Patent GB-881661-A (GB)
Title: Improvements in or relating to organo-siloxane compositions
Inventor: CRANSHAW GEOFFREY HOWARD
Filed: 1957-04-09
Abstract: A composition, for imparting water-repellency to materials, comprises an aqueous emulsion of one or more siloxanes and as curing catalyst therefor one or more metal complexes which are compounds obtainable by reaction of a metal alkoxide or condensed metal alkoxide (in which the metal may be Ti, Zn, U, Fe, Ni or Co) with one or more organic compounds having at least one functional group selected from carbonyl, hydroxyl, amino and carboxylic acid groups.  Some of the complexes may be made by reacting the metal salt or hydroxide with an organic compound capable of effecting alkoxylation.  Metal complexes are described in Specifications 734,113, 784,852 and 786,388. Preferably a solution of the complex and a surface-active agent in a water-immiscible solvent is made prior to emulsifying and adding to an aqueous siloxane emulsion, or the siloxane may be added to the metal complex solution containing the surface-active agent prior to forming an emulsion with water.  In Example (1) a solution of a titanium complex made by heating tetrabutylorthotitanate with acetyl acetone and mixing when cool with a trimethylsiloxy end-blocked dimethylpolysiloxane and perchloroethylene was poured into water containing cetyldimethylbenzylammonium chloride and homogenized; (2) as in (1) except that the orthotitanate was replaced by a condensed butyl titanate; (3) as in (1) except that acetyl acetone was replaced by diacetone alcohol and xylene was an additional solvent; as in (1) with the addition of (4) toluene and (5) benzene; (7) a solution of cetyldimethylbenzylammonium chloride in isopropyl alcohol-trichloroethylene mixture was added to an aqueous emulsion of dimethyl- and methylhydrogen-siloxanes and white spirit; (8) aqueous emulsions of zirconium tetrairon tri-, nickel di- and uranyl-acetylacetonates in mixtures of toluene, perchloroethylene and C15 amine acetates were separately added to aqueous emulsions of end-blocked dimethyl-and methylhydrogen-siloxane mixtures and homogenized; (9) as in (8) but using octyleneglycol titanate as the catalyst; (10, 15) as in (8) but using the reaction product of tetrabutyl titanate and glacial acetic acid as the catalyst; (11) an aqueous emulsion was made of the catalyst of (1) and the siloxane mixture of (8); (12) an emulsion was made of the catalyst of (10) and the siloxane mixture of (8); (13) an aqueous emulsion was made by mixing an aqueous emulsion of the reaction product of butyl titanate and octoic acid with the siloxane emulsion of (8); (14) as in (13) but using as catalyst the reaction product of stearic acid and butyl titanate; (16) an emulsion was made by homogenizing a mixture of an end-blocked dimethylsiloxane, the reaction product of (10), a sulphonated methyl oleate, tolune, perchloroethylene and water; (17) as in (8) but using as catalyst the reaction product of butyl titanate and monohydroxy-ethyltrihydroxy propylethylene diamine; (18) an emulsion was made by mixing the siloxane emulsion of (8) with a solution of the reaction product of butyl titanate and succinic acid and C18 amine acetate mixture in toluene and perchloroethylene.  The emulsions may also contain conventional textile treating agents, e.g. isocyanates, urea/ and melamine/form-aldehyde condensates, wax dispersions, dispersions of fatty condensates and Al and Zn acetates and chlorides.  The subject-matter of Specifications 790,038, 809,822 and 812,505 is disclaimed.  Specifications 680,265 and 708,821 also are referred to.ALSO:A metal complex, in which the metal may be Ti, Th, Zr, U, Fe, Ni or Co, is obtainable by reaction of a metal alkoxide with one or more organic compounds having at least one functional group selected from carbonyl, hydroxyl, amino and carboxylic acid groups to effect co-ordination with the metal atom and/or a replacement of at least one alkoxy radical with an acyl radical or with an alkoxy radical containing a selected functional group.  Certain complexes may be made from a salt or hydroxide of the metal, the other reactant being capable of effecting alkoxylation. Reactants mentioned are tetrabutyl orthotitanate, tetraisopropylorthotitanate, b -chloroethyl titanate, 2-ethylhexyltitanate, zirconium isopropoxide and 2-ethylhexylzirconate; ethylacetoacetate, acetylacetone, diacetone alcohol, salicylaldehyde, formic acid, acetic acid, octoic acid, hexyleneglycol and monohydroxyethyl trihydroxypropyl ethylenediamine; titanium tetrachloride, titanium hydroxide; ferric hydroxide, ferric chloride, uranyl acetate and thorium tetrachloride.  Some of the complexes are described in Specifications 734,113, 784,852 and 786,388.  Complexes specified in the examples are (1,4,11) the reaction product of tetra butyl orthotitanate and acetyl acetone; (3) the reaction product of butyl titanate and diacetone alcohol; (7) zirconium tetra-acetyl acetonate; (8) zirconium tetra-, iron tri-thorium tetra-, nickel di- and uranyl di-acetyl acetonates; (9) octylene glycol titanate; reaction product of butyl titanate with (10,12) glacial acetic acid; (13) octoic acid; (14) stearic acid; (17) mono-hydroxyethyltrihydroxypropylethylenediamine, and (18) succinic acid.