Patent GB-487275-A (GB)
Title: Process for producing coloured spinning masses and shaped materials prepared therefrom
IPC: D01F1/10
Filed: 1937-04-09
Abstract: The Specification as open to inspection under Sect. 91 includes the colouring of masses having a basis of wax, e.g. carnauba wax or ozokerite by incorporating therein the reaction product of a dyestuff containing at least one hydroxyl group on an esterifying agent, the dyestuff being subsequently regenerated by saponification.  This subject-matter does not appear in the Specification as accepted.ALSO:In a process for producing coloured spinning masses there is incorporated into the mass the reaction product of a dyestuff containing at, least one hydroxyl group on an esterifying agent, and the parent dyestuff is regenerated by a saponification process at any time before, during or after the working up of the spinning mass.  The process is particularly useful for insoluble or sparingly soluble dyestuffs with soluble esters.  For such products esterifying agents may be used containing at least one constituent that enhances the solubility of the dyestuff, e.g. halides or anhydrides of aliphatic, hydroaromatic or aromatic carboxylic acids containing sulpho, carboxyl or alkylamino groups. Such products may be converted to alkali metal or quaternary ammonium compounds.  The esterification may be effected in presence of a tertiary base, e.g. dialkylaminobenzene, pyridine or quinoline with an esterifying agent containing a substituent having no esterifying action but capable of reacting with the base to enhance the solubility of the dyestuff in water or organic solvents.  Suitable agents are halides of sulpho-carboxylic acids, the dialkylamino-1-benzoyl halides, the 4-halogen-alkyl-1-benzoyl halides, or halogen sulphonic acids, their esters and amides. Suitable reaction products are described in Specifications 480,358 and 10146/37.  The spinning masses may have basis of cellulose, of cellulose esters or ethers, or of vinyl resin or casein. Particularly suitable are solutions in water, alcohol, glycol, a ketone, an ether, ether alcohol, ester or a mixture of solvents such as are usual for cellulose lacquers.  A solution of the reaction product may be mixed with the spinning solution or the reaction product itself may be combined with the spinning mass, e.g. with grinding.  Suitable additions to the spinning mass are a fatty acid of high molecular weight, a filler such as barium sulphate, zinc oxide, titanium oxide, and a softening or plasticizing agent, e.g. triphenyl or tricresyl phosphate, glycerine or castor oil.  Suitable saponifying agents to regenerate the dyestuff before, during, or after the working up of the spinning mass to its desired form, e.g. threads or films, are alkalies or alkaline salts or in some cases, e.g. with the reaction products described in Specifications 10146/37 and 10147/37, acids such as acetic, formic or dilute sulphuric may be used.  The spinning mass may itself saponify the reaction product. Examples are: (1) to a solution of acetyl cellulose in acetone and methyl alcohol is introduced the product of reaction of meta benzoic acid sulpho-chloride on the azo dyestuff from diazotized 2.5-dichloroaniline and 2.3-oxynaphthoic acid-o-anisidide dissolved in methyl alcohol.  The solution is worked up to threads or films which are then treated with dilute ammonia solution to regenerate the dyestuff; (2) the reaction product of benzoic acid 3.5-disulpho-chloride on the azo dye from diazotized 4.41 - diamino - 3.31 - dimethoxydiphenyl and 2-oxynaphthalene dissolved in ethyl alcohol is used with an acetyl cellulose spinning solution; (3) the reaction product of meta sulphobenzoic acid chloride on the azo dye from diazotized 2-aminonaphthalene and 2.3-oxynaphthoic acid anilide dissolved in alcohol is used; (4) a film is made from a solution containing nitrocellulose, ether, methyl alcohol, amyl alcohol, camphor, and the reaction product of benzoic acid meta-disulphochloride on the azo dye from diazotized 1-amino-2-methoxy-azobenzene and 2-oxy-naphthalene. The colour is developed with ammonia; (5) the reaction product of benzoic acid m.disulphochloride on the azo dye from diazotized 4.41-diamino-3.31-dimethoxy-diphenyl and 2-oxynaphthalene is added to a viscose spinning solution.  The dyestuff develops in the spinning mass.  The Specification as open to inspection under Sect. 91 includes the production of coloured masses generally by the method of the invention.  It includes lacquers with a cellulosic basis, or masses derived from natural resins such as copal, amber, shellac, colophony or waxes such as carnauba and ozokerite, or natural polymerization products such as rubber, balata or guttapercha, or from artificial resins such as those from aldehydes and phenols, aldehydes and aromatic amines, aldehydes and acid amides, polybasic acids and polybasic alcohols or vinyl resins, styrene resins or acrylic acid resins.  This subject-matter does not appear in the Specification as accepted.ALSO:The Specification as open to inspection under Sect. 91 includes the colouring of masses having a basis of rubber, balata or guttapercha by incorporating therein the reaction product of a dyestuff containing at least one hydroxyl group with an esterifying agent, the dyestuff being subsequently regenerated by saponification.  This subject-matter does not appear in the Specification as accepted.