Patent GB-831020-A (GB)
Title: Organosilicon compositions
IPC: C07F7/00
Filed: 1957-10-02
Abstract: Zirconium compounds of the formula <FORM:0831020/IV (b)/1> wherein each R is an aliphatic hydrocarbon radical, each R1 is R or a H atom, each R11 is R or an aliphatic hydrocarbonoxy radical, n has an average value from 0.75 to 4 and each Y is a hydrocarbonoxy radical, a halogen such as chlorine or fluorine or an oxygen atom, may be made by adding b -dicarbonyl compounds, e.g. b -diketones and b -ketoesters, to appropriate reactive Zr compounds, e.g. zirconium or zirconyl esters of aliphatic alcohols or zirconyl chloride, the reaction proceeding, it is believed, by interaction between enol forms of the b -di-carbonyl compounds and the Zr compound.  It is believed that chelates are formed.  In particular, Zr compounds in which Y is an aliphatic hydrocarbonoxy radical may be made by reacting any b -diketone of the formula RC=CO.CH.  R1C=COR or any b -ketoester of the formula RC=CO.CH.R1.C=CO.OR, in which R is any aliphatic hydrocarbon radical and R1 is R or H, with any Zr compound of the formula Zr(OR)4.  Specified values for R and R1 include alkyl and alkenyl groups.  Compounds are described derived from butyl and octyl zirconates and various b -diketones and b -keto esters in examples.  Specifications 773,347 and 804,162 are referred to.ALSO:A compression for rendering leather water-repellent comprises (a) 50 to 85% (by weight) of a siloxane composed of units of the general formula R111nSiO 4-n/2 wherein each R111 is a monovalent hydrocarbon or halogenated hydrocarbon radical, n is 0, 1, 2 or 3 and the average ratio of R111 to Si in the siloxane is from 0.9 to 3.0; and (b) 15 to 15% of a beta-dicarbonyl zirconium compound containing an average of 0.75 to 4.0 beta-dicarbonyl groups per Zr atom (see Group IV (b)). The siloxanes disclosed contain alkyl, alkenyl, cycloalkyl, aryl, alkaryl, aralkyl and halogenated hydrocarbon radicals.  A particularly useful composition consists of a mixture by weight of (1) 15 to 50% of a compound of the formula <FORM:0831020/IV (a)/1> wherein each R is an aliphatic hydrocarbon radical, each R1 is R or a H atom, each R11 is R or an aliphatic hydrocarbonoxy radical, n has an average value from 0.75 to 4 and each Y is a hydrocarbonoxy radical, a halogen or an oxygen atom; (2) 5 to 70% of a methylpolysiloxane resin composed of (CH3)3SiO0.5 and SiO2 units and having a CH3/Si ratio from 1:1 to 1.5:1,; and (3) from 5 to 80% of siloxanes of the formula ZmSiO4-m/2, wherein each Z is a hydrocarbon radical having less than 7 C atoms and m has an average value of from 2 to 2.9.  The compositions may be made by mixing the siloxanes and Zr compounds in a mutual solvent, e.g. toluene, xylene, methylene chloride and perchloroethylene, or by mixing Zr(OR)4 or a partial hydrolysate thereof with the siloxanes in a mutual solvent and thereafter forming the desired Zr compound in situ by adding the appropriate b -dicarbonyl compound.  Uses.-For rendering leather, glass, ceramic and other surfaces water-repellent (see Group VIII). The partially condensed Zr compounds can be made (1) by reacting a b -dicarbonyl compound with zirconium chloride, preferably in the presence of a hydrogenhalide acceptor, e.g. Na2CO3, and hydrolysing and condensing the resulting compound, or (2) by partially hydrolysing the b -dicarbonyl Zr compounds of the above formula wherein Y is a hydrocarbonoxy radical.  Specifications 773,347 and 804,162 are referred to.