| 摘要 |
<p>Cellulosic materials are treated with quaternary ammonium salts of <FORM:0933056/IV(a)/1> where Rf C4-12 perfluoroalkyl, R is C1-12 alkylene, R1 is hydrogen or C1-6 alkyl and X is chlorine or bromine (for preparation see Group IV(b)). The compounds may react with cellulosic hydroxyl groups. The material may be treated in aqueous medium buffered to pH 5.5 to 6.5, dried at 40 DEG -100 DEG C., heated to fix the finish at 100 DEG -140 DEG C. and then, desirably, treated with a mild alkaline wash. Examples describe the treatment of cotton cloth using sodium acetate buffered solutions; rayon, acetate and paper are also specified cellulosic materials. Specifications 471,130 and 857,906 are referred to. ALSO:The invention comprises compounds of formula <FORM:0933056/IV(a)/1> where Rf is C4-12 perfluoroalkyl, R is C1-12 alkylene, R1 is hydrogen or C1-6 alkyl, and X is chlorine or bromine; and quaternary ammonium salt derivatives thereof with a tertiary organic base. They are prepared by treating a compound of formula <FORM:0933056/IV(a)/2> with formaldehyde and hydrogen chloride or hydrogen bromide, conveniently by passing gaseous hydrogen halide into a solution of the above alkanol and paraformaldehyde in an inert solvent; the mixture may be heated to about 25-100 DEG C. for completion. Quarternisation is conveniently effected by dissolving the halomethyl compound in ether or other solvent (e.g. toluene, benzene or dioxane) in which the quaternary salt is insoluble and adding the tertiary base while heating at 25-100 DEG C. Specified tertiary bases include trialkylamines, alkarylamines and heterocyclic amines. The quaternary derivatives are used to impart water-, oil- and soil-repellant properties to fibrous materials (see Groups IV(a) and IV(c)). 5-(N- methylperfluorooctanesulphonamido)-pentanol is obtained by alkaline hydrolysis (followed by acdification) of N-methyl-5-perfluorooctanesulphonamidopentyl acetate itself obtained by reacting the sodium salt of N-methylperfluorooctanesulphonamide with 5-chloropentyl acetate. Specifications 471,130 and 857,906 are referred to.ALSO:Water-, oil- and soil-repellant properties are imparted to woven and non-woven fibrous materials such as wool, cotton, rayon, acetate, nylon, paper, leather, wood, felt and to vitreous surfaces including glass fibres by treatment with a quaternary ammonium salt of a compound of formula <FORM:0933056/IV(a)/1> where Rf is C4-12 perfluoroalkyl, R is C1-12 alkylene, R1 is hydrogen or C1-6 alkyl and X is chlorine or bromine (for preparation see Group IV(b)). The material may be treated in aqueous medium buffered to pH 5,5 to 6,5, dried at 40 DEG -100 DEG C., heated to fix the finish at 100 DEG -140 DEG C., then desirably mildly alkaline washed and dried. The fluorinated compound may react with the material. The treatment may be applied to resin-treated, crease-resistant fabrics. Examples describe the treatment of cotton cloth using sodium acetate buffered solutions. Specifications 471,130 and 857,906 are referred to.</p> |
