Patent GB-636878-A (GB)
Title: Process of producing an aqueous dispersion for treating fibrous materials and the treatment of such materials therewith
IPC: D06M13/402
Filed: 1946-06-04
Abstract: A process for treating fibrous materials to impart water-repellant properties thereto comprises wetting or impregnating them with an aqueous dispersion comprising (a) an N,N1-diacyldiamino-methane in which the acyl groups are derived from aliphatic acids containing 12 to 28 carbon atoms; (b) dimethylol urea, a dimethylol urea ether, tetramethylol melamine, or a tetramethylol melamine ether, and (c) a dispersing agent, and thereafter drying and heating the material. Suitable diacyl compounds are those in which the acyl groups are stearoyl, oleyoyl, or montanoyl, or are derived from technical lauric, palmitic, or stearic acid.  The methylol-urea- or melamine-ethers are those of saturated aliphatic alcohols of one to six carbon atoms.  The treatment may be applied to cotton, linen, wool, jute, wood, paper, artificial silk, or fibres and textiles of polyamides, polyvinyl acetals, polyethylene or vinyl chloride-vinyl acetate copolymers.  Preferably the dibutyl ether of tetramethylol melamine is used.  Crystalline tetramethylol melamine is obtained by heating 1 mole of melamine, 4 moles formalin, and an alkaline buffer at a pH of 9.5 and 80 DEG  C. until a clear solution results.  This is then cooled slowly, and crystals of the product washed with alcohol.  It is then etherified by mixing with butanol, heating to 45 DEG  C., adding phosphoric acid, and heating to 50 DEG  C.  After reaction, the acid is neutralized, the solution cooled and inorganic salts filtered off from the butanol solution.  Dispersing agents specified are ammonium oleate, triethanolamine oleate, or 2 - amino - 2 - methyl - 1 - propanol oleate or stearate or a salt of a fatty acid having 12 to 20 carbon atoms with ammonia sufficient to give the dispersion a pH between 9 and 10.  When the dispersion contains sufficient ammonia or other fugitive base to make the dispersion of pH 9.0 to 10.0, and the dispersed diacyl diamino methane and amine-aldehyde condensate are of particle size between 0.5 to 10.0 microns the dispersion is stable up to 80 DEG  C.  It is applied to the fibre in a jig or padder or by spraying, and the fibre, after drying, is heated to 100-175 DEG  C. which further polymerizes the resin until it is insoluble in hydrocarbons.  In examples: (1) a fatty acid (molten if necessary) is added to water, ammonia is added, and the mixture passes through a colloid mill.  Finely powdered N,N1-distearoyldiaminomethane and then tetramethylolmelamine di-butyl ether in hydrocarbon solution are added and the mixture again passed through a colloid mill.  As prepared the suspension contains 15 to 47 per cent of solids and for use is diluted to 1 to 10 per cent; (2) the procedure of example (1) is followed, molten paraffin wax being incorporated by melting with the diamide, the fatty acid being stearic or oleic; the product is suitable for outdoor textiles where the fabric is not to be washed with soap; (3) the procedure of example (1) is followed, and aluminium stearate is included in the mixture.  Permanent water repellency results on heating at 120 DEG or 130 DEG  C.  Testing for water-repellency of the treated fabrics in examples; (4) strips of Indian Head cloth are passed through the dispersion prepared according to example (2), of 2.5 and 10 per cent solids respectively, followed by air drying and baking at 150 DEG  C. The cloth was also tested after standard laundering and dry-cleaning processes; (5) cloth is treated in a dispersion of water, triethanoalmine oleate, paraffin wax, N,N1-distearoyldiaminomethane and a butanol solution of di-butylether of tetramethylolmelamine, and dried, baked and laundered as in example (4); (6) 2-amino-2-methyl-1-propanol oleate is substituted for the triethanolamine oleate of example 5 and cloth passed through a 30 per cent dispersion is baked, and laundered, as in example (4); (7) a dispersion is prepared by the procedure of example 1 of oleic acid, ammonia, water, paraffin wax, N,N1-distearoyldiamino methane, mineral spirits and a solution of a tetramethylol melamine condensation product dissolved in butanol and xylol.  Cloth was treated, dried, baked, and laundered as in example (4); (8) the procedure of example (7) was employed, substituting a dimethylol-urea condensate for the melamine-formaldehyde resin.  The process is applicable to treating linen, wool, jute, wood, artificial silk, and synthetic fibres such as polyamides, polyvinyl acetols, polyethylenes, and copolymers of vinyl chloride with vinyl acetate.  The products may be prepared as a dry powdered mixture of wax, diamide and resin, or may have a dispersion agent in dry form mixed with it, or a mixture of wax, diamide and resin may be treated with solutions of the dispersing agent, and dried to obtain a powder. Other suitable diacyl derivatives of diamino methane include those from oleic and montanic acids, or from technical lauric, palmitic, or stearic acids. Specifications 495,714, 501,288, 506,721, 537,971 and 543,360 are referred to.