Document G6JVV6bR3xandZox2d6Xp093m

J. to It KBT-54-24 CPC UEG&HS AHD PIHI3HIHG (LABORATORY AND SEMI-WORKS) By: P. H. Griswold, O.J.C. Kle E. I. DU PONT DE NEMOURS & COMPANY 256 YANDERPOOL STREET NEWARK, NEW JERSEY /(liSH-Xi ~ - Serial No. Copy No. f RETURN TO JACKSON LABORATORY FILE ROOM NEWARK PLANT PIGMENT COLOR RESEARCH REPORT KbU a*srt CPC BBa j u irruT.QnTBn (t.RWfmywf iim & JWZ, 1949 - HTCCH, X951 Period Covered .1 4 X TO * d <4 HJ 4487 FILEt DATE: ****** 7/8/54 DUP050069932 "S' DON'T SAY IT--WRITE IT To------- library----------------------------- v. : . t FfROM:y;X-:r .V; v. \'V'.: O.v'i-v,:;: / V'Yv.-fX X- '! /.y Xy IYY;:Yy ',y : :! V :S. / A-. ;VVi-^ >$y. VA',:^!:" V'p: 'v y .j l:'V V-: ' S'** X; ^ -1 ^ -Vv^ :r~ d at e___ 3/l9/f?4.......... f E;- O'/' :V^ ':.' l-V ivi; y.j!;V ; KN-54-7, titled "CPC Green Milling and Finishing (Laboratory and Semi-works}' dated July 3, 1954, should be renumbered to read KN-54-24. Please change yo.ur copies accordingly. , iigjmj! STOP ACCIDENTS BEFORE THEY STOP DUP050069933 Copy to* #1 Saaorleal Filo 2 - RMOftroh Qffleo (342) 3 * Libra? W3 (22342) 4 * V* 8* Cbalqpakl, Kawport 5 J. 8* 7*039/4* Slogel 6 j# H Cooj*r 7* 8# P# Klonko, Nwport 8 - H4 HWfi. Pllo 9 8# A# Paridw# Jaeksoa 14b# 10 * V# J. Cl*, CfaSBbOM Worka 11 - P. J* Monahan (For Z p&lo) 12 * Extra 33 - 14 * Ktf-m-i-y Sorlol m>* V#f Copy Mo. / NEWARK PLANT nmafTfiAT. DIVISION * COLORS Final Raport ryyrje^ CPC waai imiTm AHD FINISHING (LABQRATOKT AND SEMI-WORKS) p e r io d c o v er e d * Mi# 1949 * k ar c h , 1951 CHARGE* A-I-C-18 d a t e s u bmit t e d * April 6,1954 DATE ISSUED* July 8, 1954 DUP050069934 Between June, 1949# and Mareh, 1951# several investigations on the finishing of CFG Ovsen ware suds in the laboratory and Sesd-work*. this report stsnarisoe this voxIt# whioh was largclyoonoeniod with texture trestawate, solvent willing# dispersion willing, and extinction* The principal findings and conclusions reached as results of the several studies are llstad belowi a* Ink adll properties almost equal to those of CJT-486-D, lot 168, are obtainable by treatment of solvent allied CPC Green (5*624) In the draft-tube, with 5% of eastern tetrachloride and 25 triethanolaodne eater. 5-624 derived fron either sulfur chloride or euteotio erode ie suitable; A deoreaee in strength ani&ktmimi.mm thtt treatment* 8* WTMft TOIHg (1) Alkaline materials vere found to be effective in inhibiting deterioration of color dosing solvent Billing* Trleodiun phosphate was the preferred material* (2) Sodion nitrite la superior to sodiuft chronate as an caddlalng agent to inhibit eolor deterioration during eolvent Billing* (3) Plant milla, the 200 gallon Ssad-uorks aill# and the ld gallon laboraftosy adlla gave similar rate# of strength development during Billing* The Bead-works $0 gallon adll and the laboratory 0,65 gallon adlla likewise gars equal performance, but slightly faster than the others* Eight-ounce Jars were the elowset of ell* (4) Buteetio prooeee crude behaves essentially like sulfur chloride process erode in rate of strength development during solvent adlling* (1) Diepeieion adlling gives yellower product* than advent adlling# regardless of whether the erode le derived fron euteotio process, sulfur chloride process# or day chlorination prooese* (2) Dispersion Milling gives products of improved texture and excellent ink sdU behavier without special eoft-povder treatments. (3) The presence of "Span 80" in dispersion willing laprovsa vinyl dispersion# but not strength or intensity by rUbout. DUP050069935  2 * (1) "Trltone X-100 wm found to be the beet agent for promoting tfee vetting of rotating dryer erode in tbe extraction etep. '% (2) Laboratorystudy shotted no oxidising agent to be enperlor to sodium chromate in extractions of still slurries, but that chromate iteelf u hannful to quality* (3) la Seai**iorka extractions of etiil slurries froei Seaport, it one found that! (a ) Cbrocnte ehouM be from aoid edneline* (b) Aoid concentrations beta* $$ are effective. (o) KaOG is equivalent to in alkaline.extractions. a. The lota comprising the Send-morka study on texture improvement are listed under "References" at the ad of the report* The overall results are reported in IS-53-1 (Sew lfceft-Tube Processing Methods), although idle Scoi-morks lots are not referred to there specifically by lot maker* All tbs lots enumerated in the "References" represent variations in the technique of adding an agent in the draft-tube, such as determining tbs effects of heat, cycle tine, point of addition, amount of agent, ate* B. 8?lTffllt Kfflllg (1) litoai2EZ-2Mtt (a) Various agents mars introduced into laboratory half-fdnt grinds to radnao deterioration in quality, because it had bsen sbctm (134S-50) that ]Qh deterioration uu morse in steal adlla than in dan* A amis CPC Gasan ubioh containa amr teaidnal aoid msteriaL from hi n<w m bh not removed by in noat jugofosbly deteriorated daring nilling operation by the redwing action of nescHit hydrogen evolved .In the re* action of the auidlo material with the steal shot in the mil* To prevent this deterioration a laboratory milling study mas made in Uhlcb natarlala mars duoad tot 1) Ramova any neaoant hydrogen formed* 2) Prevent iron from reacting with said by ocmplagdng its ions or 3) Keep iron from going bate solution. j* i sun 'OCKiLfluLttjLsut ttjdUbooi# ,5) Maintain an alkaline medium* :j| DUP050069936 * 3 alm lotrodUIKdl (X) To remove hydrogen war* nitrobeasene, benaaldehyde, wi<lAnMwma . nWmnU awl bh Iw mmi. (2) STESpJlren from reacting by oaaplwcing lit sodium fwwoywldt mk I sodium uyaiiide, wd (3) So keep iron fro* |Mi3i Into solatiom sino, aluedxusa Of tngyi*>|<ww BaiSXfall XwOHZtS M^ia" thStt lND ia the eleotromotive series* (1348*53)* m. beneficial effects mm observed free addition of any of the above to the Bill ohargas. "i; Materials introduced to maintain m oxidising nedium were potassium permanganate, sodium chromate and sodlm nitrite. the perumagenete woe reduced during grinding, thus becoming ineffective* Sodium nitrlto gave wy satisfactory raaulta and sodium chromate slightly poorer (1348*43, 58). introduced to w*<ntf<*> an atannyp ned^uiw thereby neutralise realduaX aeld in the crude CPC dram were sine oaddo, alumina hydrate, aodlua carbonate, dlaodium hydrogen phosphate, triaodlua phosphate* She addition of we alkaline material had a decidedly beneficial effect, with trisodium phosphate the beet (1348-50, 56, 58, 62, 65, 66, 70, 71)* To determine uhether any sulfur, which might remain with the green from SCXo hydrolysis during dgaeoua eactraotlon, would be harmful dining grinds, sulfur uas also introduced ia I grind* ho deleterious effect was observed (1348*36, 37), (b) *t A comparison of the various types of wills used for acetone willing was made in the plant, Sami-worke, and laboratory. Grinds were continued for 120 hours in a 1200 gallon plant adU, 200 gallon & 58 gallon Semi-works sills, 1*8 gallon and *65 gallon laboratory mills, and 8-ounoe glass Jars* The grinding aurves (see graph) (strength ve* time) of the 1200 gallon, 200 gallon, and 1*8 gallon Bills were practically identical* The grinding ourves of the 58 gallon and 1*8 gallon sills were likewise practically identical* The 8*oaao9 jars were completely different from all the others, and very slow* As color characteristics appeared to be the seme at the sues strength levdl regardless of will siss* The particular lets of sUlfur chloride crude used were vs dull and vs bine at the strength level of or-674~D, lot 430* further grinding gave considerably wore intensity, more blueness and a snail increase in strength* DUP050069937 DUP050069938 T t me, Cflours) 4- (a) In the Secd-warks, solvent wil l Inga were Bade for the study on rate of Billing as described in the section on laboratory Boric* In addition, evaluations vere Bade of the relative nerlta of sodiuoi nitrite and sodtoa chromate additions to solvent Billings, and of the response of Orcha* eutectic prooess orude to solvent Billing* Lot nustoere are listed under "Beferenees1*. The evaluation of nitrite end ehronats was dons in three acetone ajllinge of a sulfur chloride prooess erudei a control containing chromate, a second with nitrite instead of chromate, and a third with nitrite using re-extracted orude. Use of nitrite gave a product we strong, intense, vs yellow versus the control* Be-extmotion of the erode gave no adgniftoant toprovestent. (b) Solvent Killing of Euteotio Prooess Crude ||a studying the response of euteotio prooess orude to solvent Billing, only the 200 gallon, 58 gallon, and 1*8 gallon willa were mad* Milling ms continued for 120 hours* Grinding of the euteotio green coopered favorably with that of the sulfur chloride Material* The strength in both oases use squid to GT-674-D, lot 430 at 24 hre. is the 200 gallon Bill, end at 18 hre* in the 58 gallon aill* The euteotio green showed an initially higher rate of strength development, bub the sulfur ohlorlde green reached a slightly higher Ultimate strength after the 120 hre* grinding tine* The naestoae of euteotio green equaled that of CHM&74-8, lot 430 nosh sooner then the sulfur chloride green, being equal at 12 hre* and 6 hra* in the 200 gallon and $8 gallon sills respect- , ivoly. The aasstone after 120 hre* was very Jet* In several Semi-works series, salt Billings end dispersion allllngs were esrried out on euteotio prooess, dry chlorination prooess, end sulfur ohlorlde preeeas erodes* Control solvent millings were wade either to 1*8 !4. gallon or 58 gallon wills* (Sea Seni-works and laboratory references for m nunbers of Billings sad experiment nuabers of evaluations)* The results arf given to the eeetlon on "Swamary and Conclusions0* Inoonolusive resulis wars Obtained frost the dispersion Bllllnga of h sulfur chloride prooess orude from Newport and of a euteotio prooess crude frost "OretuaP, because of deterioration during extraction* The deterioration to believed due to the presence during sold extraction of flaks iron to excessive quantity* The origin of the flake iron to attributed to faster than aoxuwl wear frost a charge of new "Qyl-pebatt used to the ailllngs* DUP050069939 (i) () Turkey Bad Oil, weed se a wetting agent for crude ext|ietlctt, was found to haws a hgrarcL offsot on ultimate pigment quality, Laboratory la* Mtijitlo) to the following conclusionss increasing caused greater deterioration (1343*60)} Insufficient removal ty ^""jfrg was harmful (1348*61)i taafU odeplete of Turkey Sod ^ gave iwofr Improved quality (1348*62)# The foUowing were examined in ^ laboratory as watting agonist 2s b s l > Colloidal HX fVfefffnl mg triton B*25 Sotex C Viotawet 12 TetradeeylaniDS acetate Triton 18*100 4lmNH9Q99C MV Glyceryl Konorloinoleate Spin 20 lissapol B Cetyl pyridiniwa bromide Triton X"45 Soya leolthsn Sodium hydrocarbon sulfonate Polyether alcohol Condensate product of fatty acid jUarlosQ Lsolthen Co# Graham Bohn & Baas Synthetic Chemicals Ootylphsnyl polyglyool ether rtl OSide Sorbitan monolsurato Victor Chemical tfoadcm Amour & Co# Bohm& Haas Onyx Oil & Chemical Co. 0# P. Ball Co# Atlaa Powder Co# Oleic acid chloride p*anicidine*o*eulfonio acid mant1 nn oroduot ib sodium nit I#C#Z. Polyether aloohol*ebort chain William S. Kerrell Co# Brfai & The beat of these was Triton K-100, which gave good wetting, ariLniaraa feasing and no deterioration in the Hatching of the green# Mum iron uu xareeeat dur** ttu extraction of the crude with acid gave iapmwssnft in quality of ths final product (1348*35)# Strong HCL proved to be a good aoid for extraetion of crude (1348*40)# Addition of oxidising agents to eruie extractions was tried as a nsans of improving quality* Potassium psraanganate .mad s0|iui hypoohlorlte gave produsts superior to a eontral (1348*48). la one experiment on acid extraction after elimination of chromate gave an improved product it appeared that DUP050069940 m 6 * (*> (*) MngUga-ftff MUJlvrrtffl Several M<4NUVto series w n ran to detemlne the causes of wraVnnee In plant lots* Vlrioua acnbloiticm of cxtfeotlon at different ocxjoentrations, with and without 'tbo preeenoe of sodiun blreaNfee* and with or without previous or subsequent oauetio soda or nene^neiL^e oat* The results aro sumsriBed as followei I. Filtration of the atm slurry, with no extraction} 3% %SOi extraction of tho atm slurry} HHj ,QH extraction of the atlli slurcy) HH^OH extraction of tha atm slurry followed by 3$ KiSCk extraction (no ohronata) yi im produota easen&iauy equal in quality and Kara as bins and doll ooopared to Gr-674-D* lot 430* IX, 411 aoid **fcraff1tiaws containing ohronate resulted in significantly weaker products than corresponding controls extracted without obrooate. HI. There was no eignifleant diffaranoa between products extracted with It* 3% and 5% HjjSQ^ (no ohrooate)* IV. in awwnnla extraction followed by an acid ohrcnate extraction ia equal to tha ravaraa procedure* V* in add axtraotion following an eamonla extraction offered no quality inproveoant* VI* The ocngwrisen of BaOH and WUM to tha alkaline extractions disclosed no significant quality differences. VII* Tha HUMtonee of all products ware lighter than that of lot 430* VIII. Tho fewer tha nutiber of extractions, the darker tha neastons* IX. Basstoaesof produota extracted with add bhroaate 'Ware limudably lighter than those without ahrooate. DUP050069941 7 i (1) DnfUtdM trsstmsnts Loti 2037, 2Q36, 2043, 2046, 2047, 2059, 2060* 2062, 2063, 2Q6, 2065, 2066, 2060, 2096, 2097, 2101, 2103, 2104, 2107, 2flf, 2257, -B. JSmSoGlUvmeMnUtMSBIWIH4im, (1) Substitution of nitrite for ohranate, 200 gallon Bill grinds. Loti 2562, 2563, 2564, (2) Bat# of grind study* Lots 2572, 2573, (3) Solvent Billing of auteotlo orate. Loti 2606, 2607. 0* ^ffPTTftiTn MiUliw (1) Salt and dispersion Billing* of soteotio prooess orudes. Loti 2211, 2212, 2213* (2) Salt and dlsporsion ailllnga of sulfur ahlorlds prooass orudes. Loti 0^4, 2215, 2222, 0005, 2226. (3) Dispersion alllingi of four lots of euteotlo prooess orate. Lots 2262, 2263, 2264, 2265. (4) Solvent allied controls to lots in (3) above. Lota 2250, 2259, 2260, 2261. (5) Dispersion Billing ini solvent Billed oontrcCL of dry ehlorinsted orude. Loti 2302, 2503* (6) Dispersion Billings of sulfur chlorite prooess oroiss. Loti 2502, 2535. (7) Dispersion Billing of antsetio process orals* Lot 2600. DUP050069942 D. MOS^OB (X) Extraotion of Htuporb atlll alortlaa* Lots 2503, 2504, 2505* 2506, 250?, 2508* (2) Extraction* of fiva different tilX slorricM frat Seaport* Xot 2530, 253X, 2332, 2533, 2534* ** 4M2llWotOtL3flyfcMftfl^ Reported in KB-50-4* 2* WTffil Mp&M (X) Sato of gjind tod}' on *olfur ohlorlde process orude* Hotebook 167, Experiments 39, 40, 41* 43, 47, 42, 49* (2) Rato of grini atodjr on eoteotio proe*** crude Hotebook X367, Experiment* 56, 57, 58* wt5S3TSSWTBp!w^pR36f 43, 50, 53, 56, 57, 5, 62, 65, 66, 70, 71* o* faffpmiffli w u im (X) Evaluation of Sonl-vorics lot* of salt and diapaxflon milling*. Ratebook 1336, Experiment 69* - (2) Evaluation of 8o|i*ork comparisons of advent and dispersion adlling*. notebook 1367, Experiment 7* (3) Evaluation of 8mlai'ka solvent and dleparaioo milling*, notebook 13670 Experiment 9* D. Extraction (X) Tidal* of Hatting igect*. notebook 1342, Eaplrinaat* 60, 6X, 62, 67* (2) Acid extraction of Iron containing avndaa* Botateook 1342, Experiment* 35, 40* (3) Evaluation of oxidising *1**^* in vdnatioit* Hotebook .1342, BxpexdaMHSCt* 22, 42* DUP050069943 Ifci'JK KS t-c- ' " - i 'i * i > v O^iS V^xG^ .\\v ^ ^vssS* ^ -. j q >. s a rAftV'5^ hOS AS??^ w\X'^T`'!'a*'-Afc" DUP050069944