Patent GB-759158-A (GB)
Title: Method of fulling fabrics composed of or containing a substantial proportion of wool
IPC: D06M13/52
Filed: 1953-07-27
Abstract: Textile materials comprising at least 20 per cent. of wool are fulled in an acid aqueous colloidal dispersion of a carboxylic acid containing at least 6 carbon atoms in the molecule and an ester of ortho-phosphoric acid which has at least one hydrocarbon or substituted hydrocarbon radical containing at least 6 carbon atoms. The acid and the ester may be added together to the fulling bath or may be used together as a spinning lubricant in a composition which may also comprise a mineral oil or a fatty oil, the composition being allowed to remain upon the fibres and being carried thereby to the fulling bath, which then contains water only, or the acid may be used as a spinning lubricant or in a spinning lubricating composition and may be carried thereby to the fulling bath, which then comprises an aqueous solution of the ortho-phosphoric acid ester.  After fulling, the acid is neutralized with soda or ammonium and is washed out.  The acid may also be neutralized during the fulling operation and the operation completed under alkaline conditions, or the fulling may be commenced under alkaline conditions and completed under acid conditions.  The acid may be caprylic acid; lauric acid; stearic acid; oleic acid; ricinoleic acid; chlorostearic acid; mixtures of these acids; the acid mixtures obtained by splitting peanut oil or soya-bean oil; benzoic acid; phenyl-acetic acid; salicylic acid; benzoylacetic acid; dioxybenzoic acid or mixtures of these aromatic acids with the above aliphatic acids; the oleic acid ester of p-oxybenzoic acid or of glycolic, lactic, tartaric or gluconic acid; oleylglycocoll; oleylaminobenzoic acid or fatty acid condensation products with amino-acids from decomposed albumen.  The phosphoric acid ester may be a neutral water-soluble alkali metal, ammonium or alkylolamine salt of a primary or secondary ester of orthophosphoric acid with a fatty alcohol containing at least 6 carbon atoms in the molecule or with the corresponding fatty acid, fatty acid amide or fatty acid mercaptan which has been substituted by a glycol or polyglycol group, or with sorbitol or polyglycerine; an ester obtained by directly esterifying phenol, cresol, butylcresol, octylphenol, dodecylphenol or cyclohexanol, either as such or as a polyglycol ether, with orthophosphoric acid; a neutral ester produced by afteresterifying a tertiary oxyalkylphosphate with lauric, stearic, oleic or ricinoleic acid; a polycondensed tertiary oxyalkylphosphate or a mixture of two or more of these esters. The fulling bath may also include a neutralized cellulose ether carboxylic acid or cellulose sulphonic acid or cellulose or starch solubilized by the introduction of a polyglycol residue.  The fulling may be conducted at a pH of 4 to 7, which may be obtained with the aid of a low molecular weight organic acid, e.g. formic acid.  A spinning lubricant which is carried entrained in the fibres to a water fulling bath may comprise benzoic acid, a mineral or fatty oil and phosphated dodecyltetraethylene glycol. In examples, (1) an aqueous spinning lubricant comprises a mineral oil and iso-octylphenylhexaglycol ether, and the cloth produced is fulled in a bath comprising the acid secondary ester of orthophosphoric acid and oleyl octoglycol, the sodium salt of the secondary ester of orthophosphoric acid with lauryl tetraglycol ether, oleic acid and water; (2) the spinning lubricant is oleic acid and the fulling liquor comprises a neutral ester of orthophosphoric acid with a polyglycol of M.W.450 esterified with oleic acid and paraoxybenzoic acid; (3) the spinning lubricant is an emulsion of ammonium oleate and oleic acid and the fulling liquor comprises the secondary ester of orthophosphoric acid with oleyl-octoglycol and the tertiary ester of orthophosphoric acid with lauryltetraglycol ether; (4) wool-viscose rayon fibres are lubricated during spinning with a mineral oil isooctylhexaglycol ether aqueous emulsion and the fabric is fulled at a pH of 4 to 5 with a composition comprising oleic acid, stearic acid, a neutral ester of orthophosphoric acid and a polyglycol of M.W.200 after-esterified with oleic acid, and a neutral ester of orthophosphoric acid and a polyglycol of M.W.450 after-esterified with stearic acid; (5) wool-nylon fibres are lubricated during spinning as in (4) and are fulled with a composition comprising white oil, para-oxybenzoic acid and the tertiary ester of orthophosphoric acid with lauryl-tetraglycol ether; (6) a spinning oil comprises oleic acid, an ester of orthophosphoric acid and a polyglycol of M.W.300 after-esterified with oleic acid, an ester of oleic acid and an octylglycol, an ester of orthophosphoric acid and dodecyltetraglycol ether and, as a bactericide, trichlorphenol or benzoic acid; the lubricant is carried entrained in the fibres and the fulling bath comprises water only.ALSO:Textile materials comprising at least 20 per cent of wool are fulled in an acid aqueous colloidal dispersion of a carboxylic acid containing at least 6 carbon atoms in the molecule and an ester of ortho-phosphoric acid which has at least one hydrocarbon or substituted hydrocarbon radical containing at least 6 carbon atoms.  The acid and the ester may be added together to the fulling bath or may be used together as a spinning lubricant in a composition which may also comprise a mineral oil or a fatty oil, the composition being allowed to remain upon the fibres and being carried therebyto the fulling bath, which then contains water only, or the acid may be used as a spinning lubricant or in a spinning lubricating composition and may be carried thereby to the fulling bath, which then comprises an aqueous solution of the orthophosphoric acid ester.  After fulling, the acid is neutralized with soda or ammonia and is washed out.  The acid may also be neutralized during the fulling operation and the operation completed under alkaline conditions, or the fulling may be commenced under alkaline conditions and completed under acid conditions.  The acid may be caprylic acid; lauric acid; stearic acid; oleic acid, ricinoleic acid; chlorostearic acid; mixtures of these acids; the acid mixtures obtained by splitting peanut oil or soya-bean oil; benzoic acid; phenyl-acetic acid; salicylic acid; benzoylacetic acid; dioxybenzoic acid or mixtures of these aromatic acids with the above aliphatic acids; the oleic acid ester of p.-oxybenzoic acid or of glycolic, lactic tartaric or gluconic acid; oleylglycocoll; oleylaminobenzoic acid or fatty acid condensation products with amino-acids from decomposed albumen.  The phosphoric acid ester may be a neutral water soluble alkali metal, ammonium or alkylolamine salt of a primary or secondary ester of orthophosphoric acid with a fatty alcohol containing at least 6 carbon atoms in the molecule or with the corresponding fatty acid, fatty acid amide or fatty acid mercaptan which has been substituted by a glycol or polyglycol group, or with sorbitol or polyglycerine; an ester obtained by directly esterifying phenol, cresol, butylcresol, octylphenol, dodecylphenol or cyclohexanol, either as such or as a polyglycol ether, with orthophosphoric acid; a neutral ester produced by after-esterifying a tertiary oxyalkylphosphate with lauric, stearic, oleic or ricinoleic acid; a polycondensed tertiary oxyalkylphosphate or a mixture of two or more of these esters.  The fulling bath may also include a neutralized cellulose ether carboxylic acid or cellulose sulphonic acid or cellulose or starch solubilized by the introduction of a polyglycol residue.  The fulling may be conducted at a pH of 4 to 7, which may be obtained with the aid of a low molecular weight organic acid, e.g. formic acid.  A spinning lubricant which is carried entrained in the fibres to a water fulling bath may comprise benzoic acid, a mineral or fatty oil and phosphated dodecyltetraethylene glycol.  In examples (1) an aqueous spinning lubricant comprises a mineral oil and iso-octylphenylhexaglycol ether and the cloth produced is fulled in a bath comprising the acid secondary ester of orthophosphoric acid and oleyl octoglycol, the sodium salt of the secondary ester of orthophosphoric acid with lauryl tetraglycol ether, oleic acid and water; (2) the spinning lubricant is oleic acid and the fulling liquor comprises a neutral ester of orthophosphoric acid with a polyglycol of M.W.450 esterified with oleic acid and para-oxybenzoic acid; (3) the spinning lubricant is an emulsion of ammonium oleate and oleic acid and the fulling liquor comprises the secondary ester of orthophosphoric acid with oleyl-octoglycol and the tertiary ester of orthophosphoric acid with lauryltetraglycol ether; (4) wool-viscose rayon fibres are lubricated during spinning with a mineral oil isooctylhexaglycol ether aqueous emulsion and the fabric is fulled at a pH of 4 to 5 with a composition comprising oleic acid, stearic acid, a neutral ester of orthophosphoric acid and a polyglycol of M.W.200 after-esterified with oleic acid, and a neutral ester of orthophosphoric acid and a polyglycol of M.W.450 after-esterified with stearic acid; (5) wool-nylon fibres are lubricated during spinning as in (4) and are fulled with a composition comprising white oil, para-oxybenzoic acid and the tertiary ester of orthophosphoric acid with a lauryl-tetraglycol ether; (6) a spinning oil comprises oleic acid, an ester of orthophosphoric acid and a polyglycol of M.W.300 after - esterified with oleic acid, an ester of oleic acid and an octylglycol, an ester of orthophosphoric acid and dodecyltetraglycol ether and, as a bactericide, trichlorphenol or benzoic acid; the lubricant is carried entrained in the fibres and the fulling bath comprises water only.