Patent GB-975463-A (GB)
Title: Improvements relating to agents and processes for flame proofing cellulosic materials
IPC: C07F9/54
Filed: 1961-11-20
Abstract: A storage stable composition comprises a tetrakis (alphahydroxy organo) phosphonium chloride compound having the formula <FORM:0975463/C1/1> where R is hydrogen, lower alkyl having 1 to 3 carbon atoms, chlorinated lower alkyl having 1 to 3 carbon atoms, lower alkenyl having 2 or 3 carbon atoms or chlorinated lower alkenyl having 2 or 3 carbon atoms and a sulphite capable of combining with an aldehyde. Phosphonium chlorides mentioned contain hydroxymethyl and alpha-hydroxy-ethyl propyl, propenyl and butenyl radicals. Sulphites (including bisulphites) or alkali and alkaline earth metals and of such tertiary amines as triethanolamine, tripropanolamine, triethylamine and tributylamine. The sulphite may be produced in situ by passing SO2 into an alkaline solution of the halide. The compositions are used to impregnate cellulosic material to impart flame resistance. Preferably urea is also an ingredient. In a typical Example (1) a storage stable solution is prepared by adding sodium sulphite and bisulphite to an aqueous solution of tetrakis (hydroxymethyl) phosphonium chloride. Specification 975,462 is referred to.ALSO:A storage stable composition comprises a tetrakis (alpha-hydroxy organo) phosphonium chloride compound having the formula <FORM:0975463/C3/1> where R is hydrogen, lower alkyl having 1 to 3 carbon atoms, chlrorinated lower alkyl having 1 to 3 carbon atoms, lower alkenyl having 2 or 3 carbon atoms or chlorinated lower alkenyl having 2 or 3 carbon atoms and a sulphite capable of combining with an aldehyde. Phosphonium chlorides mentioned contain hydroxymethyl and alpha-hydroxy-ethyl propyl, propenyl and butenyl radicals. Sulphites (including bisulphites) of alkali and alkaline earth metals and of such tertiary amines as triethanolamine, tripropanolamine, triethylamine and tributylamine are specified. The sulphite may be produced in situ by passing SO2 into an alkaline solution of the halide. The phosphonium chloride can be polymerized in the presence of a water-soluble nitrogen compound, such as an ammonium compound, a primary amine, a cyclic amine, a semicarbazide, a hydrazine, a hydrazide, aminoguanidine, ethylenediamine, phenylenediamine, hexamethylenediamine, tetramethylenepentamine trimethylene-tetramine, or a secondary amine containing at least two amine groups. Particularly advantageous is a composition of the phosphonium chloride, the sulphite, a water soluble triazine or dimethylol cyclic alkylene urea and an ammonium, primary amine, aromatic amine or cyclic amine salt of strong acid as a catalyst. The compositions are used to impregnate cellulosic material to impart flame resistance. Preferably urea is also an ingredient. The material may be impregnated with a single solution of all the components, or the catalyst may be applied separately, by spraying or by means of squeeze rolls. On drying followed by heating the resin is formed on the fibres. In typical examples (1) a storage stable solution is prepared by adding sodium sulphite and bisulphite to an aqueous solution of tetrakis (hydroxymethyl) phosphonium chloride.  A textile-treating composition is made by adding methylolmelamine, urea and ammonium sulphate.  Fabric is impregnated, dried, cured at 300 DEG F. and scoured (5).  A polymer is formed by heating a solution of tetrakis (hydroxymethyl) phosphonium chloride, triethanolamine sulphite, ammonium sulphate and ammonia; (13) to (17) portions of an aqueous solution of the same phosphonium chloride, trimethylol-melamine, urea, sodium sulphite and sodium metabisulphite have added as catalyst: ethanolamine sulphate, hydrazine dihydrochloride, ethylene-diamine di sulphate, diammonium phosphate, ammonium sulphate (\sB polyethylene softener), diethylamine sulphate (for comparison) Specification 975,462 is referred to.ALSO:A process for preparing a flame-retardant cellulose material comprises impregnating a cellulosic material with a composition p  which comprises a tetrakis (alpha-hydroxy organo) phosphonium chloride compound having the formula <FORM:0975463/D1-D2/1> where R is hydrogen, lower alkyl having 1 to 3 carbon atoms, chlorinated lower alkyl having 1 to 3 carbon atoms, lower alkenyl having 2 or 3 carbon atoms or chlorinated lower alkenyl having 2 or 3 carbon atoms, a sulphite capable of combining with an aldehyde, a methylol substituted triazine or dimethylol cyclic alkylene urea and an ammonium or primary amine salt of a strong acid as catalyst, drying, and curing the resin in the material. Phosphonium chlorides mentioned contain hydroxymethyl and alpha-hydroxy-ethypropyl, propenyl and butenyl radicals. Sulphites (including bisulphites) of alkali and alkaline earth metals and of such tertiary amines as triethanolamine, tripropanolamine, triethylamine and tributylamine are specified. The sulphite may be produced in situ by passing SO2 into an alkaline solution of the halide.  The phosphonium chloride can also be polymerized in the presence of a water-soluble nitrogen compound, such as an ammonium compound, a primary amine, a cyclic amine, a semicarbazide, a hydrazine, a hydrazide, aminoguanidine, ethylenediamine, phenylenediamine, hexamethylenediamine, tetramethylenepentamine, trimethylenetetramine, or a secondary amine containing at least two amine groups.  Preferably urea is also an ingredient.  The material may be impregnated with a single solution of all the components, or the catalyst may be applied separately, by spraying or by means of squeeze rolls.  On drying followed by heating the resin is formed on the fibres.  In typical examples (1) a storage stable solution is prepared by adding sodium sulphite and bisulphite to an aqueous solution of tetrakis (hydroxymethyl) phosphonium chloride.  A textile treating composition is made by adding methylolmelamine, urea and ammonium sulphite.  Fabric is impregnated, dried, cured at 300 DEG F. and scoured; (5) A polymer is formed by heating a solution of tetrakis (hydoxymethyl) phosphonium chloride, triethanolamine sulphite, ammonium sulphate and ammonia; (13) to (17) Portions of an aqueous solution of the same phosphonium chloride, trimethylolmelamine, urea, sodium sulphite and sodium metabisulphite were added as catalyst: ethanolamine sulphate, hydrazine dihydrochloride, ethylenediamine di-sulphate, diammonium phosphate, ammonium sulphate (\sB polyethylene softener), diethylamine sulphate (for comparison).  Specification 975,462 is referred to.