Patent GB-439114-A (GB)
Title: Improvement in vat dye compositions
IPC: D06P1/28
Filed: 1934-05-25
Abstract: Vat dyes, dyeing with; printing; dye preparations.--A dry solid vat dye composition comprises a vat dye compound and a soluble salt of an ester derived from an alcohol and an inorganic polybasic acid, e.g. sulphuric, phosphoric or boric acid, such ester consisting, on the one hand, of the inorganic acid residue containing at least one replaceable hydrogen atom and, on the other hand, of one or more hydrocarbon residues each containing, in the unsubstituted condition, a maximum of 5 carbon atoms.  A hydrocarbon residue may be substituted other than by an aliphatic hydrocarbon radicle.  The salts may be, for example, those of the alkali or alkaline earth metals, zinc, magnesium, ammonium, urea, guanidine, alkyl- or oxyalkyl-amines or pyridine and quaternary ammonium salts may also be used: The acid esters may be of the following types.  (a) alkyl esters of open-chain monohydric aliphatic alcohols, e.g. ethyl-, propyl-, butyl- or amylsulphuric acids and the corresponding mono- and di-alkyl-phosphoric acids; (b) alkyl esters of open-chain aliphatic polyhydric alcohols, e.g. glycol- or glycerol-sulphuric or phosphoric acids, di-glycol or di-glycerol-phosphoric acids and glycol- or glycerol-disulphuric, diphosphoric or triphosphoric acids; (c) alkyl, aralkyl or aryl ethers of the esters in (b), e.g. the ethyl isopropyl and butyl ethers of glycolsulphuric acid, diethylene glycol-disulphuric acid, alkyl ethers of diethylene glycol-sulphuric acid and the 4-methyl-2- nitrophenyl ether of glycol-sulphuric acid; (d) oxyalkylamine derivatives (cf. Specification 181,750, [Class 2 (iii)]), e.g. aminoalkyl-sulphuric acids, the acid sulphuric, phosphoric or boric esters of N-mono- or di(hydroxyethyl) - 2 - ethylcyclohexylamine, N - mono - or di - (hydroxylethyl)cyclohexylamine, N - hydroxyethyltetrahydronaphthylamine, N - hydroxyisopropyl - n - butylamine, the monohydroxyethyl ether of N-hydroxyethyl - di - n - butylamine, N - hydroxyethylcetylamine and N-hydroxyisopropylcyclohexylamine.  The vat dye, in aqueous dispersion, may be mixed with the acid ester salt and one or more diluents and/or assistants and the mixture be evaporated to a thick paste which is further evaporated to substantial dryness, e.g. on a rotary drum drier or is mixed with an anhydrous salt such as trisodium phosphate, sodium sulphate or sodium acetate. Specified dispersing agents are benzenesulphonic, phenolsulphonic, naphthalenesulphonic and naphtholsulphonic acids and their alkyl, aralkyl and hydrogenated derivatives, e.g. 1 : 7-, 2 : 6- and 2 : 8- naphthalenedisulphonic, isopropyl-, dibutyl-, amyl-, butylbenzyl-and cyclohexyl-naphthalenesulphonic acids, methylene-di-, acetal-di- and benzal-di-(b -naphthalenesulphonic) acids and methylene - di - (diisopropylnaphthalenesulphonic) acid; sulphite cellulose waste liquors; sulphonated resins; abietene-, abietine- and abietane-sulphonic acids; soaps; sulphonated higher fatty acids, fats and oils; sulphuric acid esters of hydroxy-fatty acid esters of monohydric alcohols.  Specified diluents are sucrose, cerelose, dextrin, glue, gelatin, gum arabic and urea.  Printing, including discharge or resist printing, preparations may contain also catalysts, reduction accelerators or enolyzing or hydrotropic agents, such as urea, thiourea, hexamethylenetetramine, potassium ethylsulphonate, potassium or sodium isovalerate, alkali metal salts of isobutyric, phenylacetic, benzoic, o - toluenecarboxylic, salicylic, benzenesulphonic, p - toluenesulphonic, benzenesulphinic, p - toluenesulphinic, naphthalenesulphonic, anilinesulphonic, 1 - aminonaphthalene - 3 : 6 : 8 - trisulphonic, picolinic and hydroaromatic carboxylic or sulphonic acids.  The vat dye may be present in the compositions in unreduced form, as the leuco compound or a salt thereof or as a soluble ester salt of the leuco compound. The following examples are specified:  (1) A 20 per cent indigo paste is stirred with Leukanol to a thin fluid, sucrose and sodium n-butylsulphate are stirred in and the mixture is evaporated to a thick paste which is placed in drying pans, evaporated to dryness, ground and screened; the product may be used directly in preparing an alkali-hydrosulphite vat.  (2) An 11 per cent paste of National vat orange R is mixed with Leukanol and sodium ethylsulphate and the mixture is evaporated to dryness, ground and screened; the product may be mixed with British gum, potassium carbonate, sodium formaldehydesulphoxylate, glycerol and water and the mixture printed on cotton.  (3) An 11 per cent paste of National vat orange R is mixed with Leukanol, sodium anthraquinone-2-sulphonate, sucrose, sodium isobutylsulphate and triamylamine and the mixture is evaporated to dryness, ground and screened; the product disperses readily in a printing paste.  (4) An 11 per cent paste of National vat orange R is mixed with Leukanol, potassium 2-carboxy-benzophenone-4<1>-sulphonate, sodium isobutylsulphate and dextrin and the mixture is evaporated to dryness, ground and screened; the product may be incorporated in a printing paste.  (5) A 15 per cent paste of National vat pink FF is mixed with Leukanol, sucrose and sodium isobutylsulphate, disodium glycerolmonophosphate or sodium glyceroldiphosphate and the mixture is evaporated to dryness, ground and screened; if the product is to be incorporated in a printing paste, ferrous sulphate and sufficient caustic soda to make the mixture slightly alkaline are preferably added before evaporation.  (6) A 20 per cent paste of 5 : 5<1>-dichlor-7 : 7<1>-dibrom-indigo is mixed with Leukanol, sodium isopropylsulphate and sucrose, gum arabic, dextrin or glue and the mixture is evaporated to dryness, ground and screened; the product may be incorporated in a printing paste.  (7) An 11 per cent paste of National carbanthrene violet 2R is mixed with Leukanol, sodium n-butylsulphate or the potassium salt of the sulphuric acid ester of dimethylethylcarbinol and sucrose or cerelose and the mixture is evaporated to dryness, ground and screened; the product may be incorporated in padding or printing preparations.  (8) An 11 per cent paste of National carbanthrene violet 2R is mixed with sodium isopropylsulphate and sucrose and the mixture is evaporated to dryness, ground and screened.  (9) An 18 per cent paste of National carbanthrene blue BCS is mixed with Leukanol, sucrose, dextrin and sodium secondary butylsulphate, the sodium salt of the sulphuric acid ester of N-cyclohexyldiethanolamine or the potassium salt of the sulphuric acid ester of dimethylethylcarbinol and the mixture is evaporated to dryness, ground and screened.  (10) A 16,5 per cent paste of National carbanthrene blue GCD is mixed with Leukanol, the sodium salt of the monoethyl ether of glycolsulphuric acid and urea, sucrose, dextrin or glue and the mixture is evaporated to dryness, ground and screened; hydrotropic agents and soluble salts of aminocarboxylic acids, e.g. sarcosine, may also be present in the mixture.  (11) A 23 per cent paste of National carbanthrene flavine GC is mixed with Leukanol, sucrose, the sodium salt of the sulphuric acid ester of secondary butylcarbinol and the disodium salt of 2 : 6-dioxyanthraquinone and the mixture is evaporated to dryness, ground and screened.  (12) A 21 per cent paste of National vat orange R, Leukanol and sodium isobutylsulphate are added to a mixture of an aqueous solution of sodium anthraquinone-2-sulphonate with dextrin and the mixture is evaporated to dryness, ground and screened; alkali metal phosphates, silicates, carbonates, sulphites, hydrosulphites or formaldehydesulphoxylates may also be incorporated in the mixture; the vat dye may be replaced by any of a large number of others specified.  (13) A 20 per cent indigo paste is mixed with Leukanol and sodium n-butylsulphate, the mixture is evaporated to a paste which is mixed with anhydrous trisodium phosphate and the mixture is ground and screened.  (14) A 10 per cent paste of National carbanthrene golden orange 2RT is mixed with Leukanol, sucrose and sodium isobutylsulphate and the mixture is evaporated to a paste which is mixed with anhydrous trisodium phosphate and the mixture is ground and screened.  (15) An 11 per cent paste of National vat orange R is mixed with Leukanol, sodium ethylsulphate, sodium anthraquinone-2-sulphonate and sucrose, the mixture is evaporated to a paste which is mixed with anhydrous trisodium phosphate and the product is ground and screened.  (16) The dry sodium salt of leuco-National vat orange R is mixed with Leukanol, sodium glycerolphosphate, sodium naphthalene-1-sulphonate and dextrin.  (17) The dry sodium salt of leuco-National vat orange.  R is mixed with Leukanol, an air-free aqueous solution of sodium isobutylsulphate, sodium naphthalene-1-sulphonate and dextrin and the mixture is evaporated to dryness, ground and screened; the product may be incorporated in a printing paste containing an alkali carbonate and sodium formaldehydesulphoxylate.  (18) A 20 per cent paste of indigo white is mixed with Leukanol and sodium n-butylaminoethylsulphate, the mixture is evaporated to a paste which is mixed with anhydrous trisodium phosphate and the product is ground and screened.  (19) A 25 per cent paste of the sodium salt of leuco National vat orange R is mixed with Leukanol, sodium naphthalene-1-sulphonate, sodium isobutylsulphate, water and anhydrous trisodium phosphate and the mixture is ground and screened; the product may be incorporated in a printing paste.  (20) The sodium salt of the sulphuric acid ester of leuco-dimethoxydibenzanthrone is mixed with dextrin and the sodium salt of the sulphuric acid ester of the 4-methyl-2-nitrophenyl ether of glycol, the mixture is dissolved in water and the solution is evaporated to dryness. (21) An aqueous solution of the sodium salt of the sulphuric acid ester of leuco-dimethoxydibenzanthrone, with an addition of the sodium salt of the su