Document zdD1NmEgXpG6Jz95QLVJZOopn

E. I. DU PONT DE NEMOURS & COMPANY PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY it Copy No. 1 Numerical File jL-.-J-->iv \"m V 1 Period Covered t NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Progress Report DIRECT LAKING FORMULA FOR RT-499-D (M TONER OF LITHOSOL RUBINS 3G ) JANUARY 12, 1946 to JULY 29, 1946c FILE: DATE: 222e23 8/8/46 N39973 Serial No. KN-46-5? Copy No. 1 Copy to* #1 - Numerical File 2 - Research Office (222.23) 3 - Library File (222.23) 4 - #10 Building File 5-# 6 * 6 - Imperial n Chemical n Indusiitries, Ltd. it n n it 9 - W. F. Spengeman NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Progress Report DIRECT LAKING FORMULA FOR RT-499-D (Mn TONES OF LITHOSOL RUBINS 30) JANUARY 12, 1946 to JULY 29, 1946. DATE SUBMITTED* 8/2/46 DATE ISSUED* 8/8/46 N39973.01 DUP050150186 A direct laking formula for the manganese toner of lithosol Rubine 30 was developed in 1945 (XH-45-39) and was coded RT-533-D. This product received a treatment to Improve its baking qualities, glycerol being mixed into the press cake prior to drying. As a result of the method of manufacture, RI-533-D is lighter in full shade enamel than RT-499-D, the original code for this Mn toner. Because of continued interest of Pdf, Phila. in the latter, work was undertaken to improve the depth of the product which is obtained by the straight through process. M^L^SQMCLS.iogB At the present stage of the problem, it is not possible to increase the depth to equal RT-499-D by application of the usual variables such as temperature and time of development although these are effective in developing strength. A product close to RT-499-D in enamel masstone was obtained by use of higher alkalinity of development but tinting strength was abnormally low. A formula, K-2334, was developed using sodium bisulfite in the BOH solution preceding the addition of manganese sulfate. The action of the sulfite is not clear but may be ascribed to prevention of oxidation of the manganous hydrate. The product obtained was equal to RT-499-D in depth but slightly duller. Strength was greater. A semi-works trial of this formula gave similar results. The dullness appears to be greater than could be accepted in a passable match for standard. A number of intermediates were tested for their effect as accessory first components. Of these naphthylamine sulfonic acids such as ortho naphthlonle and LaurentSs acid were effective in pro ducing darker masstone as rated by rubeut. However, in enamel grinds an objectionable degree of dullness occurred. H Acid gave similar results. Depth and strength were also Improved by use of 4-chlor-2-amino anisole but baking and bleed resistance were adversely effected. It is planned to continue work on the direct laking formula. In the early stages of the study, all products were characterised by extremely low tinting strength, compared to the current RT-499-D standard. In full shade enamels, they were very close to the latter. While the importance of strength in an enamel color was uncertain, control of this property was considered desirable and was accomplished by reduction in alkalinity of develop ment accompanied by use of a slightly higher temperature. This had the effect of lightening the masstone to a slight extent. A longer development period also tended to give stronger products. Variations in strength were not eliminated by these changes but were greatly reduced. DUP050150187 The folio-wing variables were also studied, Reduction In amount of manganese sulfate may possibly be made to the extent of 20 to 40% but results were Inconclusive due to weakness of the control. Addition of all the MnSO. to the BOH solution showed a slight advantage over other points of addition. Stirring the BOH - MnSO. for longer than 5 minutes showed no advantage but a shorter period appeared to cause weakness* During the stirring period, the slurry usually becomes greenish gray in color. This change is difficult to control and appears to have an effect on the strength. It is accelerated by the presence of sodium sulfite, the use of which is discussed above. Sodium sulfite or bisulfite increased.tinting strength in proportion to theamount used (within the limits of the experiment), added to depth in enamel but as previously stated caused some dullness. The optimum amount appears to be 30# HagSO^ per mol coupling. Sodium acetate added to the BOH solution preceding the manganese sulfate also gave strong products with slight dullness. The presence of Para Soap in the coupling had very little effect but use of larger amounts might be worth investigating. Stirring the coupled seda salt for two hours resulted in a darker product in one experiment but could not be duplicated. The following intermediates were tried for possible use as accessory compounds in addition to these referred to above. Para toluidlne raeta sulfonic acid. Para toluidlne ortho sulfonic acid Ortho toluidlne meta sulfonic acid 6-chlor-2-smlno toluene 4-chlor-2-amin toluene 6-chlor-3-amino toluene-2-sulfonic acid 6-ohlor-2-aaino toluene-3-sulfonic acid 6-ehlor-2-amlno toluene-5-stilfonie acid 4-chlor-2-amino anlsole >-nitro-2-amine anlsole Para anisidine ortho sulfonic acid Tobias Acid DUP050150188 -3- go^S9.m..lia8..flMa3g.4 1188-32 34 37 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 Variations of RT-533-D formula* Ac id! type coupling Reduction in amount of MnSO^ pH and temperature of development RT-533-D* Effect of glycerol treatment pH of development Repeat Bxp. 41 Use of Para Soap and sodium acetate in coupling Oxidizing and reducing salts in BON solution* Vary time of stirring after coupling Point of addition of MnS04 Amount of sodium sulfite in BON soludion Amount of alkali used with sodium bisulfite Treatment with Resinous oil, naphthenic acid and sodium restnate RT-499-D. Test Lithosol Rubine 30 dye* Accessory first components PTOSA, PTMSA, OTMSA Accessory first components PCAOSA, Red 2B acid and Lake Red C base. Amount of Lake Red C base used* Time and temperature of development Repeat Exp. 51 with longer development time Time of stirring BON - M11S94 suspension 1224-4 >6 7 8 9 10 12 Vary proportion of MnSO. added to BON Reoheck time of stirring after coupling. Amount of alkali for development Accessory first components - chlor amino toluene sulfonic acids Chlor amino toluenes and anisole as accessory intermediates Miscellaneous accessory components O-naphthlonlc acid, Laurent's acid, H acid* 7\ DUP050150189