Patent GB-938990-A (GB)
Title: Treatment of cellulose with tetrakis (hydroxymethyl) phosphonium resins
Inventor: COATES HAROLD
IPC: D06M15/673
Filed: 1961-06-16
Abstract: Cellulosic material is modified by treating with an aqueous or alcoholic solution of a tetrakis (hydroxymethyl) phosphonium (THP) salt of pH 3-9,5, drying and heating for a time and temperature of 80 DEG -180 DEG C. sufficient to fix the THP salt on or in the material, and then treating the material with ammonia to produce a substantially insoluble polymer.  Suitable THP salts are the chloride, sulphate, acetate and phosphate.  The pH of the THP salt solution may be adjusted, preferably to 5,5-7,0, by addition p  of alkali metal hydroxides, organic bases or alkali salts of weak acids. The impregnated cellulosic material is preferably heated at 100 DEG C. for 30 minutes, 180 DEG C. for 1-2 minutes or intermediate times and temperatures.  The ammonia may be applied as a gas, an aqueous solution, or as an aqueous solution of a partially-hydrolysed ammonium salt, e.g. ammonium carbonate or carbamate.  During the heating step, the THP molecules are condensed, and joined by ether links to the cellulose molecule to give a system which does not migrate to the surface on subsequent curing with ammonia. The cellulosic material e.g. fibres, yarns, fabrics, films, pulp, paper fibre-board, wood and especially viscose material is fire-proofed. Increased dyeability, resistance to creasing and bacterial attack and reduction in lustre may also be attained.  In Example 9, a spun viscose rayon fabric is immersed in an aqueous solution of tetrakis (hydroxymethyl) phosphonium chloride and triethanolamine, dried at 120 DEG -130 DEG C. for 10 minutes, exposed to ammonia gas, and then immersed in aqueous ammonia.  In Example 13, cotton-wool, similarly treated, is immersed in a solution of 5 parts Kiton Fast Red G and 5 parts anhydrous sodium sulphate in 1,000 parts of water at 90 DEG -95 DEG C. for 1 hour with a liquid/cotton ratio of 40:1. The treated cotton-wool is dyed to a greater depth of shade than is untreated cotton-wool.  Specifications 761,985, 882,993, 906,314, 935,098 and 938,989 are referred to.ALSO:Cellulosic materail is modified by treating with an aqueous or alcoholic solution of a tetrakis (hydroxymethyl) phosphonium (THP) salt of pH 3-9,5, drying and heating for a time and temperature, i.e. 80 DEG -180 DEG C. sufficient to fix the THP salt on or in the material, and then treating the material with ammonia to produce a substantially insoluble polymer.  Suitable THP salts are the chloride, sulphate, acetate and phosphate.  The ph of the THP salt solution may be adjusted, preferably to 5,5-7,0, by addition of alkali metal hydroxides, organic bases or alkali salts of weak acids.  The impregnated cellulosic material is preferably heated at 100 DEG C. for 30 minutes, 180 DEG C. for 1-2 minutes or intermediate times and temperatures.  The ammonia may be applied as a gas, an aqueous solution, or as an aqueous solution of a partially-hydrolysed ammonium salt, e.g. ammonium carbonate or carbamate.  During the heating step, the THP molecules are condensed, and joined by ether links to the cellulose molecule to give a system which does not migrate to the surface on subsequent curing with ammonia.  The cellulosic material, e.g. fibres, yarns, fabrics, films, pulp, paper, fibre-board, wood and especially viscose material is fire-proofed. Increased dyeability, resistance to creasing and bacterial attack and reduction in lustre may also be attained.  In Example 9, a spun viscose rayon fabric is immersed in an aqueous solution of tetrakis (hydroxymethyl) phosphonium chloride and triethanolamine, dried at 120 DEG -130 DEG C. for ten minutes, exposed to ammonia gas, and then immersed in aqueous ammonia.  In Example 13, cotton-wool, similarly treated, is immersed in a solution of 5 parts Kiton Fast Red G and 5 parts anhydrous sodium sulphate in 1000 parts of water at 90 DEG -95 DEG C. for one hour with a liquid/cotton ratio of 40 : 1. The treated cotton-wool is dyed to a greater depth of shade than is untreated cotton-wool.  Specifications 761,985, 882,993, 906,314, 935,098 and 938,989 are referred to.