote^ ,. to Cowlaa Dissolver* GMWM* M..wh..Mftr..im,<as8i..I, .,,, ...of. ytesak* ..............1 yyyy.^^y^^y -- . yy^y^^^^yyy'y^yff-y: -- y-- ij&u. JEga^fitegt. .Xrsm ------V.y . , yyyy--y'yyyy-- y.yyyy -yyy yy yyyyy yy -->^>4. --------------------------- X-** --k~~ VAT 20 A..--..... MXSC* 7 j30*L................... ................._ ..... I-........... :...... ygUZJiassC^ ,,.j a&JUU . "v aFl o 8 MISC. 9 ^SMMSSsZ 4j b MISC. 10 i&stsi DUP050069786 tm VAT 17 11 VAT 9 12 DRUM 13 j E 3 ' OOSB:<B) BT352P t3S*^J5m4*L^ JjfifcJBsBiEjiaJfcgJ^ v95 /AAj K 6m moiBUKA*** '$ '5`W | $?* if i.WO*U USDMAgX IfcaCMPBi m *-;.v^*.. JL i '1 r WrK'lW LUdu.............4a .M.,,5b.___________ __ __,.,,,.____ u ^j p o ie j ^ I 43. Test and record: pH . nonmi l>0-2.0. ^.jpi,.1.0-2*Q...Mt^..,l527*,..... , I Record pH 44. Heat to 195~20Q ,,F In Q-10 ndmites. I II U4U~JteJ^JZJOZ5s&0&L^^... i-..-JL... 1,46s,...,StirJ0.M^.......... I I! L4Z^,te ........... .... ,,,,, <ff is-MHWWpKWNtt IA9^.M I r... ,.. :5 :|1 3 |i <r I WM'i h'-S'y^i-rw t) MW Kimt oortttwW DUP050069787 "Mwsastral" Blue Pul}. /C.G. 20 DUP050069788 DRUM LOADING 1. Install nXdghtninT> Mixer in full drum* 2. Stir to sake uniform. 3* Adjust to pH 7*Q~9*0 with N-742 solution prepared in Making Area.. 4* Take 8 oz. sample for dry content* DUP050069789 \-f Stf ^,,,^,^r,.,^,,x.. f;fe? 30?.-?.;?1;-; % Mc -j iim H*]$ i$insm ?*tm w^m-, f t ?#;? 6^6 111: # 600 * I . x &?) ** II -?3^ i ' ''.j o o j $*** 3-. 3 W%*w WUViAte* > iT&Is 2 i.r. mm 0i#**US fW fOv &$ #.*wis$ ?# t a^U m fTii3 3D, I, <hw* *rr trio f *k #f i:4t i^is r^ 5, *jf 0'.>.>* m**W9 Tf? I sS `4',-i- r s-mi at si* '\f m-& paw * r**?# sv*.. 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OREM cut** true* rskp VM.m *m M&m mi 20 . >* 00 M9T -WS# *m Stig fit YAt 20* vis "22. 0IOEP4.VSR 86. tfE8 ITS* i2 COMMUTne* &m 5|0 f#.fl8 10 Crntt 0iSO#IH.VSRj CAUTJ0.MS TO MPCR W*gte mjX tk-ms. mmm i# ** o v er eo o e or t *m*. ,Stor mn&'t-m* turn off cooutte mtea, Po mr cM^tt Y*wt Cwuts 0i.i,tsm to Va t 20 #*wr$#* CM?lU0.ygiY MSTM 4*ER mu,z pmJl0* Ma s h u Y Co w l es Di.eLV* rum# et wr mm* t o Va t 20, "Va t '20 5 27. A*UT VAT 20 TS 30M350&4. MOStS Do MOT fF A'tfT9R. 28, ftereAT $rem f-27 vatu. 5 c&mm& a m Va t IQ. m ?AY 10 "' 6 #tc. ? 29* Piih f v at 10 t Vat 9. 30, f MATEO tAA T.Wj 1s t . Csss 3ml " km. 5t. TrOOTAAS i,,B4 >, ## # `# ## # i. #. # # #. LOT S., # # # .# # # NOTEt ooRnm owi,e9 tin am #r mmi HAROS RERF0RM f0i.l.S3: TSEAWEHT m S0iOR IN Va t 9, Pr e,' 8 31- W.B.IOH AMO HOLD AT VAT $ PR STEP 39. I4___________ _ ME I OH ANO MOjUP AT VAT FOR STEP 35 33* VfSIOH AMP MOt.0 At VAT if FOR STEP- M COMT JHUSe ON TM 3 27 50 3^5 I * 290. 50 so DUP050069791 3 ml r*TSW> 6o q ? i | 3^* Ryu 'SBn C850} v a t e s nm v a t 17* ^ 35. >UMJ IN M-365 V&!Oftg$ i K OW 32* 336. Po8 IN ii-fcf ViN)> $* NTSE* * 37* Meat ?o 115*F - io5*F # mu t o comets sotat son, ''jT* 38* 0. 39* 40. 4|. 42, 43. 44, 45. Smiit ANITATOft IN V*? 9* Pyy** mrs *** 9 N~27 v!* m s t e p 3*> T**t AMO ccft; rn^................ .StoaiNW. 1,G~20* fr NECESSARY AJ#)f"10 W J*8-%.0 XMTM N-&7* HEAT to f95*-200*F 'IN 8-fv) NiNUTES < Ru n Va* 17 At ?75'f80'T ir v at 9 At ?95BF - SOOT, IN 3*3 MtNV?S. St ir 30 tumms* At !'0-EOO cf, l*RE9'vttN WWIOH* mmnsm c j -mh t o p n e s s b o o m* *7 J \ ..."-'J - -'' * > :: ** DUP050069792 "MONASTRAl'1 GREEN (o) OT-B5-P PASTE /c.G. JB &0# -RAH: MH-54 IfeHs f/iS/54 9-?o s l o g {? 3000 % !N 5 DRUMS, Wear Svst.eau F,oa am cosatiRt. Costae*. imwMem f DUP050069793 (D) GT-735*?P StHi mm The (D) GT-735-P process replaces the previous (C) GT-735-P process and differs from it as follows? 1. The amount of dispersing agent, Blaneoi, B-56?, has been increased from 12# to 15#. To compensate for this added amount of agent, the diphenyl guaMdiaa, N-365, has been increased from 40# to 50#. 2. The gLancol, N-567, is put in solution in the supernatant liquor from the Borax sludge, instead of being added directly to the Cowles Dissolver* 3. Since the supernatant liquor is therefore added to the Cowles rather than being poured into the classifier, the percentage of Borax In the sludge is calculated to be 62# rather than 72#. 4* Alkali-extracted !mastraln Green G Crude, 33-770, is used instead of flJkiaastralw Green G Crude, H-736. 5. The silling cycle has been increased from two to three hours to insure adequate milling. 6. The power input is regulated between 28-30 amperes . 7. The rate of flow through the classifier has been reduced slightly, from 35~4*0 to 3.0-3.5 gallons per minute. 8. The presscake is stored on the acid side until used, rather than being adjusted to an alkaline pH.1 2 1. Classifier - The rate of flow through the classifier has been reduced slightly in order to avoid as much as possible any carry-over into Vat 10 of large particle size aggregates and excessive amounts of Borax* 2. Cowles MU - The power input mast be rigidly controlled between the stated limits of maximum operating efficiency* When the power input exceeds 30 amperes, the temperature of the grind tends to increase rapidly. At a temperature of approximately 130-135f * caking results. Formation of the Borax cake on the walls of the Dissolver tends to reduce the heat transfer of the cooling jacket. It is believed that this caking is a result of the partial transition of Borax from the decahydrate to the pentabydrate. It has been recommended that the cooling jacket be cleaned periodically and that future Cowles Dissolver units he equipped with modified and more efficient cooling systems. 3* Milling Cycle - Development studies indicate that a 3-hour cycle seems to be necessary to achieve minimum particle size and to realize maximum possible strength of the product . It may be possible, however, to reduce this cycle to 2-1/2 or 2 hours when further data concerning the behavior of Alkali-Extracted Green Crude, H-770, is compiled, and still achieve a product which is entirely acceptable strength-vise. DUP050069794 2- Throughout the grinding cycle it is important that a good vortex and good circulation of the charge be maintained* 4* Imaredienta - Fresh Borax, when used or added, must be relatively free of hard Imps* This Borax is to be added as rapidly as possible to gain the proper power input and still not impair good circulation of the charge* Alkali-Extracted Green Crude, N-770, responds very favorably to aqueousndlling and leads to a marked reduction in the amount of unground pigment in the final product and in the classified sludge* Xt is recommended that only this type of Green Crude be used in the future* 5. Borax Sludge ~ When using the non AltealirBxtracted Green G Crude, N-736, it was found that the Borax sludge could not be reused effectively. This was due to the relatively large amount of grit in the aonrextracted crude, which tended to accumulate in the sludge. For this reason, only fresh, dry Borax appeared to give the desired particle size reduction and strength* however, excellent results have been achieved by grinding Alksili-Exbracted Green Crude, M-77Q, with sludge borax obtained from previous grinds of this type of crude* This sludge appears relatively grit-free oven after being used several times* Xt is recommended that whenever Borax sludge is dried for re-use, the drying be carried out at a temperature nohigfaar than 120F. Higher temperatures may result in the transition of the Borax from the decahydrate to the pen&a* hydrate* 6* Presscake Adjustment - Adjustment of the final presscake to the alkaline side appears to be detrimental strength-wisej therefore, it has been decided to hold this presscake on the acid side. Signed: Approved: bl 8*. A* Hassamaa - 1/14/5 DUP050069795 / DUPONT NEWARK JMCM'TJTS -S?FPAKmDfr MAY 25 1954 COLOR RESEARCH LIBRARY