Document xn8Rw8M4e9EE130M8ojV8rmb

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial No,' Copy No. KN-53-17 / f\ X NEWARK PLANT I PIGMENT COLOR RESEARCH REPORT b "LITHOSQL" VIOLET 4RN LAKES Period Covered MY 1950 - OCTOBER 1950 A-IC-52 FILE; DATE. 223.61 MJ n A COPt TO; #1 - InSloriiltti TlAg 2 * Research file (223*41) 143 {223.41) 4. H. Tully/A. Siegel H. Arooal #. H. Cooper F. P. Ehrich - #14 file J: Extra Serial Ho. KN-53-17 Copy Ho. / $| XSMUK PLAIT pic w r t s c o l o r r es ear c h r epo r t FINAL REPORT TITLE; *LITHGSOLP VIOLET 48H LAKES Of IMPROVED CHARGE: A-IC-52 PERIOD COVERED; MAT 1930 - OCTREE 1950 SUBMITTED BI; APPROVED BT: DATE SUBMITTED; 7/16/53 DATE T^UKP: DUP050069342 --1* 18-53-17 Work on improving BP-176-B was started specifically to meet the requirements of the Ford Motor Company. BP-176-B is an alumina hydrate lake of BLithoaol* Brilliant Violet 4M containing ten percent of dye. This violet i need by Ford ae a red toning-' agent and dee to poor texture and dispersabllity, tha desired strength level and degree of redness wee not obtained within a .reasonable alkyd grinding cycle* Whereas seas of the difficulties associated with BP~17&*B were due to quality variations in the Lithoaol" Violet W dysabUff purchased from Orcfceo, the major problem centered about poor texture which could be attributed to aggregation of the acid* pasted dyestuff on drying* Furthermore, tin texture problem was intensified ter the Ford Motor Company rUbout procedure for pigment evaluation, which involves milling the pi&mnt together with titanium dioxide and alkali refined Linseed oil under conditions which undoubt edly cause little work to he done on the pigment* In the course of this development* Harmon offered to the Ford Motor Company a violet lake {B-4000} which was decidedly superior to our BP-176-D offering* Because of the urgency of the problem, the initial attempts to improve BP-176-D quality were made directly in the semi-works and in the plant. Work on improving the texture and rate of strength develop ment of BP-273-D wee a direct outgrowth of the work done on the Ford Motor Company problem* The ammonium rosinate technique was found to be preferable to the sodium rosinate method for the purposes of texture improvement. STOSAEf IRQ C0miBllCB8l BL-333-D lake prepared by extending a 50$ Eaaapo of ^ "Lithosol* Violet 4B1 (H-612; with blanc fixe to approximately 10$ dye content was offered to and was accepted by the Ford Motor Company as satisfactory against Harmons B-4000 counteroffering. A BP-273-B(E) formala involving the use of__ __________ in place of sodium -rosinate has been -developed end has been accepted by the plant for future production of thig Code* The product Is decidedly superior in texture against the sodium rosinate counterpart* Initial studies related specifically to the requirements of the Ford Motor Company were carried out directly in the pi semi-works and laboratory and were concerned mainly with the variations from the standard BP-176-D formula. in the semi-works draft tube unit with and without DUP050069343 -2< KB-53-17 the nee of Goulac as a dispersing uw end extended with dry Alenina hydrate* The products hews a narked strength advantage over standard and over a product made by the standard formula frcn the sans let of dye* The reheat (standard nsthod) strength advantage exhibited by the Goulac dispersed products over the wndiepsrssd products is not duplicated in an alfi,': enamel system* A 2000# batch of notarial prepared in the plant draft tube unit without the use of Goulac was e. red to red wad 92:100 in strength against standard BP-17&-D by the Ford rubout procedure* of BP-273-D and extension thereof in slurry form with blanc fixe to the timer content of BP-176-D. Two batches prepared in the seni-wnrks # draft tube were red and strong against standard BP-17o-D (standard rubout). BBP-32&-D Reaiurrying of BF-299-P (washed presseake of BP-273-D) and extension thereof in slurry fora with dry blanc fixe* One 500 lb* plant batch prepared in the Abbe*-Lenart sixer was . 90;100 e* int* and red vs* standard BP-176-D by ths Fori rubout method. d. of BP-299-P and extension thereof In alnrry fom with dry alumina hydrate* A seal-works draft tubs batch was v.s-. bine and strong vs* BP-17o-D (standard rubout)* Two 500 lb* hatches were made in the plant Abbe*-Lenart mixer* Both proved red and strong by the Ford rubout method* of BP-273-D and extension thereof in -slurry Wms, ' with alumina hydrate* A seal-works draft tubs batch was red and strong -against BP-176-D by both the Ford 'rdbout method and lit standard rubout procedure. A 3B00 lb. blend of several of the abovepjduct for shipment to .Ford.mas prepared*- The Control laboratory d^eeilbsi'the product as being essentially equal in strength, v*s. red to rMm and intense against standard BP-I76-D by the Ford rubout method* Attempts to recover substandard BP-176-D by rsslurrying in the presence of wetting end dispersing have given marked improve ment in strength wad redness over the original* The most nteMLCaarote- ment was obtained by dispersing with Biameol and precipitating m$ Biancol as the barium salt* By the Ford test* ths resulting product was equal in strength and v*S* bine against standard BP-176-D and s* strong and distinctly red against the original* DUP050069344 3- Kn-53-17 la general, it has been found that significant variation in strength and hue i possible for a given lot and for a given dye content, depending upon the manner of processing the product. Further, the Ford reboot method gives strength and hue readings which are in marked con trast with those obtained bv tbs standard varnish drisr rubout procedure and there are indications that strength shown by rubout, will not necessarily be realised in an alkyd grind* Analysis of the Harmon counteroffering (B-4000) to oor BP-176-D suggested the following composition: 77*45$ 6a as BaS% 1.96$ 41 as 412% 9,000 gosin 10.690 Toner (by difference) This corresponds to a 500 "Raaapo" type of toner extended with barium sulfate to approximately 100 toner content, BI*333*D 4 series of roainated lakes of the above type have been prepared by the ammonium rosinate and sodium rosinate methods. The products are very strong against standard by the Ford rubout method and compare favorably with the Harmon counterpart in strength although S, blue. BL-333-D lake, prepared by extending a 500 Bamapo* lake of "Litbosol" Violet 4Hs Th -6i2) with blaac fixe to approximately 10 dye content closely approximates Harmon** counteroffering. Evaluations of various experimental products including ABL-32&-D, ABL-331-0, ABL-333-B and BP-176-D, utilising the FowT* test. Ink grinds in alkali-refined linseed oil* sad grinds in alkyd revealsd marked differences in rate of strength development despite small differences In texture as detsrminsd by grit rstingi#' The results indicate that BP~17~D made by standard formula la quite variable in this respect and that a product of the ABL-333-D type is nn, of test in rate of strength, development, Two semi-works batches of ABL-333-B have been made* tm first (lot 2364) made from Orchem, lot 17* dye was vs* strong and slightly red versus the initial Harmon offering to Ford, The second batch (lot 2366) made from lot 19dT as somewhat weaker and bluer than both lot 2364 and the Harmon product. The results essentially confirm the previews quality reports on lot If dye ` ` " ` " hw la dependent to a significant 'e***#*^ on -the qu Strength development seri Ford alkyd system confirm? the sr-- standard 8P-176-D, which in turn i5 products in the material over of tlhv recent - DUP050069345 KS-53-17 production of the letter code* There sppesrs to he & significant o^einfp between the strength Mild ^ the Ford rubout test end the rets of strength w development realised in practical alkyd grind, mis scene to he in x order in slew of the obeervation that the Ford rubout method affords little opportunity for meric to be done on the pigaent and consequently 4 requires it to be of good tenure in order that a given strength level be realised. A 2000 lb. bateh of ABL-333-D has been manufactured in the plant (lot 1779*# and approved for shipment to Ford. The product rated IQSflQO, a. bine, e. dull against ths experimental seal-works sample lot 2369# (A 50/50 mix of lots 2364 and 3366 ABL-333-D). Ths difference in quality mas predicted oaths baeii of ^ the lots of dye availablefor use (32.1$ lot 17*J,2.2$ lot.ld# 15.7$ lot 19). The'experimental sample consisted of 50$ lot 17 (the bill of recent Qrchea shipments), and 50$ lot 19* Lot 17790 m* superior by Ford rubout to the latest ship ment of Baxmon'a Inks (C#53661) against which it mas rated` 9531~0~0* red, and intense. "Llthosol** Violet 4BS toner recovered from substandard BP-I76-D by aeid extraction of ths alumina hydrate has been converted to the BP-273-D and ABL-333-D lakes. Ths produsts appear m&ak by rc&axxt* Evaluation of the BP-273-D lake in Dulux in an attempt to Throe plant batehea (2,000 lbs. each) of ABL-333-D mere made using lots 20 and 21 of Orehsm dye (N-612). Based on Ford ruboutt eand Ford alkyd e_n_a_m_e_l__e_v_a_l_u_a_t_ior_n, all three hatehee mere satisfactory for Shipment versus lot 1' the first lot of manufacture, and which Ford has set up as a temporary A 200 pound blend of the first four plant batches of BL-333-0 has been prepared end has been accepted as ths standard. Three lots of general*# Indanthrene Brilliant Violet MA presscake (chemical equivalent of DuPont*# "Lithoaol" Violet 4HN) mere tested in the ABL-333-& formula and found to he uniformly un satisfactory by ths Ford rubout procedure. Ths products prepared from General*a dyestuff mere exceedingly weak versus their counter parts prepared from current DuPont dye (H-612). mmri A 50$ "Haaapo" lake of acid-pasted "Llthoaol* Violet km DUP050069346 XH-53-17 (li-612) has been prepared (seal-works) for comparison teacturewia versus a standard BP-273-D <7251 "ftamapon lake). The product is coded ABF-337-0. was superior to tnst or Standard BF-Z73-B SW.LokJ, Mm&MAsm SBP-273-B 22441177 7722$$ dye--aamasmaoonniuiuma , _ rosinate ABP-337-D 2412 50$ BP-273-B -SD-90B70 Alkyd evaluation* of BP-273-D lakes prepared by tbs ammonium rosinate process (EBP-273-D) and the standard sodden roslnate process indicate a higher initial consistency for the ammonium roslnate products, presumably due to a higher oil absorption* There is no significant evidence of greater reactivity in the amsosiua rosinate products* An P & P, Fhila. evaluation of an experimental ammonium rosinate-type product (EBP-273-B, S.W* 2417) revealed no evidence of reactivity in paint; but the product was criticised on the basis of tinctorial properties* Quality Control evaluations of the two typos of lakes confirm our findings with respect to the inherent superiority of the ammonium rosinate material in aUcyd enamel (.slight redness, intensity, and strength) and by the varnish drier reboot procedure (up to 30$ strength advantage), the superiority of the ammonium rosinate product in texture and rate of strength development by ink mill test has been previously reported. Recommendation has been made that all future production of this code be made using the (E )BP-273-B formula end that a new standard be set up. The work reported hen is recorded in the following notebooks: .Hi DUP050069347 KR-53-17 0.05 &sm* 0.5 * 0.5 iefined linseed oil 0% Place on Hoover miller plate, in by hanti with soatula. loll 10x50 with 150 lbs. - weight on smller.Mount on glass. (2) (A)BL~333-0 formula (attached) (3) (S)BP~273~D formula (attached) (4) BL-333-D formula (attached) (1) Exposure Program Violet Lake. BL-333-D and BP-1?6~D, Ford Alkyd Tints, 2/12/50. (2) Letter L. F. Andrews to F. P. Bhrieh, 6/9/50. Karaon B-4000 vs BP-176-D. (3) Letter L. F. Andrews to d. B. Cooper. 6/16/50. BP-176-0 Ford Motor Co# (4) Letter F. F. fberieh to J. H. Bailey, 6/22/50. Platinum Violet Lake BL-333-B(B). (5) Letter F. F. Shriek to F. B. Bolton. 1/1/30# "Ponsol* Violet Lakea for Ford Motor Co. Oil Absorption/ (6) Letter J. C. Hiasen to F. B* Bolton. 9/15/50. Proposed lew Standard. Platinum Violet Lake BL-333-B (lot 716. SB~7lSi and 9/19/50. Supplementary Report. (7) Letter F. F. Ebrleh to B* Arnoul, 9/19/50. "Platinum?* Violet" iP-273-B. (S) Letter C. Botti to f, F. Speragaman, 9/26/50, Platinum Violet Exposure. (9) Letter F. F. Bhrich to H. Amoul, 10/20/50 "Platinum Violet** (E)BP~273~B (10) Letter J. C. Hieeen to F. B. BBoolton, 2/14/51. Viscoaity ToataPlatinum Violet Lake, BL-333-D, SD-71S. DUP050069348 VM Prep* 1 OCC.&, -. re*.. _....ALL).. . SGiUl. SOQM.............SI23:. .....-.......... FFE i/21/50 Dia;o r:zr.................. ....... ..... . ha ooomsa vaa..... ......... -.......... .... csroTS/Sh/#} stxm y m; ZbSX,A~39Sl,^.. -________ ^ .XsTM&- HAMS: P4ATXI0M FXOLET LAKE KSTPOCTtOHS USE IBS, N- ii^QCXCODS ]} UBS. 1.*.Chop; to./&** AtzumbBr. ..or le^.^mlis^Ljand.Mid.. . ..at Fat. 311 .for stop. 9 ... ....... .... ..... ..... ,..., , .... 2. Walsh and hold at. Fat...3.62.for* step 2.1 ........... ,.., 3, Weisch and hold at Fat. 390 for step 29................ . 200 239 j 200.. 100 161 100... 1600 1 .65 1 ,1600.. 240 4. Pimio.or ran Into va,t 240... .... ............ ... ,............... 1{^52 612 tj 2 S Lot of- 5. Wash in drams* .... ................................. ,..., ,....,, V1.. 6. Ad hist to 15 (6630*).,.......... ........ !! II -.7.. . Ff?.0.... ......... ^ ITT-: 3 ft* 9* Run. Q (1350} Booiro in I~39 water into .vat..313.*... . tsremrod in Stop 1. ., .,................ ....... ..........j 1.0. Stir 3 miriates or lopsfsr....................... 11- Weigh and ooar in ... ......... ....--................... ..... .. .. 61... 12- Stir 15 nrinat.as ..... ............. ....... _ 11. Whop stpp 12 stirring Gpraplptod...adjust' -Fat. ,,3.1,3 po" 23** f 3A.5Dk . '. . '..................... 1 fi * ii ... it _____... 122 II..67 .... s -.... I. ..._ 1L.. Host to boil . . .... ..................... . 1 5 ,, Stir 30-A5 laf.nvtos at boil, to stable...whit.... ...... ........!_._:....... :. #*Rupii on - .EfljwlsJ op DRwt. remain faille whits, pnd.. not heooma transnarsnt. on ..c.ooJ.ins . Test and RannrdJ' Btahilitv * . ......I . L. L 1,,6- ifiRt. And RapprdS. t>R ......... .Jfpttfipil 9---0,~9*3.. . 1 ......... ,. 240','~'<7- Ran Vat 313 into lint. 2ij.D at. oiipo. .th'f'ii. 20 i^psh 4* > , Ri'TOPn IS- Sti r 60 miT?t.s-. ..... ....... ,.......... ..... ...... .... . .......... ...... 5 .. .. To. ?ft Rim oiJ (indfrl ter into, Vat ift?.. . Tnpn on agitat.or and shegp.......... ... .. .. _ 31. Thmo in W-16 wei *rhd in Str>. 2 ....... ...... ... . 39. Adihpt to 12* # 1 *?^a>' at ..1 50^155? ?3. Stir until disspi.irad . ........ .......... 1 . ..1 I 390-24Cb/,... Wnan .stem .1# stJ.rring.r.pio.mnjl^tod.J...st.riko Fat , .,3ii2_- 6 a-h 1 50-1 55'S* into rat 24.O..op . ..hl^e...surfs oe in .... 10.--15. aiivn'ito.s . ..... _,........... .......... ..... 35. Start oirmlatiop .ntimn. snd.-imlv 390 agitator at...... onnh r .p .m. . .*.. .* ..... ...... ...... 7. ......... ...... ?6- to Pn0.~2ff5oP r,..25-3n_.wi :mtas. ............ 37. Hold at- .2,00-205F .for..30.niroalat.* irg Vat. .p'4h thm.draft., tnbo. maintain ing Vat _3Q0. lo-iral 16F from thedon,.. . SITMit off Rst.Aawt.,.......... .... ... '... ........... 9Q . &AA H.f%5 vi jrbod in.. step .3 ..1 nt.0...rat..;3Prh.dra.ffc . 30 . Sti r and oi nonlate.ma.irta i 1 iif* from., ton - .. .,..... .............. .. '.................. ... c o h t d o p mm z. 1 -. .1 "1 .. 1 1 ! DUP050069349 PASS; 2 CODE: ' BSTRS^OHS M. w e 1m. COD'S ACCi.'. IBS. .. 3......... 4Jkd.J&t $L%p&ti,ixe^ ...................,........... ................ .... ........................... 18.. 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JJi Uj l ..u....u......,I Jim 1 .......turn' v n, ...,. 1 .> '* DUP050069350 DUP050069351 ptmi 2 CODS:b l 333~d A^S^S ,., . >fn)M -fw* "1 Yi qrt **.A. ms! 2000# ms s u c bq b s | u s eis s . co.inf-s ACG3. m. : y*"f'f*i ^-g- .JlW* Oxftm..... i* oa,....... . ,,....: j|fltfia3iiMS.t,. $im&.Btmvfi&el -,,,.n...,.... .... _-..,....,_____ *.... ... . .$*..... ... .Tip.. `n-11_ .Jjflflg * rCifitii. Hffij&jS ^ | ^ .ulfj * "1 1 .......... .bs addsd. ^...Drf.;^.._t.l3at.....slii?y...Mill.....^t.I,.,..'.. ....... :....,.._.... 'vab...390- ....'..' .... A*!'.'............ ... ^..', '..' .......... ".'..... ..,....-...pimp.....5id .,^1t.....39.0..,iagS,t.s.t.^.*............ ....... ,,....... , ,.....,..,... 3.1..-........fem3,p._______________________ ____ .........,,.. ?2L-JfajihA..sraij 390*...- '-....... ..... .Y,,ri..... . ......... 33..:C]-?frrte. and.Stoisardi. .......... ... .' * ................... 34*-. .PiffSMMf- .w^.t,k.4gi:|;-tfi.oa,.... .......... .............. ............. ... .. 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'invhil. . . . . . . ^. i.B.aol..^.rl .......................................... . . . . . . . . . . . . . . . . . . . . ... . . . . . . . . . . . . . ,,. . . . . . . . . . . . -. . . . . . . . . . . . . . . . . . . . . . . 'Si. AfSh-a-** srhap 1 K as-i-l-w5Mmrfita 4*.a 4 at.vile -twa*. Ifl'i 6 alt 1 ^nl *S*v T? -?*ho fcr>llrsi v*h n 4*Jh^ *3t , , IO.-.I.5. nsi.wt.ft'P,. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ......^. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ....,T. ......... S2.. . . . Tfeaf. fcn. . . . . . . hm` 1. It s .. S.5<$.0.. mlmihaa.*,. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .................... .. .. tJSfe 4 *. Afc hf>il $11. *. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ,... . *>5 -. . . . . . Pv -j .s? .*rif..*:li(i'.m.fv ..agit.at.-f an.. _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ -...._ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . . . . . . . . . . . . . . . . . . . . . . . . . . , _ _ _ _ _ _ _ _ _ _ _ S-fcaarh Sj . ... 1$ ...,_.,__Ctofca.. . i'l 9. ,' S '4-tNM f? ,, , Hi WlC.'i HWW'H-TVHS ..--o o mi'd Grvissrr*1- __ 19 IW!|III>*IWM IIMIIOIIIIIftWW , '. '. ! j DUP050069353 DUP050069354