Patent GB-675188-A (GB)
Title: Organo-silicon compounds
IPC: D06M15/643
Filed: 1948-10-28
Abstract: An organo-trihalosilane, in which the organo radical is an alkyl or an alkenyl radical, is subjected to direct alkaline hydrolysis with an aqueous solution of an alkali metal hydroxide to give an aqueous solution of a hydrolysis product suitable for use in providing silicone coatings on fabrics.  In general, an ethereal solution of the trihalosilane is hydrolysed with excess alkali solution to give a solution which has a lower surface tension than an alkali solution of comparable concentration and may be used to wet out textile materials and, by neutralization after impregnation of a fabric produces siloxane resins in situ. In examples: (1) to (15) aqueous alkaline solutions are prepared by the hydrolysis by caustic potash or soda of trichlorosilanes having methyl, ethyl, n-propyl, isopropyl, n-butyl, sec.-butyl, tert.-butyl, methallyl, amyl, 2-ethyl-hexyl, n-octyl, lauryl, octadecyl and oleyl radicals; (16) n-butyltrifluorosilane is hydrolysed by sodium hydroxide; (17) n-butyltrichlorosilane is hydrolysed by lithium hydroxide.  The Specification as open to inspection under Sect. 91, comprises also substitution by other organo radicals and the preparation of solid compounds by treating an organo-trihalosilane with liquid or aqueous ammonia to form a precipitate, dissolving the precipitate in ether and treating the solution with solid or alcoholic caustic alkali.  In examples: (16) to (19) and (22) aqueous alkaline solutions are prepared by the hydrolysis by caustic potash or soda of trichlorosilanes having benzyl, amylphenyl, amylbenzyl, ethylphenyl and tetrahydronaphthylyl radicals; (23), (24) n-butyltrichlorosilane is hydrolysed by barium and tetraethanolammonium hydroxides; solid compounds are prepared (25 to 27) by treating phenyl, benzyl or amylphenyl trichlorosilane with concentrated or liquid ammonia and hydrolysing the product with solid or alcoholic caustic potash; (28) by treating amylphenyl trichlorosilane with potassium acetate in glacial acetic acid to give amylphenyl trioltriacetate, saponifying by refluxing with alcoholic KOH and crystallizing to give a monomer/dimer mixture; (29) by treating amylphenyl trichlorosilane with alcoholic KOH, the filtered solution being crystallized to give a monomer/dimer mixture.  This subject-matter does not appear in the Specification as accepted.ALSO:An organo-trihalosilane, in which the organo radical is an alkyl or an alkenyl radical, is subjected to direct alkaline hydrolysis with an aqueous solution of an alkali metal hydroxide to give an aqueous solution of a hydrolysis product suitable for use in providing silicone coatings on fabrics.  In general, an ethereal solution of the trihalosilane is hydrolysed with excess alkali solution to give a solution which has a lower surface tension than an alkali solution of comparable concentration and may be used to wet out textile materials and, by neutralization after impregnation of a fabric produces siloxane resins in situ. In examples: (1) to (15) aqueous alkaline solutions are prepared by the hydrolysis by caustic potash or soda of trichlorosilanes having methyl, ethyl, n-propyl, isopropyl, n-butyl, sec.-butyl, tert.-butyl, methallyl, amyl, 2-ethyl-hexyl, n-octyl, lauryl, octadecyl and oleyl radicals; (16) n-butyltrifluorosilane is hydrolysed by sodium hydroxide; (17) n-butyltrichlorosilane is hydrolysed by lithium hydroxide.  The Specification as open to inspection under Sect. 91 comprises also substitution by other organo radicals and the preparation of solid compounds by treating an organo-trihalosilane with liquid or aqueous ammonia to form a precipitate, dissolving the precipitate in ether and treating the solution with solid or alcoholic caustic alkali.  In examples (16) to (19) and (22) aqueous alkaline solutions are prepared by the hydrolysis by caustic potash or soda of trichlorosilanes having benzyl, amylphenyl, amylbenzyl, ethylphenyl and tetrahydronaphthyl radicals; (23), (24) n-butyltrichlorosilane is hydrolysed by barium and tetraethanolammonium hydroxides; solid compounds are prepared (25 to 27) by treating phenyl, benzyl or amylphenyl trichlorosilane with concentrated or liquid ammonia and hydrolysing the product with solid or alcoholic caustic potash; (28) by treating amylphenyl trichlorosilane with potassium acetate in glacial acetic acid to give amylphenyl trioltriacetate, saponifying by refluxing with alcoholic KOH and crystallizing to give a monomer/dimer mixture; (29) by treating amylphenyl trichlorosilane with alcoholic KOH, the filtered solution being crystallized to give a monomer/dimer mixture.  This subject-matter does not appear in the Specification as accepted.