Patent GB-855547-A (GB)
Title: Cellulosic textile materials and processes for making the same
IPC: D06M13/278
Filed: 1957-03-18
Abstract: Configuration-retaining properties are imparted to fabrics and yarns containing or consisting of cellulosic fibres having an average of at least 1,8 hydroxy groups per anhydroglucose unit by applying to the fibres (1) a proportion of water at least sufficient to swell them, but not exceeding 130% by weight of the bone-dry cellulosic fibres, (2) a catalyst which is an alkali metal hydroxide or an alkali-metal salt which, as a 1% aqueous solution, has a pH of at least 10, or a quaternary ammonium hydroxide, the proportion of hydroxide on a dry weight basis and calculated as sodium hydroxide being 2-30% by weight of the total water present and, where a salt is employed, the limits of the proportions being those equivalent to the proportions of hydroxide employed by the above definition, and the numerical product of the proportion of catalyst employed, calculated as sodium hydroxide and in terms of per cent by weight of the total water present, times the proportion of water present, in terms of per cent. by weight of the bone-dry cellulosic fibres, being not more than 4,000 and (3) at least 1% by weight of the cellulosic fibres of a cross-linking agent which forms a cross-linkage including a chain of at least 3 carbon atoms and is represented by one of the formulae: <FORM:0855547/IV(a)/1> wherein X represents halogen, R1, R2 and R3\t represent, in each instance, hydrogen or monovalent non-functional organic radicals, R4 represents a divalent connecting organic radical and Z, in each instance, is a divalent organic radical represented by one of the formulae:  <FORM:0855547/IV(a)/2> wherein R5 and R6, in each instance, represent hydrogen or monovalent non-functional organic radicals, and X represents halogen.  In a modification of the process the cross-linking agent is applied to the dry textile material and the catalyst is thereafter applied in the form of an aqueous solution. Alternatively the catalyst in the form of an aqueous solution may be applied to the textile material and the cross-linking agent thereafter applied.  The cellulose fibres may be natural or may be composed of regenerated or partially esterified cellulose. Preferred crosslinking agents are 1, 3-dichloro-2-propanol and 2, 3-dichloro-1-propanol.  Other agents which may be used are m-di (b , y-epoxypropoxy)-benzene; 1, 3-di(b -hydroxy-g -chloropropoxy)-2-propanol; 1, 2-di-(b -hydroxy-g -chloropropoxy) ethane; 1, 2-di(b ,g -epoxypropoxy)ethane; 1, 2, 3, 4-diepoxybutane; 1, 2, 5, 6-diepoxyhexane; 1, 5-dihydroxy-2, 4-dichloro-cyclohexane and 2, 6-dichloro-3, 4, 5-trihydroxy-5-hydroxymethyl-heptane.  The preferred catalyst is sodium hydroxide, but trimethylphenylammonium hydroxide, sodium silicate or sodium sulphide may also be used.  The proportion of cross-linking agent employed is preferably 6 to 30% by weight of the cellulosic fibres.  In an example, a length of dry, desized and mercerised cotton material is impregnated with about 15% by weight of a mixture of about 70% of 2, 3-dichloro-1-propanol and 30% of 1, 3-dichloro-2-propanol and then passed through a 10% aqueous sodium hydroxide solution containing 2% sodium 2-ethyl-hexyl sulphate as a wetting agent to give about 70% pick up.  The cotton is then passed through a short tenter frame, wound into a tight roll, stored at room temperature for 12 hours wrapped in polythene, unwound, scoured, washed and dried.  Fabrics treated according to the invention can be repeatedly bleached with chlorine bleaches without yellowing.ALSO:Configuration-retaining properties are imparted to fabrics and yarns containing or consisting of cellulosic fibres having an average of at least 1,8 hydroxy groups per anhydroglucose unit by applying to the fibres (1) a proportion of water at least sufficient to swell them, but not exceeding 130% by weight of the bone-dry cellulosic fibres, (2) a catalyst which is an alkalimetal hydroxide or an alkali-metal salt which, as a 1% aqueous solution, has a pH of at least 10, or a quaternary ammonium hydroxide, the proportion of hydroxide on a dry weight basis and calculated as sodium hydroxide being 2-30% by weight of the total water present and, where a salt is employed, the limits of the proportions being those equivalent to the proportions of hydroxide employed by the above definition, and the numerical product of the proportion of catalyst employed, calculated as sodium hydroxide and in terms of per cent by weight of the total water present, times the proportion of water present, in terms of per cent by weight of the bone-dry cellulosic fibres, being not more than 4,000 and (3) at least 1% by weight of the cellulosic fibres of a cross linking agent which forms a cross linkage including a chain of at least 3 carbon atoms is represented by one of the formulae:  <FORM:0855547/IV (c)/1> wherein X represents halogen, R1 R2 and R3 represent, in each instance, hydrogen or monovalent non-functional organic radicals, R4 represents a divalent connecting organic radical and Z, in each instance, is a divalent organic radical represented by one of the formulae: <FORM:0855547/IV (c)/2> wherein R5 and R6, in each instance, represent hydrogen or monovalent non-functional organic radicals, and X represents halogen.  In a modification of the process the cross-linking agent is applied to the dry textile material and the catalyst is thereafter applied in the form of an aqueous solution. Alternatively the catalyst in the form of an aqueous solution may be applied to the textile material and the cross-linking agent thereafter applied.  The cellulosic fibres may be natural or may be composed of regenerated or partially esterified cellulose. Preferred cross-linking agents are 1, 3- dichloro -2- propanol and 2, 3- dichloro -1- propanol.  Other agents which may be used are mdi(b , g - epoxypropoxy) -benzene; 1, 3-di(b - hydroxyg - chloropropoxy) -2- propanol; 1, 2 -di-(b - hydroxy-g -chloropropoxy) ethane; 1, 2- di(b , g -epoxypropoxy) ethane; 1, 2; 3, 4- diepoxybutane; 1, 2; 5, 6- diepoxyhexane; 1, 5- dihydroxy-2, 4-dichlorocyclohexane and 2, 6- dichloro -3, 4, 5-trihydroxy -5- hydroxymethyl-heptane.  The preferred catalyst is sodium hydroxide, but trimethylphenylammonium hydroxide, sodium silicate or sodium sulphide may also be used.  The proportion of cross-linking agent employed is preferably 6-30% by weight of the cellulosic fibres. In an example, a length of dry, desized and mercerised cotton material is impregnated with about 15% by weight of a mixture of about 70% of 2, 3- dichloro -1- propanol and 30% of 1, 3- dichloro -2- propanol and then passed through a 10% aqueous sodium hydroxide solution containing 2% sodium 2- ethylhexyl sulphate as a wetting agent to give about 70% pick-up.  The cotton is then passed through a short tenter frame, wound into a tight roll, stored at room temperature for 12 hours wrapped in polythene, unwound, scoured, washed and dried.  Fabrics treated according to the invention can be repeatedly bleached with chlorine bleaches without yellowing.  Permanent pleats may be imparted to fabrics by conducting the cross-linking while the fabric is in a pleated condition.