Document zoVw63VgYvDDjVXzgVjrJQeJm

pi E. I. DU PONT DE NEMOURS 6* COMPANY PIGMENTS DEPARTMENT isb VANDERPOOL STREET NEWARK, NEW JERSEY Serial No. KH-53-18 Copy No. / \ NEWARK PLANT CHEMICAL DIVISION - COLORS t "LITHOSOL" VIOLET 4BN - SOLVEOT-MILLESG AHD OTHER FINISHING METHODS Period Covered FEBRUARY 1950-SEFKNS8R 1950 A-IC-52 FILE: DATE; 1 223&! 8/21/53 A rl Pi i A i COPY TO: #1 - Numerical Pile 4/ 5 - H* Arnoul o - J H. Cooper 7 - P. F. Ehrlch S - #14 Building Pile 9 * Extra 10 - Extra Serial Ho. KH-53-18 Copy Ho* / NEWARK PLANT PIGMENTS COLOR RESEARCH REPORT TITLES "LITHOSOL" VIOLET 4RN * SOLVENT-MILLING AND OTHER FINISHING METHODS PERIOD COVERED* FEBRUARY 1950 - SEPTEMBER 1950 CHARGE: A-IC-52 SUBMITTED BY* ^P. F. EHRICH APPROVED Bit DATE SUBMITTED* 7/16/53 MW ISSUED: DUP050069333 KH-53-ld The original plans for the Pigments ^apartment phthalocyanine plant at Wswport called for tha eventual manufacture of a red shade of blue similar to that purchased from Orchem, as *MonaatraI" Fast Blue 2B and which is sold as the barium rosinate lake BP-243-D. laboratory work was initiated to this end* and considerable interest was developed in the violet pignent Itself which is used to shade the CPC to give the redder product * Pressure on this violet work was further intensified by the Ford Motor Company interest in a violet for shading pwposes* At present, acid-pasted "Lithosol" Violet 4RU is purchased frost Orchem in pulp fora (N-612) for conversion to the barium rosinate lake BP-273-D and to the blanc fine-extended barium rosinate lake BL-333-D. This acid-pasted violet, although purchased as a standardiz ed product, shows considerable variation in strength and hue when converted to these lakes by standard formulas. Baaed on the Pigments Department experience with the solvent milling of phthalocyanine pigments, the solvent-milling of crude "Lithosol* Violet as a means to greater pigment consistency with respect to strength, hue and texture was undertaken* "Lithosol Violet 4RH crude can be solvent-milled in acetone to give products superior to those obtained from the acid-pasted counterpart (N-612)* The solvent-milled materials give lakes (BP-273-D, BP-243-D, BL-333-D) superior in strength and texture to the acid-pasted materials and give greater product consistency from lot to lot* limited experience with acetone-HF milling suggests that this method may be a satisfactory alternate* Salt and dispersion milling yield inferior products* Work on solvent-milling and other finishing methods for "Lithoaol Violet 4RS was discontinued due to the decrease in volume of such eolors*and the anticipated strong competition from Barmen*s Thio Fast Red MV-6606, which appears to offer better money value for the shading of CPC Blue. DISCUSSION OF RESULTS: "Lithosol* Brilliant Violet 4RR crude in aolvent-milled in acetone in a manner analogous to the solvent milling of phthalo cyanine pigments. To a 1*8 gallon steel mill charge: 13,000 gr. 5/32* steel shot 150 gr "Lithosol* Violet crude 1,500 ml. acetone DUP050069334 Grind 72 hours. Screen the Billed slurry from the steel shot end dilute to 6 liters with mater. Steam distill acetone-free. Add cone. H2SO4 (as a 111 solution) so as to yield a 3*5$ solution. Soil 1/2 hours. Filter hot, wash culfate-free. hhsh on tlm funnel with a solution of 50 ml* cone. HH4OH in 1 liter of water, hash alkali free to Brilliant Yellow, Hold as pulp. A BP-273-D type "Bamapo** lake prepared from laboratory solvent-milled bitho*ol* Violet ABB crude was strong (100 parts*140 parts), bins, and al dull against the control prepared from N-612, (acid-pasted "Lithosol" Violet), and against standard BP-273-0. The distinct strength advantage offered by solvent-milling as against acid-pasting, in final products such as BP-273-0 and BP-243-B, was established using six lots of "Lithosol" Violet 4RH crude received from Orchem. All the products (solvent-milled In 1/2 pint glass jars and evaluated as barium roslnate lakes) were strong and blue against BP-273-D standard. Rubout evaluations of both the solvent-milled toner products and the BP-273-0 lakes prepared there from indicate acme alight strength variation from lot to lot, but far less than that obtained with the use of the acid-pasted counter parts. Borne hue variations from lot to lot were indicated. Six additional lots of crude violet solvent-milled in 1/3 gallon steel mills and converted to the BP-273-0 lakes showed greater strength variation than that exhibited by the glass-milled products, and also greater hue variations. The products, however, are all stronger than BP-273-0 and are consistently blue against this standard. There are indications that acid chromate treatment of the finished solvent-ground or acid-pasted (H-612) toner pulps yields a redder, more internee product. Likewise, the use of chromate, or a combination of chromate plus phosphate In the steel mill grind yielded redder products although the materials in these initial trials appeared weaker than corresponding products milled without chromate. All the products, however, are still blue against standard BP-273-0. Alkaline hypochlorite or alkaline peroxide treatment of the finished pulps did not give products comparable to those obtained by chromate treatment An ammonia wash after chromate treatment appears to offer some advantage. MILLIKG Salt-milling with either BaCl or $a$SO4 yielded products blue and weak against the solvent-milled counterparts. Dispersion milling with salt, "Percleme* and Span 80 yielded a product very blue and dull against the solvent-milled products and very blue against the salt-milled products. DUP050069335 -3- KH-53-18 HF>MILLIHG Acetone HF~ailling of "Lithosol*1 Violet 4BH crude using either borax or sodium chloride as a grinding medium yielded products essentially equal to those obtained by solvent-milling in acetone (see KH-52-13). A comprehensive weatheroaster exposure eeriee <300 hre*) designed to compare the relative behavior or acld~paated "Lithosol* Violet. H-612 (in the BP-I76-D formula) versus solvent-allied and HF-ailied "Lithosol" Violet (in theBF-273-D formula extended to equal the toner content of BP-176-D) indicates the essential equality of the variously finished violets with respect to change on exposure. Six plant lots of BP-176-D, standard BP-I76-D andBP-273-D, three solvent-allied lots and one HF-milled lot were used. A comparison of solvent-milled violet versus Orchem acidpasted material (N-612), the latter being a better* than average material of recent Orchem production, permits the following conclusions a. Regardless of the strength level and method of laking, the solvent-milled material results in a product of better strength by rubout than the acid-pasted product. b. Without exception, the use of ammonium rosinate in place of sodium rosinate (as in present BP-273-D) results in a product of better strength by rubout. c. A 50% "Bamapo" type lake reduced with blanc ftps to ABL-333-D gave better strength by Ford rubout than a 75% *Raraapo lake reducad with blanc fixe to an ABL-328-D type product, where the materials were prepared freo acid-pasted dye. However, there the corresponding materials were prepared from solvent-milled dye. no advantage was evident for the product of higher rosixistt ion * Alkyd evaluations of BP-273-D and ABL-333-D lakes indicate that greater strength may be realised by our testing method trm solvent-milledttLithosolrtViolet as against the acid-pasted Violet (N-612). Approximately four pounds of an FBP-273-D lake has been prepared in the Semi-works frSm bolvent-milled Violet for F & F*e examination. F & F, Phila., alkyd enamel evaluation of two experimental BP-273-D type lakes prepared from N-612 (Orchem acid-pasted Violet) and from Newark aolvent-oii:ied"lithosdl"Violet, resi indicated the latter to be bright and rad in tint (10/90 TiOg) 10$ strong versus the former. By actual analysis, the solvent-milled DUP050069336 KH-53-1S violet lake (F)BP-273~D let 2424, contains 69*311$ of violet toner# Whereas the acid-pasted violet lake* (BJBP-273-D, lot 2417 contains 70.89% of violet toner* An alkyd enamel w d from a BP-176-D type lake produced by adjusting a BP- l-B lake^(frcm solvent-ground violet) to the toner content of BP-1' B {12.8%) with blanc fixe wa* very strong against standard BP-3 Weatherometer exposure (336 hrs.) of a BP-273-D alkyd enamel prepared from solvent silled violet indicated the material to be very slightly inferior to standard BP-273-D and against a control* A 50% aluminum bensoate laks of either solvent-milled "Lithosol" Violet or its acid-pasted counterpart does not offer any advantage with respect to resistance to flocculation in alkyd enamel compared to standard BP-273-B* Ink mill evaluation of a BP-273-D lake prepared from solventmilled *lithosol* Violet Crude 48B showed a marked strength advat over the standard (42 parts * 100 parts) as Judged by the five-tJ inks. The solvent-milled product was vastly superior to the atm in rate of strength development and in the Beaman gauge texture rating# The product was bluer than the standard* Evaluation in alkyd enamel showed the product to be blue, dull, e* strong and essentially equal in bleed (baked white overaprxpe) The ink mill evaluation tabulated below indicates the texture obtained by the use of solvent-milled "Lithoaol" Violet crude versus standard 8P-273-B. At equal toner content, the solvent-allied product (FBF-273-0) returns greater strength than the acid-pasted counterpart (SBP-273-D). EBP-273-D FBP-273-B BP-273~D SB-241? SB-2424 SB-90870 n 7 $-3/2 rosinate 1 M Mm 7 7-1/2 7-1/2 6-1/2 , t ' 7 6--1/2 6-3/4 6-3/4 A plot of the rate of strength development verm time in three 58 gallon solvent mill grind* or "Lithosol* Violet 4RE crude indicates that standard strength (versus a -typical laboratory grind) was reached in approximately 4 hours, and maxi,mam strength (ca twice standard) in 24 hours* Maximum toner strength la reached in 12 hours DUP050069337 5 flHP'At in the 200 gallon mill, to operating difficultiesware encountered. She 93$ recovery yield reported was confirmed in the Semi~works in the solvent^milling operation. Typical barium rosinate "Bamapo" products prepared from the finished material compare favorably with the laboratory eolvent-ailled counterparts. The work summarised in this rspsrt is recorded in the following notebooks s HB-. jc DUP050069338