Document qmw9EKrR1QEX2LYzg1Y3X01VR

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 YANDERPOOL STREET NEWARK, NEW JERSEY Serial No, KH-51-2 Copy No. 4 COUPIDBHTIAL NEWARK PLANT PIGMENT COLOR RESEARCH Efrogaresa Rspo^fc REPORT po l y mer g - Fteama? n rnOoSsO s e mi-w o r k s md ?um mmawm ----------- gCTO'gH--------- DECEMBER 8* 1940 Period Covered DECEMBER 31, 1950 FILE: DATE: BIO 15, 1951 NJ 3707 Copy to* #1 Nusssrioal File 2 - Research Office (210 3 * Library File (210 4 - V. Clmicjpsidt f- %rZk. Serial Ho, KSf-51-S Copy So* l ZJULMJJUULU^ fflEBTAWy HAHtP PIGSGSOT COLOR RESEARCH REPORT Progpeas Report POXgHBR K - PJ] I-glk&g DECEMBER 8, 1049 - DECEMBER 31, 1980 Charge* A-IIC-2S8 APPROVED BJ * B* H* PERKINS BATE ISSUED* 1-18-31 DUP050068463 saraag. Introduction SmsBipy ftfjp Patent Situation QmimmI laboratory Forwalaa Newark laboratory Study OavaXojxmt of Standard Processes Hgaant Variable Studios Flushing Variable Studios Testing Physical Instability r Qpift Physical Studios Chemical Qoaspcsltioa Vielda Sesoansnadations fee? Future Study daferenees AA-8HP Forarala and Botes AAS*F Foreulumd Botes X X X 1 1 8 Z 4 8 4 6 7 7 8 8 8 DUP050068464 IWCTJCTIDBs This report &wmmvlz& study conducted at the request of the Finishes Division of F J F directed toward the development of plant processes for manufacturing Hydrous Nickel (II) Oxide and flushing it in alkyd resin* Tbs product was designated as 9Pigment IT* throughout the study* It has subsequently been designated as ''Polyiaar K* by F and F* In m extension of earlier work on the fortification of lacquer and alkyd films by hydrous Iron oxide,, F, and F* found Pigment n (hydrous nickel (II) oxide) to b tho nost offactive and generally desirable of the several oxides studied* not only from the viewpoint of film fortification alone* but also because the extreme transparency and optical clarity of Pigment U permits attainment of novel tine* torlal effects hitherto unapproachable in finishes of acceptable durabilityo mmELmjmsmxm* The Pigments Department Chemical Division was requested to develop practical plant processes for the manufacture and alkyd flushing of Pigaeub N* based on laboratory formulas supplied bar Fand F0 The development program has culminated temporarily with initial plant manufacture and determination of manufacturing oosts The plant product was equal in clarity md durability to semi-werke products* #iich were* in turn* reportedly superlea* to the laboratory products which had aroused P and F 's original interest in the development* Process standardisation remains to be completed and i con tingent upon authorisation of further production,, Guidance for the future program has been provided in the standard manufacturing form ulas and notes included in this report* Previously specified modifications in existing plant flushing facilities are prerequisite to routine manufacture of flushed products* PATENT SITUATION* Patent aspects of the development and application of Pigment H are under the jurisdiction of F and F* Bona of the operations involved in Newark prosessing appear patentable per sso >tes~ This section supplements the standard formal* notes which Ended in this report* mi which contain all major conclusions de rivable from the development study* Use fcrmala originally recommended in F* and F*s Philadelphia Laboratory Memo Report M-273 (Ncv* 15* 1940) specified reaction of nickel sulfate with sodium hydroxide* washing by repeated filtration DUP050068465 -s-. and doeantutioia* and flushing inti EG"448 alkyd at P/B 1/2 2b report Indicated that the major portion of fchclr work bad involved precipitation of the hydrous oxide from nickel chloride rather, then from the sulfate, hut that they had encountered serious difficulties in washing the precipitate sufficiently chloride free to avoid blistering on exposure and were recommending the use of nickel sul fate because they considered sulfate ions to be less destructive in paint films than chloride ions* (Informal advice from P. & F per sonnel indicates that the latter viewpoint has been reversed by the results of recent independent study Involving systems in whloh cor rosion is not a controlling factor*) Xn a supplemental report dated Bec 14, 1948, Philadelphia Laboratory retracted the sulfate recommendation because of inferior optical clarity nod specified the use of nickel chloride for optissue clarity. as well as a mximm Unit of 0g% ox on the pigment solids basic for satisfactory Mistering resistance Their proposed wash ing cycle involved four decantations* filtering and roslurrying, followed by two decantations and ultimate filtration As related below, it. was later established during the Reverie development study that adequate salt reis&vsl far standard blisterrreslwtamae can be obtained by a one-cycle wash-pross operation, and that the aotual tolerable Cl oontent Is semeWhat greater than ten tines the Unit specified above, the major portion of the discrepancy in specifi cation Units being due to inadequacy (iaeemplefc extraction) of the analytical method on #*ich the initial specification was based A final laboratory formula revision. transnitted informally by F and F on Jan* 11, .1060 (tiewaxfe H.B. X8S1-17), substituted 80-3078 resin solution for *W% of the initially specified RG-448* This cheng, initially made in the interest of increasing ultimate film hardness, appeared to Increase considerably the quantity of breakout water (and contained salt) dining flushing, and also appears independently to have contributed importantly to the excellent opti cal clarity of semi-works and plant flushed products r 82G33f Preliminary laboratory series were run, using niekel sulfate as initially specified, to develop familiarity with the precipitation process and to investigate possible variables for accelerating suit removal either by decantation or by frees-washing* 2be limited quantity of products Obtained precluded flushing by orthodox: vacuum mixer procedures* Attempts to apply micro-flushing technique# were partially successful but the recognised uncertainty as to signifi cance of results obtained from sum tests prompted the decision to conduct the major portion of the development study at semi-works batch else* One promising result indicated the possibility of aeoelerating filtration by heat treatment of the slurry, but attempts to confirm this in the semi-works were unsuccessful. DUP05006S466 A pilot semi-works batch (lob 1143 and splits) was struck from nickel ohloria following receipt of revised specifications fpcm Philadelphia Laboratory, and experimentally processed with, tbs following results* (a) The pressing and pres a-washlag characteristica of tha slurry were similar to those of iron blues (perhaps intermediate between B-300-D and B~63-D), sad definitely better then those of owe wore difficultly processed products such as Pigment Green B (b) Excessive press-washing did not attain the 0,2$ maximum Cl limit specified by F, and F, Aotu&l analysts of tbs washed pigment indicated 01 oontent to be 2,8p (o) Beat treatment of a portion of the slurry produced no inprovessent in processing characteristics, (d) Bsemfeatiam washing* attempted on a portion of the slurry, appeared to be completely impractical, (e) Attempts to farther decrease the salt content of the washed pressoSke (2*&$ Cl as Is) by rslurrying re sulted in pepttsation shlch precluded the possibility of subsequent filtration or decantation. Laboratory flushing of the press washed (2*5$ CX) pulp, at Phila delphia, produced mill base of excellent initial quality and it waa agreed to proceed promptly with the manufacture of three additional seal-works batches, each to be flushed at Sewark, with dewonstration of mutually satisfactory reproducibility and satisfactory blistering resistance by accelerated test to scree as sufficient basis far manu facture of a 600 lb, plant batch. Two additional semi-works batches (1160 and 1164) mere wade promptly and duplicate 2,5 gallon flushed will bases of each prepared at Hewark using the modified resin composition later incorporated in the standard AA-S-F formula* Pigment/fiC-548/RC-S07a m l*0/0.6/loS She pigment processing character!sties as well as the ehlenlde eontests of the new batches hooked those of lot 1X43, During the course of analytical work at Howark it was demonstrated that the analytical procedure previously employed at Philadelphia resulted in extraction of only approximately 10$ of the total chloride actually present in the semi-works products. The semi-works flushed products possessed excellent resistance to blistering in accelerated teste, and were sufficiently premising In general quality to Justify author isation of plant manufacture prior to completion of the full threebatch program. DUP050068467 One 600 lb* plant batoh of pigmsut w h o struck March 27, I960* A semi-works processed portion of the plant slurry was normal in presesalag characteristics* hut ahiomal washing wa* experienced In the plant, with unexpectedly early appearance of peptization bleed Whioh compelled termination of washing.. The Cl content of the plant pulp, however, was normal at 2,2$ on the solids* Upon opening the filter press It was obvious that the press burden was consider ably below options, the *oah* being abnormally quite fluids Correetive measures have been incorporated in the standard AA-2-P formula* Two plant batches of flushed base were manufactured* The processing of each batch was grisly complicated by unsuitability of heating facilities for the distillation cycle and various other diffienlties of relatively less serious character all of whloh have been discussed in the writer* s letter of 9-IX-SO to y* H* Bailey, "Flushing facilities - Building #12*" Further complications resulted, in the case of the first batch. Cron the abnormal fluidity of the plant pnesecake* These were corrected in a single semi-works flush ing by modification in aimer loading technique. The correction was satisfactorily confirmed in the seeded plant flushing, and the modi fied technique has been incorporated in the standard AA.-3-F process and discussed in the formula notes* Daspite the operational difficulties encountered, each of the flushed plant batches waa fundamentally satisfactory in initial properties and In durability. Ho final decision as to fixture manufacturing policy has been made to date* in the event that manufacture Is resumed at Hewarfc it will be necessary to effect recommended modifications in plant flushing facilities end complete the plant standardisation study along the lines suggested in the AA-8-P and AA-5-P formula notes. Heating the slurry prior to filtration Clots 1144, 1169} has no beneficial effect on processing characteristics or yield, sad apparently is detrimental to quality in that flushed bases of such pigments are abnormally seedy (1351*27-28) As discussed under "Yields an indication was Obtained in the ease of lot 131 that significant improvement in yield may result from use of very mild agitation conditions during strike* This batch, however, was made for experimental use In Duoo subsequent to termination of active study at Hewark, and therefore was never eval uated in standard AA-5-P* The lead merits further investigation* An attempt was made to establish the maximum 01 tolerance limit of Pigment H, The available results (1351-62) Indicate that extremely superficial washing - to approx, 150 ohms (66j 01 cm nresseake solids, 2*3% 01 in resulting base after 6Sj water decant)is adequate insofar as Philadelphians practical Delaware exposure DUP050068468 blistering results ere ooncerusda A mors ant!das interpretation* however* suggests tentative specification of & wash mbs* effluent specific resistAm end point in tbs 1000-1500 ohms range* with 8 to 4$ Cl on tbs ju^ssoake eolids, or 1 to 3# Cl on the flushed mill bass pigment after breakout. Actually* indications bars boom observed that the ma&wm Cl tolerance may bo fixed on tin basis of optical clarity of the mill bass ratios* than on tbs basis of blister susceptibility. Th foregoing considerations confirm tbs vribor*e previous view* expressed la the AA-2-F formula motas * that incipient peptisation bleeding in the wash press effluent is an indication of adequate chloride renewal* Cm seal-works batch (1168} was struck from nickel sulfate rather than nickel chloride* using the standard stoichiometric quantity of caustic* end was washed to 4f SO4 on the solids* She mill bases prepared therefrom (1551-85-25) amply confirmed Hj IIa delphiasa prediction of substandard turbidity or ollklnecs. Baaed on an apparent laboratory lead, a seoend sulfate batch was made in the semi-works (1X81) using twice the stoichiometric quantityjof caustic* Sulfate analyses of the pulp (l.Sjf) end the base (S* after &?% breakout) are in conflict* unresolved to date* The resulting flushed mill base (1501*40) teas satisfactory in clarity although In ferior to normal chloride bases in dispersion characteristics Bo attest has been made to correct the dispersion characteristics* because accelerated blistering tests at XhiladeXphla indicated the sulfate mill base to he extremely poor* Subsequent Delaware exposure evaluation* however* has not eoaftrrned the accelerated test* but indicates the sulfate produet to be satisfactorily blister resistant on practical exposure, This reopens the desirability ef further study to oerrcct the dispersion deficiency end confirm the blister resistance in order to realise the significant potential ingredient eooneay which would result from the use of the sulfate pigment pro cess despite the increase in caustic* Specific surface determinations failed to differentiate significantly between the two sulfate pigments* or between sulfate and Chloride pigments,. FSPS5IBB VARIABLE ST51XBB8 The AA-8-F formula notes discuss the currently available known facts and plausible hypotheses concerning optimum flushing conditions* except for an attempt to establish a iwtxjman tolerable IfeO limit in the flushed base (1877*48), The results of this attempt indicate that satisfactory optical clarity and transparency aa Ob served through the mixer sight-glasses provide sufficient evidence of adequate water removal (to 8-1/8S6 or less* by toluene distill ationh Inastsuohas samples of base withdrawn while still opaque and milky (at 8.8JK cr greater BgO content) gelled very rapidly it Is desirable to review Philadelphia* complete evaluation of the 3877-48 mill bases prior to resumption of manufacture. A standard 2.5 gallon mixer process for A-3-p is given in 1851-56. and a process for flushing abnormally fluid A-8-P is recorded in 1381-57. Experience with the 2.5 gallon DUP050068469 xer has been mseh more satisfactory than that with the 0*99 gallon mixer* possibly because of less frequent use of the letter sad uwfamilianity of psreeunel with its distillation oh&raeteristies A very high Iml&mo of substandard dispersion properties resulted from attempts to use the small? wiser* At 1bhe request of Philadelphia Laboratory* normal palp was flashed Into Basils alone (1961-44) according to the formula origisally proposed* She product was extremely turbid (milky) compared to & control (1951-46) flushed in standard formula* M offset was duplicated with another lot of pigssnt in experiments 1951*48 and 46* Also at Philadelphia laboratory* a special request* a flushed base (1977-45) was prepared in vhioh 80*9079 was substituted for EC-0078,, The product appeared inferior to normal products in colorP dispersion and turbidity* The flushed product must be eewpletely free of ttmbidlty m mllkimess ifeen reduced to enamel composition* applied as a 5 nil clearsue film over black* and baked* This troperty has been desig nated "optical clarity59 in this report Xi is not to he confused with "opacity"? at least in certain restricted or specialised appli cations of the latter term* for example* m "opaeibomebey" designed for eouS^oXXed-vlew oomparieon of uniform films of slisaftna hydrate inks with nerioally graduated standard white films of increasing opacity was found to be completely useless in distinguishing between figment 8 enamels of widely different milklasssp A prescribed ^othod for conducting the enamel test Is given in the M-3-F formula notes* As also stated in Idas notes* however* the clarity of the mill base an always be accurately appraised by looking at a sample of the mill base in a glass Jar or on a bright spatula* The only certain test of AA-8-F presseeks quality available at present is a vaoWMW-wtwir flushing by the AA-3-P process* Attests to develop micro flushing rubout type tests have been completely nusncesasfisl* but it is suggested that a test involving change can mixing of preseeake and resin elution followed by evaporation trans fer using the back rolls* only, of a wans (120 - 140F) roller mill be investigated* when study is resumed*: mMSBLMmmmiAMm Figment B demonstrates the geaarioally eharacteristie ten dency of. hydrous oxides to undergo growth of particle else during aging of aqueous pressoak, with coasequsnt loss of transparency which eventually results in inability to produce satisfactory optical clarity of flushed mill bases* Th rate of this "drift9 has been tentatively established* as discussed in the AA-2-P formula notes* DUP050068470 to to sufficiently to forebode so difficulty is routine manufacture of fluahod M\s bases provi d& the too week ago limit specified in the A&-8-P and the AA-3-F formula i* rospeotedL So Information is available as to ago specifications for preparation of Dace bases; all investigation of the latter lias toes the exclusive responsibility of F* md F* Insofar as the optical end rheological stability of flushed bases is eim&ernsd* Philadelphia laboratory stated at toe beginning of the development steady that ao problem had been encountered up to that time* Horn has been reported si&soqumtXy* apeolfto surface measurements of dried pulp temples* as mall as the relative last of definition of X-ray diffraction patterns of aqueous presseekss,, indicate the wXtim&tft crystallite else of Mg- neut U to be in a rcag having .Qlx* as its maximum (RIM report 50-89)* Electron micrographs of flushed mil bases also support this eon- elusion* since all objects larger than the practical limit of resolution have the appearance of aggregates rather than of crystallites 9 In experimsmtal application* of very limited extent* none of these techniques distinguished between samples of satisfactory pig** went or mill base and samples having unsatisfactory optical clarity* #o further attempts were made to develop fundamental data relating optical properties to crystallite sine* because of the lack of readily available methods for precise sine measurement in the region of interest* X-ray scatter!Eg has been reeomsanded by Dr* Banks of the Bewerk Physics Group as the method most likely to be capable of development to a satisfactory applicable state if need for suck data arises* Direct evidence of crystallite growth during aging of aqueous pressoake was provided by s significant reduction in the quantity of resin required to effect transfer in the flushing preeess* Avail** able data* with estimated precision of + 5g or better* indicate that plant pigsemt had decreased in particle also by 88Jf after 8 months aging as presscake* and that a semi-wort* pigaemt had decreased by 88$ after 7 months aging (1877-58* 89} Pigment if is essentially SiO.HgO* Basic nickel salt* if present at all* ocmprlaes less then 0,,6$ of the weight of satlafaetcr; plgwemt precipitated from chloride* and approximately 1% of the weigh of unsatisfactorily milky pigment precipitated from sulfate by the stoichiometric caustic process* (General laboratory Analytical Report AA-2-P dated 4-12-SO), The e&pirio&l formula of standard quality semi-works pigment (1160) after toluene distillation followed by drying at 160*0 is 1*00 BiO. 1*08 HgO* Average Cl analyses corre spond to approxlmtsly 3 to 4g ffaCl* Analysis of the plant lot cheeks that of the semi-works products very closely* DUP050068471 Coat v*t .ffiwimMi 09 * IS Qcm 1--:-*bt TM WTO GOAL? fOW , ,, BVSBt. 'EM* mm ilD,' covftusa v m?s. Apppotrvd by* lOMs 5*^ t t i3P?h BTBIKB VAV s SAHBt -N**sy*a*.*h (sisa) std* s<w, tsmm IB OF HOMiassxro t**im**i*mi#t B com AOCf IBS* X. Bnn 15* (BOOC,) *atr Into vat .800 8a * Start AgltatCS?* 3 ttelgh dasip te 4 stir 10 Ijag@i* to dissolve MW sxo '.490 \ Bsea $* (4390*) w*t#r lato wfe 899* A* Strt agitator* ?* .tfaigb *d pow Ia % S.- 4da* t.0 $S* (9800.) *t ?0H8X*F* 313 *8 !;& fi'-SXO i coeplataly dissolved, adjoil .mvt 800 tc 2s8?e*s f(1inOruGn0C?&U>) a*t ?0X*F* 10* Test ml rm&ord* g>Hn........ r..,_, wwl 8*8HW2: Up strife Mj.s;t SSO aithcrat agitatim at 70H3O*F* Sato ?at 80S at 79HSX*F m Wm mm-tm in 83-08 admit ,8(Mddt Haw started? Seaord* Tet It* Stir S S 13 a Tost feqd rarnerd* Ilia I-rass agiiabim* Sfcsrm&i 103" XX*0 $Sm Start j?im sin,. HS jQpiBP, DUP050068472 ....................... ..................... _.r........ r_ HSOOESS g (k) A-8.-P . Z?M?E TOg 5*7-50 h ie s s w Am iMTmmtm Vofc t Mot ftet EslaasM Bfs .. VmB& Ho,* 3 ....., Ho,, of CzJm i *6 . . Bseas srlfc&oofe jftgifca&ioa HfesSt t g8400 Ctea H#; Ssat fcst JtJtfito tea# tm 4 tetaae ~ ises plaafcio ISmam Special t Ee^BXsodissg dote mh *et& All Wash msw. wbej? <110 ISO0?) Splas __ . .. . .. . . . ............ .. .. BoXiw to: ................. .... ... . DUP050068473 Cost Gronp " X4 w NAME: COiAe I M-pmomt) b t * ^iiUgdL, mUetezm g o a l * sie&f SIZE BSf* PROMOTE GOGFbXSG VAT^ STRIKE VAT*___ S8S2. HOH-Bigsanm ';W.SWW.'HUS il ftft 11 w WiiXWHBiMW------ PLUSSBB PIOKEHT H OSS XBS, ACC'I.IBS, bam PEHKBiS ttTVBB Xo Install rcoerdor chart la tessperatwo contraller* . Eo Set tomper&tnra controller at 10C S weigh and shovel Into 4* Start s&xsr with top raised., 8* Eua Sa from scale dram tfcroogh E* line la 18 minutes 6 Rm. in K*S94 from scale draw ibroagb 8* line no faster than 4 lbs. per wbnte* Watch wiser constantly, Stop B-894 udm water Is about to break onto Record 8-894 GenhUn* asixiBg vatlX water separates* T* Decant repeatedly nnbil all sepa rated water has been removed fro 808 6* Weigh and shovel into mixer 9,, Start wisero A Whoa water sheds* decant repeat edly ontil all separated water has been nawHrod* or B Xf Oharas In mixer becomes erably and does not shed water id.thin 18 minutes* slowly add 8-884 as In Step Q uafcil fcre&kout osenrso 0, Xf harge In mixer remains pasty and does not shed water within 6 wtssssfcea* cheek tmw ( ) stop mixero and proceed with Step 10 XOo Weigh and shovel Into wiser lx* Hepeat Step 9* Check A or B or C be! OW9 Aft ( ) water shed and oowpletely deantedo B* < } erisd&y after IS win* Added 8-894 to shed C ( } pasty after 8 ala* Bo shedding* xs Weigh and shovel Into wiser xs Repeat Step 9* Chech A or B or 0$ A, { ) water shed and completely decanteda B ( } emWbly after IS win* Added $-694 to shod C < ) pasty after 8 win* Bo A-g-B 380 90S 894 A-2-P 80 894 A-8HP A-2-? 80 css y&* -* DUP050068474 VAT PAGE* e COSE* A-3-F X*SSs TTT USE LBS CODE ACCT.IB8. 14o ttelgi and 3hovel into mixer* IS* Ropeat Stop 9* Check A os* B as? C? A ( ) water shad and completely decanted* B* ( } erujs&Xy after IS rain. Added 3-694 to shed C. { ) pasty after S raitu Ho shedding 10* Weigh, dad Shovel into mlsxsr 1 ,, Repeat Step 9. Steak A er B or 0* A. ( ) water shed and completely decanted 5 { ) crumbly after 10 min. Added B-894 to. shed c ( } pasty after 8 mi*u Ho shedding* IS* Close mixer 19 * Calculate total B-894 added In steps 0 thru 17* Record total lbs* Sid)- treat total from '900 IbsT^Tery slowly add the .required difference 000 through the 8* 11ms in 8-0 hours. Impoot charge closely md f^quesaisly. If lumps appear* atop B-694 at once tag til charge is again uniform* then rsswsb H-094 addition* Record time started and time finished* on temperature recorder charto 20* Very slowly add through the 8* lino 1? 1 hewn 308 Keep hatch luasp-feee .and uniform as in step 19* Hotes If necessary, the operation nay he shat down, at this point only* for 10 hours or less* If shutdown is desired* A* Stop mixer and scrape down aides* B Run in through the 2 line a one-half inch layer of B-090 onto the urfae< of the charge* G* Rook out drive motor until read? to proceed* 81* Open mixer and start mixing. 82 Weigh and pour in during 5 minutes 11 23o Drain distillate exhaust lines Behind mixer. 84. Open condenser spray valve 1-8 turn. 25o Close mixer and distillate drain valves. 26 * Start vacuum* 27. Set temperature controller at 50C. 28. Continue mixing under vacuum at 50C, until Charge becomes dark, green and semi-plastic. 29. Two hours after start of distillation start adding H-690 slowly through 2* flexible line* no faster than is required to prevent charge from becoming granular. (Cont*d on Page 5.) A-8-P 30 094 A-2-P 30 894 094 900 098 388 090 895 11 DUP050068475 PAGE? 3 CODE? A-3-F USE LBS, CODS SO, Fifteen minutes after fog disappears fro mixer eight glasses* tmreeae rate of H-890 addition as stash as possible without permitting charge to become Xmsspy* 31* Immediately reset regulator to 10*0* sad shut off heating steam* 32, Maintain vacuum while adding 9*690* 33* Continue adding 9*690 until total added in Steps 20 3 through 33 la approx* 2 1*2 drums 34. Shut off vacuum steam and condense spray* 35. Start cooling water in mixer jaetmt* 36. Stop and open mixer* 3*7. false two 4 os* samples for duplicate moisture and solids deteminatlono 38. Immediately run in 1/8* layer of 9*690 on top of charge and lock out drive motor* Becord 9*680* 38. Deliver samples taken In Step 3? to laboratory* 40. If moisture is o#g$g or lass* proceed* 41. Calculate 9*690 required to adjust film solids to standard 40$ value t (Actual solids % * 40%) *l*00 Factor x 2000 *(9*690 Sttep 9*390 to add. 42. 9hen ready to pack batch* start mixer and run in 9*690 calculated in step 41* 43. Six IP minutes* 44. Stop sixer* Pack out hatch immediately through screen into 13 gallon drums (9*645) at 130 lbs* net* 690 69 690 ACCT.LBS, 1158 DUP050068476 Wivz&Jl, A~3~F is a flushed *.DaXttx" dispersion of hydrous nickel {IS) oxidsj. designate! as topol'fmr JC-* by the F&? Bcpart&$nta It is manufactured et Kcwark, exclusively for JP&?.* fhe flashed fredact must Isa completely free of turbidity when reduced to engine 1 compo sition applied os a *003" clearance film over blse'k* aM baked, freparation of the anurous Pifaant H prcsscrls used In the flashing process is described in the {i}JU2~r formic and notes* Tfcfe appro::ls-.oto weight composition of the flushed bass product is*. A2~-P Pigment solids 300 lbs. a 13,33$ 8-693 EC-448 solias 150 lbs 6,&7$ 8-694 Re-3073 solids 450 lbs* a 20.00$ 1-690 Amsco B eoiventit1358. lbs, a &oiK3|L Total 2250 lbs, 1DD,0Q# Fifty percent of the &~2P is charged into the 250 gallon Baker-Farkins' vacuum miner* slowly treated with all of the EC-44S resist solution (H$33) cud than treated *i th EC-3078 res la solution (H-69-4) until tha oil-in- i?ater emulsion coagulates and reverses to water-is-oil, expelling breakout water which Is decanted The remaining half of the pigment presscake is added in five equal steps with breakout and decantation of water after each step. The re mainder of the BC~30?8 solution is than slowly added to the wry viscous paste in the mixer, followed by 55 gallons of Jaaseo A solvent tI-692) and 11 lbs* of trlatheuoXsaInc (~695) Besidual water is removed fro the batch by vacuum distillation, the anhydrous base is reduced to the desired solids content by addition of Aitseo B solvent (JM$90), and the product is screened into shipping containers* mm&m .Because of the instability of 1-2-P the strike and flushing schedules "must bs sc integrated that the presscake is never acre than one or two weeks old when flushed* mmuMmmMm 111 safety regulations applicable to the flushing area and to the handling of petroleum seluants must be strictly enforced, The most important tinctorial properties of Figment N are extremely low strength and high transparency. The most exacting "Son-Bleeding-* processing precautions must bo extended to prevent contamination with any foreign material* DUP050068477 Only plant batches hav- bam i.-ade to Baba Clots 10208 and 10271) 0 Dos-pits operational. 4 iff lenities during vacuum distillation* resulting from limitations of the agisting facilities, both batches' wore iuadcr,mntail:y satisfactory .to initial properties aM durability, Specific racosaaeatktiers for action, to eliminate the equiparent difficulties hare been transmitted to the Production Division* in the writer* letter of j?~ll-53 lo JH,Ballsy, "Flushing Facilities Building #12-." smmmumm the **&'' foraulsi represents *?.s firm a process as can be written oa the bests of the very Halted plant experience to data, Ite'ny of the details ers tentative, as indicated be 1cm x* Dus to scarcity of available pigsent presaeaks, the two plant batch as mats to dote were breed on 245 and 280 lbs,, respectively, of rather than the 300 lbs,? as formulated* The full 300 lb, charge can certainly be carried through the breakout and <31st illation stag as without difficulty* but there is seno uncertainty rs to whether the final standardisation volume will be too grout to permit .attainment of uniformity without use of a Digitpin Iflaser* 2 Breakout. ?rocpn$ - gMSSJbJl' In ell 3Moratory flushings <2,p gallon mixer) in which 1-2-P of normal solids content i.26*>l0%) was employed, satisfactory performance was obtained by adding ?0f; of the total prasscaks for the first breakout, foliated by three 10:1 .stepwise breakouts, fba pressevke <74910) used in the plant flushings was abnormally low In solids (21*23/0 end vary lev; in consistency* with the result that the ?C-IC~10-1D flushing .sequence failed to. build the con sistency of the flushed mass up to the rather viscous state required to effect complete dispersion of the presscako to t.hp resin* lire modified sequence (50 followed by five 30*$} com pletely corrected the dispersion, difficulty-, and has been incorpo rated in tbs nAn process, boon establishment of optimum A~2**P press burden in the plant it should be possible to simplify the Incremental flushing ssqu-ni'ice to something like ?G~15*X5 It is believed to he important to attain a state of soar-clasticity .at the end of the breakout -sequence in order to attain optimum pigment-rosin dis persion, Ibis, however., has not bean proved by controlled experiment* Approxirsately 65$ of the total water in the hatch is decanted* The remainder must he distilled* All decanted breakout waters are very turbid, as discussed below under "Goal field"* DUP050068478 -3~ 3 * Li<mtLMs& Addition of !U>30?8 to the total 1*2 pigments binder ratio prior to distillation has bean s poo If lad by MF. IIo opportunity has bean obtained for investigating obvious economy measures to* volvtog alteration of the composition of the finished 'product or the sequence of addition of ingredient** Addition of both the resin (;0tfp 3-9) and the initial portion of solvent (8trp 20) trust be conducted sufficiently slowly to maintain a ststs of Bear uniform composition in the batch*. If the very slog? critical rate is ernecoded longer than momentarily if is virtually certain that the batch will become lumpy and that it will remain ncc-vunttorm and lumpy throughout the distillation process ' This condition is believed to be detrimental hut no controlled experiments to chock this point have baas permitted to date * SyiS^l'lafet..i>hufel9M3 - Shutdown at the point indicated has no detrimental affect in the laboratory, provided the sides of the mixer are scraped domi and the surface of thp batch is covered with a thin layer of clear solvent to prevent shinning* 5* * &SSLg&% Tm quantity of triethanolamine used imst not be varied without consent of F&lk Decreasing tbs triethanolamine in the final base tends to increase reactivity* Increasing the agent inhibits reactivity and improves dispersion, gloss and clarity* but also retards enamel drying rat and increases degree of darkening on baking* The agent is added prior to distillation, as spacified by yF* If is not .known whether it would be more, or less, effective if delayed until near the and of distillation* 6* The detailed directions represent the best apparent description of ns a of the present equipment* ' The object of this step is the .removal of residual water from the batch by vacuum distillation of s:n sseo 'opic mixture of water and solvent, Excessive temperatures tend to gel the resin* Gelled material cannot bC T'ibcWbv**er*esdv-* mIni tvhj.1esa mlawbvo4rcatiworiy;4* the distillation pro- ceccls smoothly and effectively* at 24-2b xnckias of vacuum* if the mixer ,J.acket is maintained at a temperature of 1 '**190oF, by -a constant supply of- `hot water.* fTp he batch is allowed to become progressively more viscous. throughout the distillation* As the desired anhydrous condition is approached, the batch* which has been distinctly milky in atroaarance, abruptly becomes dark green and clear* Actual batch temperature ranges from 120 to 130F, during distillation at the above pressure* Upon complete removal DUP050068479 * ill SR. of wst&r free* t'r- letch to the Q2-nUO;4 range) the hatch tem~sretmr? arr-v^iy -and tog discpv-r.crs from ike mixer sight^glet :k..t dispersion $i~$. dcrit/ fcav* hcsn obtained by the writer 'tc/i the charge has bcsn p,y.V!itted. to ranch a highly viscous, s-ar/Wylsstic consistency at this stage., Shis cordItlor cannot b? nicked, hoprever, if the? mixer ^refcet is heated only ^.tfch .high pressur etedu Css has been true in the ease of the plant nirnr to dais), because of the great risk of resin gclaticnt this occurred in the ease of the first plant batch# Steps horn been taken to provide -the desired improvement in plant facilitt,: prior to future manufacture* Solvent iiktit ha added throughout the final, stage of 4is* tlll&tfon, in sufficient quantity to maintola the charge in a smooth, nbn-&re.m'.Xar state Upon canpieiioa of distillation the heat enpcly is replaced with cold rater, ;*' sol re at is added to the hatch as torpidly as possible without fmc.ing lumps of non-uniform nredtiet* Experience gained in the course of the next three or four plant runs should rerntt svueh sore precise specification of thustcape.ratura cycler ml yf solvent addition tines end rates* ? tmiUm, Iks product is to bo standardised at 39-41$ solids content# Film sclifs arc dot-:rained by drying a wclg^isxl sample of the mill base. Specifically, using an analytical balance throughout* 'weigh a 1/4 o.2o pill box ar.d lid, pour a of the sample {+500 mg) i4n*mt.>o.U.....tU.h.l.i.eV....p.y.<.L~JiLlJlL tX-oJUt.X,* yid- plies'' ,1l`.ikd."U %, ImF**s.i4ig.*h$, dr. sHni ov-y eK3 hl.i&dV * place Uo^p/Ceiini pp-S.i^lAl' box and migktd film in 113C ovoo,' ro'^igh with lid after 3 hours, and continue heating until weight is .constant* Calculate percent fils soliia from respective net eights of: m% and baked films# Exposure series are not? underway to establish maximum peraissable moisture content, YMs is determined by the conven tional tol.uaas distillation method Clarity and transparency arc the vital optical .properties of Pigment So Officiallys these properties can be determined by reducing 50 ,g> of the .Gill base with 41 g* BC-1Q3* adding 2 g* VC-1000 ascl 05 g# VP-7750, applying a 0*003" clearance applicator film over, black, and baking 1 hour at ,225F $he baked film must be free from cloudiness* If desired, direct c-oapariEon can be made in this test against a pigsaeat~f.ro clear enamel* In practice, however., it is always possible to .appraise the .clarity of the product accurately by inspecting a somplo of the mill base in a -glass container or on a bright spatula* Bases of bright dark green mas stone color .and free of turbidity or ailkinssa ere always satisfactory* Ho limit standards of turbidity have been established to date, and no arrangements have DUP050068480 bea_n___is_e_d..e ..wFitihil? for recaptehee of cloudy ht:z-:s* Although. firm conclusions a *.> I&possihte until, further .ru'crisnce isgoi:ad"j semiro.rtes s-yj plant performance to date lards support to the'-optimistic '.'Aon tmt the tee id one a o,f cloudy production ?rill bs sufflcie.iitly rare to permit F&F to cons-an* it, without difficult,?, in selects epolications* 8* Packing in the ire plant runs to elate it fes ibeaa nacessar? to reaove lasso? undlsndrs-ad tailings b? $ ning -the product through a. 20 &h screen auppcrrioct below s discharge gte clmpe< bO h dec ant teg ri?t of the jalxets Because of their availability's 3.5 gallon d rasas have been, used as shipping c>.;.ta tears to date* 'Xu the interest of scoaottgr it H desteams be usee j-ith '?&F for use of matesi ly s s fc Is fa " .;yJ, 7*>,sr arms of .larger eias ere re rably also suit able for use in shieding the iagradiaat rosin solutions from PhiX&delebU to Iterate* 3, YIELD As tegibated on rage 1 of these notes^ the theoretical commodity yield at 40f solids coxtent, ba^&o on 900 lbs* .solids input, is 25Q Vnz* Be canted breakout wster however, invariably are oulte turbid,,$ indicating obvious yield 1 css at this stage t!hhiiss loss has been sf eteralned by imalysis in the case of four laboratory runs to rpnga betuedB 1*7/ anrd 3 <,**5*% averaging Xhe is tloroforo* 2Pi*,** -9--7--5* * 23M.JJlte to date corrected to standard batch stea and solids content (2 batches* 1955 eic 1983 lbsM respectively) * StiBillXflSD BT5 Jo 0 * Morris on 10/10/50 DUP050068481