Patent GB-1390791-A (GB)
Title: Flame retarding textiles and paper
IPC: C07F9/40
Filed: 1972-02-23
Abstract: 1390791 Flame retarding textiles and paper STAUFFER CHEMICAL CO 23 Feb 1972 [23 Feb 1971 (2)] 8330/72 Heading DIP A process for flame retarding textiles and paper comprises (a) applying to the textile or paper a composition containing a pentavalent phosphorus ester having at least one C-bonded methylol group, dimethylol dihydroxy ethylene urea and an acid curing catalyst; and (b) curing the pentavalent phosphorus ester and the dimethylol dihydroxy ethylene urea on the textile or paper so as to effect coreaction of the ester and the dimethylol dihydroxy ethylene urea with one another in situ on the textile or paper to render the textile flame-retardant. The composition preferably contains the ester and the dimethylol dihydroxy ethylene urea in a weight ratio of between 3:1 and 1:2. The composition may further contain a peroxygen bleaching agent such as sodium perborate, a supplementary quantity of an aminoplast, a softening agent and a wetting agent. It may be applied from a solution in water, a halogenated hydrocarbon, or an emulsified mixture of a halogenated hydrocarbon and enough water to swell the fibres. The application may be at a pH between 3 and 6.7 and at a temperature between ambient and the curing temperature. The treated textile is heat cured at between 100 and 180‹C. The preferred phosphorus ester is O, O-diethyl N, N-bis (2-hydroxyethyl) aminomethyl phosphonate. Alternatively the phosphorus ester may have the structure I wherein R is a hydrocarbyl radical unsubstituted or substituted by hydroxy and/or a halogen; and R 1  and R 2  are organic radical selected from the group consisting of alkyl and alkoxy which can be unsubstituted or substituted by alkoxy, halogen or hydroxy; hydroxy polyalkyleneoxy; phenyl; halophenyl; amino-substituted alkyl; -O-alkylene-O- or O- alkyleneoxy alkylene-O bonded to the same or another pentavalent phosphorus ester group; amino; alkyl-substituted amino, or hydroxy alkyl-substituted amino, with the proviso that in the aforementioned groups there is at least one carbon-bonded methylol group. A second class of phosphorus esters has the general formula II wherein R 3  and R 4  are selected from the group consisting of lower alkyl, halogenated lower alkyl, lower alkoxy alkyl, lower hydroxy alkyl, lower alkoxy, lower hydroxyalkoxy, hydroxy polyalkyleneoxy and halogenated lower alkoxy, where "lower" corresponds to up to 8C atoms; and n is an integer from 1 to 6. A third class of phosphorus esters has the formula III wherein R 5  and R 6  are alkyl, hydroxyalkyl, alkoxyalkyl or hydroxyalkoxyalkyl (1-6C), the termini of an alkylene forming 6-membered ring or a halogenated analogue thereof, the termini of an alkylene or alkyleneoxyalkylene bonded to a further phosphorus ester group, hydroxypolyoxyalkylene or a hydroxy-substituted analogue thereof; R 7  and R 8  are hydrogen or alkyl (1-6C); m is an integer of 0 to 2; and n is an integer from 0 to 1. A fourth class of phosphorus compounds has the general formula IV wherein R 9  and R 10  can be the same or different and are selected from the group consisting of hydrogen, lower alkyl, lower hydroxyalkyl, lower haloalkyl and hydroxy ("lower" meaning 1-8C) with . the proviso that no more than one of R 9  and R 10  can be hydroxy. The preferred catalysts include zinc chloride, zinc nitrate, magnesium chloride, hydrochloric acid, ortho-phosphoric acid, and 2-amino-2-methyl propanol hydrochloride. The perborate bleach may comprise 5% by weight of the treatment bath and is preferably applied at a pH between 5 and 6.6. The preferred supplementary aminoplasts are tris (methoxymethyl) melamine and tris (methylol) melamine, optionally applied together with acetamide. The preferred softeners are stearamides and polyethylene emulsions. The preferred wetting agents are alkylaryl sulphonates and polyoxyethylene derivatives of alkylphenols. The textile materials may be cotton, cotton/polyester blends, viscose rayon, jute and products made from wood pulp and may be in the form of staple, filament, yarn or woven or non-woven fabric, e.g. apparel, bedding, tent cloth, carpets, home furnishings, aircraft and automobile interior fabrics and industrial fabrics. Reference has been directed by the comptroller to Specification 1336063.