Patent GB-942616-A (GB)
Title: Flame retardant polyurethane
IPC: C08J9/00
Filed: 1961-09-20
Abstract: Polyamides, for use as fire-retardant agents in polyurethane foam (see Division C3) are prepared by reacting ammonia, ammonium carbonate, ammonium carbamate, cyanamide, cyanuric acid, diformylhydrazine or hydrazine with phosphorus oxychloride, pentachloride, or trichloride, phosphorus-containing acids, oxides of phosphorus and such compounds as O = P(OH)2NH2 The preparation of a polymer by reacting phosphorus oxychloride with ammonia is described in Example A.  This is mixed with a sucrose/ethylene oxide/propylene oxide polyol, tris (dichloropropyl) phosphate and tetramethyl ethylene (or 1,3-butane) diamine, for further reaction with a prepolymer.ALSO:A flame retardent solid polyurethane resin foam contains as fire retardant agents a phosphorus - containing polyamide and a plasticizer which is an organic halogenated phosphate or phosphonate, the polyamide containing at least about 10% by weight of nitrogen and at least about 10% by weight of phosphorus and being used in an amount within the range of about 2 to about 30% by weight based on the total resin solid, the halogenated phosphate or phosphonate being used in an amount within the range of about 5 to 30% by weight based on the total resin solids.  As polyamides mention is made of reaction products of ammonia, ammonium carbonate, ammonium carbamate, urea, urea-formaldehyde condensate, guanidenecarbonate - formaldehyde condensate, cyanamide, dicyandiamide, ammeline, cyanuric acid, dimethylol urea, guanadine, biguanadine, biuret, ethylene imine, uric acid, diformyl hydrazine, methylamine, dimethylamine, ethylamine, propylamine, hydrazine, methyl hydrazine, or ethylhydrazine with prosphorus oxychloride, pentoxide, pentachloride or trichloride, phosphoruscontaining acids, oxides of phosphorus, and such compounds as O:P(OH)2NH2.  Described are the reactions of (A) phosphorus oxychloride and ammonia in kerosene, (B) melamine and phosphorus pentoxide, (C) urea and phosphorus pentoxide, (D) a guanadine carbonate-melamineformaldehyde condensate and phosphoric acid. Suitable halogen containing plasticizers have the formula: <FORM:0942616/C3/1> in which R represents hydrocarbon group, X is halogen and Z represents -R(X)m or the structure <FORM:0942616/C3/2> in which G is the organic moiety of a glycol or ether-glycol and n is a number.  The latter compounds can be obtained by reacting a glycol with phosphoric acid to form an acid diester which is subsequently reacted with halogenated monohydric alcohol.  As polyols for the polyurethane formation these can be used: castor oil, alone or with polyethylene glycol, polycarbonates, polyesters or reaction products of alkylene oxides with polyols such as sucrose or sorbitol. Water or halohydrocarbons, cataysts such as tetramethyl guanadine, tertiary amines, stannous oleate or octoate and dibutyl tin dilaurate; and surfactants are other specified components.  In examples (1) a "first package" is made by mixing CC13F with a prepolymer from toluene diisocyanates and a sucrose-ethylene oxide-propylene oxide reaction product and is mixed with various "second packages" comprising tris (dichloropropyl) phosphate plasticizer, sucrose polyether polyol, silicon surfactants, tertiary amine catalysts and reaction products of POC13 with ammonia or of urea with P2O5.  The packages interreact to give a foam; (2) the reaction product of sorbitol with ethylene or propylene oxide and (3) a phthalic anhydride, adipic acid, glycol, trimethylolethane polyester are used as starting materials in processes similar to that of Example (1).