Patent GB-780967-A (GB)
Title: Process for rendering fibrous material water-repellent
IPC: D06M13/51
Filed: 1953-10-19
Abstract: 780,967. Waterproofing and fireproofing fabrics. FARBWERKE HOECHST AKT.- GES. VORM. MEISTER, LUCIUS & BRUNING. Oct. 19, 1953 [Oct. 18, 1952], No. 28834/53. Class 140. Fibrous material is rendered water-repellent by treatment with a solution in an organic solvent, said solution comprising a solid or semi-solid paraffin hydrocarbon, a natural or synthetic wax or a thick oily to solid polychlorinated hydrocarbon, singly or in admixture, together with a carboxylic or sulphinic acid and a zirconium alcoholate or a mixture of a zirconium alcoholate and an aluminium alcoholate, or together with a reaction product of a carboxylic or sulphinic acid with a zirconium alcoholate or a zirconium alcoholate and an aluminium alcoholate. The treated fibrous material may be heated at a temperature above 80‹ C. Specified alcoholates are those of methyl, ethyl, isopropyl, butyl, amyl and octyl alcohols. Specified acids include formic, acetic, propionic, oleic, lauric, palmitic and stearic acids, cyclohexane carboxylic acid, benzoic acid, o-, m- and p-chlorobenzoic acid, naphthoic acid, and fatty acids and mixtures thereof obtained by oxidation of naturally occurring organic substances, naphthenic acid, resinic acid, montanic acid, sperm oil fatty acid, ethane, . butane, cyclohexane, benzene and naphthalene sulphinic acids and sulphinic acids obtained from the sulphochlorination products of natural and synthetic Diesel oils. Solid or semi-solid paraffin hydrocarbons include paraffin waxes, synthetic high molecular weight paraffin hydrocarbons, ceresine and paraffin slack wax. Natural or synthetic waxes include carnauba wax, candelilla wax, esters of montanic acids with polyhydric alcohols and higher fatty alcohol esters of C 10  and higher fatty acids. Thick oily to solid polychlorinated hydrocarbons include the chlorination products of natural or synthetic aliphatic hydrocarbon oils of B.P. between 200‹ and 400‹ C., of solid paraffin hydrocarbons of M.P. between 50-100‹. C. and of paraffin slack waxes, and of aromatic hydrocarbons such as naphthalene. When these polychlorinated products are used in the absence of paraffins and waxes the fabrics are flame-proofed. The zirconium alcohol-carboxylic acid condensate may be stabilized by the addition of an aliphatic compound containing a hydroxyl group or a group capable of desmotropic rearrangement into an aci-form such as diethyl tartrate and other hydroxy carboxylic acid esters, oximes such as acetoxime or acetaldoxime, acetylacetone, acetoacetic ester, malonic acid dinitrile, nitromethane, nitropropane, malonic acid ester, and butyroin. Organic solvents such as benzine, benzene, carbon tetrachloride, trichlorethylene, and perchlorethylene may be used. The process of the invention is applicable to fibrous materials of cotton, linen, viscose, cuprammonium, wool, silk, casein, cellulose acetate, polyamides, polyacrylonitrile and polyesters, either before or after working up. In an example cotton poplin jackets are impregnated with a solution in carbon tetrachloride of the condensation product of zirconium ethylate and stearic acid stabilized by acetonylacetone and containing paraffin wax, and then dried at 90 ‹ C.