Patent GB-762683-A (GB)
Title: A process for improving the resistance of wool and textile materials containing wool to felting and shrinkage in laundering
IPC: D06M15/55
Filed: 1954-01-19
Abstract: Textile materials containing wool are treated at pH 3-6 and a temperature of 30-100 DEG  C. with a dilute aqueous solution containing a water-soluble resinous intermediate obtained by reacting a neutral alkylene polyamine salt of a saturated aliphatic monocarboxylic acid of 2-5 carbon atoms with an aryl polyepoxy compound of the formula <FORM:0762683/IV(a)/1> where R and R1 are hydrogen or alkyl or phenyl radicals, X is hydrogen or a halogen atom, Z is the glycidyl ether group and n is 0, 1 or 2; the resin is cured upon the material and, at some stage prior to completion of the curing step, the material is additionally treated with formaldehyde, glyoxal,diglycidyl ether or ethylene glycol diglycidyl ether.  The latter compounds may be incorporated in the solution of the resin intermediate and the resin may be insolubilized by drying at 200 DEG to 300 DEG  F. or by treating the impregnated fabric at a pH of at least 8 in an aqueous solution containing an alkali metal or tertiary amine bicarbonate, carbonate or hydroxide, with or without formaldehyde, glyoxal, diglycidyl ether or ethylene glycol diglycidyl ether. The resinous intermediate may be obtained by reacting a diglycidyl ether of a dihydroxydiphenylmethylphenyl methane, dihydroxydiphenyldimethylmethane, dihydroxydiphenylmethylethylmethane, dihydroxydiphenylmethylpropyl methane, dihydroxydiphenylmethane, dihydroxydiphenylbutylphenylmethane, dihydroxydi - (chlorophenyl) methane or dihydroxydi - (chlorophenyl) dimethylmethane with the acetic, propionic, butyric or isovaleric acid salt of 1,2-diaminopropane, 1,3-diaminopropane or a member of the series H2N(CH2CH2NH)n where n is 1-50.  In examples, (1) phenol is reacted with formalin in the presence of hydrochloric acid at a pH below zero and temperature of 30 DEG  to 35 DEG  C., the resulting mixture of di-, tri- and tetraphenylol methanes is reacted with epichlorhydrin and aqueous caustic soda, excess epichlorhydrin is distilled off under vacuum at a temperature below 60 DEG  C. and the resulting ethers are separated as a viscou liquid, diluted with methanol and added to a boiling methanol solution of diethylene triamine triacetate, boiling being continued until an intermediate is obtained which will form a clear solution in ten volumes of water.  An aliphatic, saturated, monocarboxylic acid of 2-5 carbon atoms may be added as a stabilizer; (3) a methanol solution of a polyethyleneamine of the formula H(NHC2H4)nNH2 and M.W.1800 is neutralized with butyric acid and boiled with the mixed para- and orthoisomers of 1,1-bis-(1,2-epoxy-3-propoxyphenyl) butane, having an equivalent weight of 230 grams per epoxy group, until a solution miscible with ten times its weight of water is obtained, which is stabilized with butyric acid.ALSO:Wool-containing textile materials are treated at pH 3-6 and a temperature of 30 DEG -100 DEG C. with a dilute aqueous solution containing a water-soluble resinous intermediate obtained by reacting a neutral alkylene polyamine salt of a saturated aliphatic mono-carboxylic acid of 2-5 carbon atoms with an aryl polyepoxy compound of the formula <FORM:0762683/IV(b)/1> wherein R and R1 are hydrogen or alkyl or phenyl radicals, X is hydrogen or a halogen atom, Z is the glycidyl group and n is O, 1 or 2; the resin is cured in situ upon the material and, at some stage prior to completion of the curing, the material is treated with formaldehyde glyoxal, diglycidyl ether or ethylene glycol diglycidyl ether.  The formaldehyde, glyoxal or diglycidyl ether may be incorporated in the solution of the resin intermediate, and the resin may be insolubilized by drying at 200 DEG -300 DEG F. or by treating the impregnated fabric at a pH of at least 8 in an aqueous solution containing an alkali metal or tertiary amine bicarbonate, carbonate or hydroxide with or without formaldehyde, glyoxal, diglycidyl ether or ethylene glycol diglycidyl ether.  The materials may be wetted, prior to the treatment, with an aqueous solution at pH 3-6 containing a hydrogen halide or an aliphatic acid of 2-5 carbon atoms.  A wetting agent may be included in each solution.  The materials treated may be loose fibres, yarns, woven or knitted materials or piece goods of wool or mixtures of wool with cotton, nylon, polyacrylonitrile or acrylonitrile-vinyl chloride copolymer fibres. The resinous intermediate may be obtained by reacting a diglycidyl ether of a dihydroxydiphenylmethyl - phenylmethane, dihydroxydiphenylmethylethylmethane, dihydroxydiphenyl - dimethylmethane, dihydroxydiphenylmethylpropyl methane, dihydroxy-diphenylmethane, dihydroxydiphenylbutyl-phenylmethane, dihydroxydi(chlorophenyl) - methane or dihydroxydi(chlorophenyl) - dimethylmethane with the acetic, propionic, butyric or isovaleric acid salt of 1, 2 - diamino - pro - pane; 1, 3 - diamino propane or a member of the series H2N(CH2CH2NH)nH, where n is 1-50.  The pH of the resinous intermediate solution may be adjusted with a hydrogen halide or lower fatty acid.  After the resin is cured the material may be rinsed, dried without tension and finished by softening, steaming, napping or decatising.  In Example (5) wool-nylon shirting is rinsed with an aqueous solution of a non-ionic wetting agent and treated at 70 DEG C. in an aqueous solution at pH 5.2 containing the reaction prdouct of diethylene triamine triacetate and a mixed polyepoxypropyl ether of diphenylol-methane, formaldehyde and a non-ionic wetting agent.  After rinsing, the cloth is treated with a cold, aqueous solution containing sodium carbonate and formalin, rinsed, treated with a cold aqueous solution of sodium stearate, rinsed at pH 6 and dried.