Patent GB-607085-A (GB)
Title: Improvements in or relating to cellulose ester or ether fibres
IPC: D06P1/642
Filed: 1946-01-25
Abstract: A non-crystalline water-insoluble alkylated condensation product of an aldehyde with an amino triazine or with an amino-diazine is incorporated into cellulose ester or ether fibres, either by treatment of the formed fibres so as to obtain intimate mixing of the condensation product with the cellulose derivative of the fibres, or by incorporation in the composition from which the fibres are made. The fibres containing the alkylated condensation product may be dyed and such dyed products have great resistance to change of shade and fading on exposure to atmospheres containing combustion products of coal gas. Alkylated products of formaldehyde and melamine may be used, or similar products derived from formoguanamine or aceto - guanamine, i.e. 2 : 4-diamino-triazine and 2 : 4-diamino-6-methyl-triazine, or from 2 : 4 : 6-triamino-pyrimidine. Formaldehyde may be caused to react on melamine to form a water-soluble product which is then subjected to the action of ethyl or other alcohol, preferably in presence of hydrochloric or other mineral acid.  The product may be soluble in acetone, ethyl alcohol, or benzene, but insoluble in water. Alternatively, a water-insoluble non-crystalline resinous melamine formaldehyde product may be prepared and then allowed to react with an alcohol.  An alkylated condensation product may also be obtained by the joint action of formaldehyde and an alcohol on melamine.  The ratio of formaldehyde to melamine may range from 3 to 6 or more molecular proportions of formaldehyde for each molecular proportion of melamine.  Alkylation may be effected with aqueous alcohol.  For the alkylation there may be used ethyl, propyl, butyl or benzyl alcohol.  Acetaldehyde may be used instead of formaldehyde.  When the products are applied to the formed fibres, solutions in organic solvents, e.g. alcohols, may be used.  Dyeing may be effected in customary manner from aqueous baths or with the aid of solutions of the dyes in organic liquids. The dyes employed may be of the class of 1-amino - 4 - hydroxy - anthraquinone and 1 : 4-diamino-anthraquinone and their nuclear and N-substitution products.  In an example, 126 grams melamine are heated 10 minutes at 90 DEG  C. with 630 c.c. aqueous formaldehyde of 40 per cent strength.  After cooling to 70 DEG  C. an equal volume of methylated spirit is added.  Upon further cooling, hexamethylol melamine separates.  This product is mixed with 630 c.c. methylated spirit containing 12 c.c. concentrated hydrochloric acid and stirred till solution is obtained.  The solution is neutralized and the product is extracted with benzene which is then distilled off leaving a clear viscous liquid.  The product is incorporated in a cellulose acetate spinning solution to the extent of about 5 per cent based on the weight of cellulose acetate.  The solution is formed into filaments by dry spinning. Knitted fabric made from the yarn so obtained is dyed with 1-methyl-amino - 4 -(beta - hydroxy - ethylamino) - anthraquinone.  In another example, melamine (1 mol.) and aqueous formaldehyde (3 mols.) at pH 8 are mixed together and the temperature is raised to 70-75 DEG  C.  The ensuing reaction raises the temperature to about 90 DEG  C.  When the reaction mixture has cooled, the product separates as a white solid.  Methylated spirits and hydrochloric acid are added, and the white solid dissolves.  The solution is neutralized, filtered and then distilled under reduced pressure, leaving an ethylated melamine formaldehyde condensation product.  The product is added to a cellulose acetate spinning solution.  Knitted fabric made of yarn produced from the solution is dyed from a bath made by dispersing an aqueous paste of 1-amino-4-cyclohexylaminoanthraquinone-2-carboxyamide with turkey red oil, diluting with a boiling soap solution, and adding the mixture to a soap solution.  Specification 569,557 is referred to.ALSO:A non-crystalline water-insoluble alkylated condensation product of an aldehyde with an amino triazine or with an amino-diazine is incorporated into cellulose ester or ether fibres either by treatment of the formed fibres so as to obtain intimate mixing of the condensation product with the cellulose derivative of the fibres, or by incorporation in the composition from which the fibres are made. The fibres containing the alkylated condensation product may be dyed and such dyed products have great resistance to change of shade and fading on exposure to atmospheres containing combustion products of coal gas. Alkylated products of formaldehyde and melamine may be used, or similar products derived from formoguanamine or aceto-guanamine, i.e. 2 : 4-diamino-triazine and 2 : 4-diamino-6-methyl-triazine, or from 2 : 4 : 6-triamino-pyrimidine. When the products are applied to the formed fibres, solutions in organic solvents, e.g. alcohols, may be used.  Dyeing may be effected in customary manner from aqueous baths or with the aid of solutions of the dyes in organic liquids.  The dyes employed may be of the class of 1-amino-4-hydroxy-anthraquinone and 1 : 4-diamino-anthraquinone and their nuclear and N-substitution products.  In an example, melamine is heated with aqueous formaldehyde of 40 per cent strength.  After cooling to 70 DEG  C. an equal volume of methylated spirit is added.  Upon further cooling, hexamethylol melamine separates.  This product is mixed with methylated spirit containing hydrochloric acid and stirred till solution is obtained.  The solution is neutralized and the product is extracted with benzene which is then distilled off leaving a clear viscous liquid.  The product is incorporated in a cellulose acetate spinning solution to the extent of about 5 per cent based on the weight of cellulose acetate.  The solution is formed into filaments by dry spinning.  Knitted fabric made from the yarn so obtained is dyed with 1-methylamino - 4 - (beta - hydroxy - ethylamino) - anthra - quinone.  In another example, an ethylated melamine formaldehyde condensation product is added to a cellulose acetate spinning solution.  Knitted fabric made of yarn produced from the solution is dyed from a bath made by dispersing an aqueous paste of 1-amino-4-cyclohexyl - amino - anthraquinone - 2 - carboxy - amide with turkey red oil diluting with a boiling soap solution, and adding the mixture to a soap solution. Specification 569,557 is referred to.