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filingDate 1975-01-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1976-09-15-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-1449102-A
titleOfInvention Preparation of silanol containing organopolysiloxanes
abstract 1449102 Silanol-containing organopolysiloxanes BAYER AG 23 Jan 1975 [24 Jan 1974] 2964/75 Heading C3T A process for the preparation of an organopolysiloxane polyol comprises hydrolysing at least one organochlorosilane of the general formula wherein a, b and c are each 0, 1, 2 or 3 and 2#a + b + c#3, optionally in admixture with up to 30 mol per cent of diphenyldichlorosilane or up to 40 mol per cent of methyltrichlorosilane, ethyltrichlorosilane or vinyltrichlorosilane, by contact with an aqueous solution of ammonia and ammonium chloride in a circulatory device at a temperature of from 10‹ to 90‹C., the NH 4 Cl content of the aqueous solution being from 1-100% of the saturation concentration and the pH of the aqueous solution being adjusted to a value of from 7À5 to 11À6 by introduction of NH 3 , separating the continuously obtained hydrolysate from the aqueous solution immediately after the hydrolysis of the silane(s) and freeing the hydrolysate from NH 3 which is still present by flushing with air or other inert gas and at least partially recycling the NH 4 Clcontaining solution for further reaction with fresh organochlorosilane and ammonia. The process is preferably carried out in the apparatus shown wherein the circulation of an aqueous solution of NH 3 and NH 4 Cl takes place via pump 1, mixing chamber 3, pH meter 4 and separator 5. NH 3 is fed in via flow meter 9 and the silane(s) and water via pumps 8 and 7 respectively. The resulting hydrolysate undergoes a preliminary separation in separator 5 from aqueous NH 4 Cl, which is recirculated to pump 1, and then undergoes a complete separation from the aqueous phase in separator 6. The hydrolysate then passes to flushing columns 11-14 where NH 3 is removed with air or other inert gas introduced from below. In the examples organopolysiloxane polyols of SiOH contents ranging from 12À8-24À8% wt. are prepared as above from dimethyldichlorosilane alone and in admixture with vinylmethyldichlorosilane and/or diphenyldichlorosilane or with methyltrichlorosilane Uses.-Structure-improving additives to silicone rubber mixtures.
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