Process for the preparation of organopolysiloxane resin

Details Process for the preparation of organopolysiloxane resin Process for the preparation of organopolysiloxane resin

1994-10-12

1996-08-20

Glass, Margaret

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

From silicon reactant having at least one...

528 21, 528 12, 528 39, 528 34, 528 23, C08G 7706

Patent

active

055480535

DESCRIPTION:

BRIEF SUMMARY
The invention relates to a process for the preparation of organopolysiloxane resin by hydrolysis and condensation of silanes and/or (partial) hydrolysates thereof, and to the use thereof.
Processes for the preparation of organopolysiloxane resin are already known. For example, EP 195 936 A (Toray Silicone Co., Ltd.; published on 1st Oct. 1986) describes a process for the preparation of so-called MQ resins by hydrolysis of alkyl silicate with a monofunctional silane, the reaction mixture comprising at least 5 percent by weight of hydrogen chloride and the alkyl silicate being slowly added dropwise as the last component. EP 294277 A2 (Shin-Etsu Chemical Co., Ltd.; published on 7th Dec. 1988) furthermore describes the preparation of MQ resins having high M:Q ratio by acid hydrolysis with acids containing sulfur. EP 345 534 A1 (Toray Silicone Co., Ltd.; published on 13th Dec. 1989) describes organopolysiloxanes which contain chloromethyl groups and are prepared by hydrolysis and subsequent condensation, the organopolysiloxane obtained by the hydrolysis being separated off from the other components by phase separation before the condensation. U.S. Pat. No. 4,605,446 (Kansai Paint Co., Ltd.; published on 12th Aug. 1986) describes a process for the preparation of siloxane resins which are free from hydroxyl groups, alkyl silicate and trialkoxysilane being hydrolyzed in the presence of water, a mineral acid and a water-soluble solvent and the product then being subjected to condensation by addition of a base. The German patent application of file reference DE-A-4 132 697 (Wacker-Chemie GmbH; applied for on 1st Oct. 1991) furthermore describes a process for the preparation of organopolysiloxane resin by acid hydrolysis of silanes or partial hydrolysates thereof, after-treatment with a base and subsequent precipitation in water.
The object was to provide a process with which organopolysiloxane resins can be prepared in a simple and easily reproducible manner with high space/time yields.
The invention relates to a process for the preparation of organopolysiloxane resin, which comprises consisting of silanes of the formula and and partly distilled off, presence of a base and at least an amount of water-insoluble organic solvent which is sufficient to obtain a homogeneous reaction mass, and removing the water and alcohol by distillation, an acid, if appropriate distilling off water and alcohol still present and removing the salt formed from the neutralization, which has precipitated out, and water-insoluble organic solvent.
The radicals R, R.sup.3 and R.sup.5 in each case independently of one another are preferably monovalent hydrocarbon radicals having 1 to 18 carbon atom(s).
Examples of the radicals R, R.sup.3 and R.sup.5 are, in each case independently of one another, alkyl radicals, such as the methyl, ethyl, n-propyl, iso-propyl, n-butyl, isobutyl, tert-butyl, n-pentyl, iso-pentyl, neo-pentyl and tert-pentyl radical, hexyl radicals, such as the n-hexyl radical, heptyl radicals, such as the n-heptyl radical, octyl radicals, such as the n-octyl radical and iso-octyl radicals, such as the 2,2,4-trimethylpentyl radical, nonyl radicals, such as the n-nonyl radical, decyl radicals, such as the n-decyl radical, dodecyl radicals, such as the n-dodecyl radical, and octadecyl radicals, such as the n-octadecyl radical; alkenyl radicals, such as the vinyl, allyl, n-5-hexenyl, 4-vinylcyclohexyl and the 3-norbornenyl radical; cycloalkyl radicals, such as cyclopentyl, cyclohexyl, 4-ethylcyclohexyl and cycloheptyl radicals, norbornyl radicals and methylcyclohexyl radicals; aryl radicals, such as the phenyl, biphenylyl, naphthyl and anthryl and phenanthryl radical; alkaryl radicals, such as o-, m- and p-tolyl radicals, xylyl radicals and ethylphenyl radicals; and aralkyl radicals, such as the benzyl radical and the alpha- and the .beta.-phenylethyl radical.
Examples of substituted hydrocarbon radicals as the radical R, R.sup.3 or R.sup.5 are, in each case independently of one another, halogenated hydrocarbon radicals, such as the

REFERENCES:
patent: 4242252 (1980-12-01), Newing
patent: 4387196 (1983-06-01), Bonnet et al.
patent: 4413104 (1983-11-01), Deubzer et al.
patent: 4605446 (1986-08-01), Isozaki
patent: 4624870 (1986-11-01), Anthony
patent: 5359022 (1994-10-01), Mauther et al.
patent: 5401821 (1995-03-01), Geck et al.

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