Patent GB-804745-A (GB)
Title: Improvements relating to compositions for flame-proofing cellulosic material, their use, and material treated therewith
IPC: D06M15/423
Filed: 1957-03-15
Abstract: Cellulosic material is rendered flameproof by treatment with an aqueous solution of a polymethylol melamine, which may be etherified, containing a water-soluble derivative of a polyphosphoric acid of at most 3 P atoms, in which at least four OH groups are replaced by monoalkylamino groups and the remaining OH groups are replaced by mono- or di-alkylamino or by alkoxy groups.  The alkyl groups contain at most 4 carbon atoms. Suitable P compounds are 1,11,3,31 - tetrakis - monomethylamino - 2-monoethylamino triphosphonic acid; 1,11,3,31-tetrakis - monomethylamino - 2- dimethylamino triphosphoric acid; 1,11 - bismonomethylamino - 2 - monoethylamino - 21 - mono-n - propylamino pyrophosphoric acid; 1,11-bis monomethylamino - 2,21 - bis monopropylaminopyrophosphoric acid.  The impregnated cellulosic fibres, e.g. wood, paper, textile materials, are heated to temperatures above 80 DEG  C. if desired after drying.  In examples: (1) trimethylol melamine and either 1,11,3,31-tetrakismonomethylamino - 2 - dimethylamino triphosphoric acid or the corresponding 2-diethylamino compound are dissolved in water.  Muslin is impregnated with the solution, dried and heated for 20 mins. at 120 DEG  C.; (2) uses 1,11,3,31 - tetrakismonomethylamino - 2 - monoethylamino triphosphoric acid; and (3) uses tetrakismonomethylamino triphosphoric acid-2-ethyl ester.  In Example (4) the solution contains dimethylol melamine, with 1,1,3,31-tetrakismonomethylamino triphosphoric acid-2b -chlorethyl ester.  Example (5) uses trimethylol melamine with 1,11 - bis - monomethylamino - 2-monoethylamino - 21 - mono - n - propylamino pyrophosphoric acid, Example (6) a mixture of dimethylol melamine and 1, 11-bis-monomethylamino - 2,21 - bis - mono - n - propylamino pyrophosphoric acid; and in Example (7) an aqueous solution of trimethylol melamine and 1,11,3,31 - tetrakismonomethylamino - 2 - dimethylamino triphosphoric acid is added to a polyvinyl dispersion known as "Geon" (Registered Trade Mark)-Latex 576 containing antimony trioxide and a naphthalene sulphonic acid-formaldehyde condensate. The mixture is used for flameproofing cotton fabric.ALSO:Water-soluble derivatives of polyphosphoric acids containing at most 3 P atoms in which at least four OH groups are replaced by monoalkylamino groups, any other OH groups being replaced by mono- or di-alkylamino or alkoxy groups are prepared by known processes with appropriate selection of starting materials.  The alkyl groups contain at most 4 carbon atoms.  In examples, phosphoric acid ethyl ester-di-(monoethylamide) is heated with (1) dimethyl-amino phosphoric acid dichloride to yield 1,11,3,31 - tetrakismonomethylamino - 2 - dimethylamino triphosphoric acid; (2) monoethylamino phosphoric acid dichloride to yield 1,11,3,31 - tetrakismonomethylamino - 2 - monoethylamino triphosphoric acid; or (3) phosphoric acid ethyl ester dichloride to yield 1,1,1,3,31 - tetrakismonomethylamino triphosphoric acid; (4) phosphoric acid b -chlorethyl ester dichloride heated with phosphoric acid ethyl ester - di - (monomethylamide) yields 1,11,3,31 - tetrakismonomethylamino - tri-) phosphoric acid -2-b -chlorethyl ester; (5) monoethylamino - mono - n - propylamino phosphoric acid chloride heated with phosphoric acid ethyl ester-di-(monomethylamide) to yield 1,11 - bis - monomethylamino - 2 - monoethylamino - 21 - mono - n - propylamino pyrophosphoric acid.