Patent GB-1071528-A (GB)
Title: Method of bonding olefin copolymers to fibres
IPC: C09J123/34
Filed: 1964-11-05
Abstract: A composition used in bonding natural and synthetic fibres to elastomeric saturated amorphous ethylene-alpha-olefine copolymers comprises an aqueous dispersion of a phenolaldehyde resin and of a chlorosulphonated ethylene-alpha-olefine copolymer containing a non-ionic surface active agent and an amonic surface active agent which has been adjusted to a pH of 7-8 after a maturing period of 4-80 hours.  The composition may be prepared by mixing while agitating a hydrocarbon solvent solution containing 1-30% by weight of the chlorosulphonated copolymer with a solution in the same volume of water of a mixture of a nonionic surface active agent and an anionic surface active agent, adding a thickening agent, e.g. carboxymethylcellulose, to produce a skimming or enriched emulsion containing 1/2 to 2/3 of the original emulsifiers which is separated from the aqueous layer, separating the solvent from the enriched emulsion by distillation in a current of superheated steam, further concentrating the emulsion by evaporation of water up to a solid content of 20-30% by weight, adding the condensation product of the phenol, e.g. resorcinol, and formaldehyde or the phenol and formaldehyde together with a small amount of alkali to catalyse the condensation, to the emulsion and the adjusting the pH to 7-8 after a maturing period of 40-80 hours.  The nonionic surface active agent may be a polyoxyethylated alkyl phenol produced from one mole of an alkyl phenol having an aliphatic chain containing 6-10 carbon atoms or a polyoxyethylated alcohol having the formula R(OCHR1CHR1)nOH in which R is an alkyl group, R1 is a hydrogen atom or alkyl group and n is an integer of 4-10 and the anionic surface active agent may be sodium lauryl sulphate, a sodium salt of a polyoxyethylated phenol sulphate or sodium or potassium oleate, palmitate or stearate.  The hydrocarbon solvent for the chlorosulphonated copolymer may be pentane, hexane, heptane, benzene or toluene and boric acid and caustic soda which produce a mixture of boric acid and sodium borate may be added to buffer the composition to a pH of 7-8.  The copolymers may be obtained by chlorosulphonating ethylene-alpha-olefine copolymers with gaseous mixtures of SO2 and chlorine, with chlorosulphonic acid or with sulphuryl chloride.ALSO:Natural and synthetic fibres and articles made therefrom, e.g viscose rayon, nylon and cotton fabrics, are bonded to elastomeric saturated amorphous ethylene/alpha-olefin copolymers by treating them with an aqueous dispersion of a phenol-aldehyde resin and of a chlorosulphonated ethylene-alpha-olefin copolymer containing a non-ionic surface active agent and an anionic surface-active agent, the pH of this resin-latex dispersion being adjusted to 7-8 after a maturing period of from 40-80 hours, applying to them a layer of a mix containing an ethylene/alpha olefin copolymer, a reinforcing filler and a vulcanization agent and then vulcanizing by heating to from 110 DEG  to 220 DEG C.  The treating composition may be prepared by mixing while agitating a hydrocarbon solvent solution containing 1-30% by weight of the chlorosulphonated copolymer with a solution in the same volume of water of a mixture of a non-ionic surface active agent and an anionic surface active agent, adding a thickening agent, e.g. carboxymethylcellulose, to produce a skimming or enriched emulsion containing 1/2 to 2/3 of the original emulsifiers which is separated from the aqueous layer, separating the solvent from the enriched emulsion by distillation in a current of super heated steam, further concentrating the emulsion by evaporation of water up to a solid content of 20-30% by weight, adding the condensation product of the phenol e.g. resorcinol, and formaldehyde or the phenol and formaldehyde together with a small amount of alkali to catalyse the condensation, to the emulsion and then adjusting the pH to 7-8 after a maturing period of 40-80 hours.  The non-ionic surface active agent may be a polyoxyethylated alkylphenol produced from one mol of an alkylphenol having an aliphatic chain containing 6-10 carbon atoms or a polyoxyethylated alcohol having the formula R(OCHR\sv CHR\sv)nOH in which R is an alkyl group, R\sv is a hydrogen atom or alkyl group and n is an integer of 4-10 and the anionic surface active agent may be sodium lauryl sulphate, a sodium salt of a polyoxyethylated phenol sulphate or sodium or potassium oleate, palmitate or stearate.  The hydrocarbon solvent for the chlorosulphonated copolymer may be pentane, hexane, heptane, benzene or toluene and boric acid and caustic soda which produce a mixture of boric acid and sodium borate may be added to the treating composition to buffer to pH to between 7 and 8.  The aqueous dispersion may be applied to the fibres or articles by immersion, spreading or frictioning, dried and the ethylene/alpha olefin copolymer which may contain as vulcanising agents organic peroxides and sulphur, as reinforcing fillers carbon black or mineral fillers, and possibly other additives, applied and vulcanized.ALSO:Fabrics made from natural or synthetic fibres, e.g. viscose rayon, nylon and cotton, are bonded to elastomeric saturated amorphous ethylene/alpha-olefin copolymers by treating them with an aqueous dispersion of a phenolaldehyde resin and of a chlorosulphonated ehtylene-alpha-olefin copolymer containing a non-ionic surface active agent and an anionic surface-active agent, the pH of this resin-latex dispersion being adjusted to 7-8 after a maturing period of from 40-80 hours, applying to them a layer of a mix containing an ethylene/alpha olefin copolymer, a reinforcing filler and a vulcanization agent and then vulcanizing by heating to from 110 DEG  to 220 DEG C.  The treating composition may be prepared by mixing while agitating a hydrocarbon solvent solution containing 1-30% by weight of the chlorosulphonated copolymer with a solution in the same volume of water of a mixture of a non-ionic surface active agent and an anionic surface active agent, adding a thickening agent, e.g. carboxymethylcellulose, to produce a skimming or enriched emulsion containing 1/2 to 2/3 of the original emulsifiers which is separated from the aqueous layer, separating the solvent from the enriched emulsion by distillation in a current of super heated steam, further concentrating the emulsion by evaporation of water up to a solid content of 20-30% by weight, adding the condensation product of the phenol e.g. resorcinol and formaldehyde or, the phenol and formaldehyde together with a small amount of alkali to catalyse the condensation, to the emulsion and then adjusting the pH to 7-8 after a maturing period of 40-80 hours.  The non-ionic surface active agent may be a polyoxyethylated alkylphenol produced from one mol of an alkylphenol having an aliphatic chain containing 6-10 carbon atoms or a polyoxyethylated alcohol having the formula R(OCHR'CHR')nOH in which R is an alkyl group, R' is a hydrogen atom or alkyl group and n is an integer of 4-10 and the anionic surface active agent may be sodium lauryl sulphate, a sodium salt of a polyoxyethylated phenol sulphate or sodium or potassium oleate, palmitate or stearate.  The hydrocarbon solvent for the chlorosulphonated copolymer may be pentane, hexane, heptane, benzene or toluene and boric acid and caustic soda which produce a mixture of boric acid and sodium borate may be added to the treating composition to buffer to pH to between 7 and 8.  The aqueous dispersion may be applied to the fabrics by immersion, spreading or frictioning, dried and the ethylene/alpha olefin copolymer which may contain as vulcanising agents organic peroxides and sulphur, as reinforcing fillers carbon black or mineral fillers, and possibly other additives applied and vulcanized.