US5359022A
Expired / Lapsed
US
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Process for the preparation of organopolysiloxane resins
Assignee: Wacker Chemie AG
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Filing: 1993-11-03
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Granted: 1994-10-25
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Expires: 2013-11-03
Abstract
Abstract A process for preparing an organopolysiloxane resin, which comprises reacting in a first stage at least one silane of the formula R.sub.a Si(OR.sup.1).sub.4-a (I) in which a is 0, 1, 2 or 3, R is a monovalent organic radical, and/or a partial hydrolyzate thereof, with the proviso that at least one silane of formula (I) in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is employed, and, if appropriate, an organo(poly) siloxane with water in the presence of acid and, if appropriate, other substances, in a second stage reacting the reaction mixture obtained from the first stage in the presence of base and, if appropriate, other substances, and in a third stage adding with stirring, the reaction mixture obtained in the second stage into water, and if appropriate mixed with additives.
Inventors
- 👤 Konrad Mautner
- 👤 Richard Weidner
- 👤 Helmut Oswaldbauer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 21:15
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/20; C08G77/06
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
182 words
A process for preparing an organopolysiloxane resin, which consists essentially of reacting in a first stage at least one silane of the formula R.sub.a Si (OR.sup.1).sub.4-a (I) in which a is 0, 1, 2 or 3, R is a monovalent organic radical, R 1 is a monovalent organic radical, and/or a partial hydrolyzate thereof, with the proviso that at least one silane of formula (I) in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is present, and, optionally, an organo(poly)siloxane selected from the group consisting of R.sup.2.sub.3 Si--O--SiR.sup.2.sub.3 (II) in which R 2 is the same as R, (R.sup.3.sub.2 SiO).sub.b (III) in which R 3 is the same as R, and b is an integer with a value of from 3 to 8, and mixtures thereof, with water in the presence of acid and optionally a polymerization inhibitor, in a second stage reacting the reaction mixture obtained in the first stage with a base and in a third stage adding with agitation the reaction mixture obtained in the second stage into water and precipitate the organopolysiloxane resin.
Claim 2
Dependent Claim
182 words
A process for preparing an organopolysiloxane resin, which consists essentially of reacting in a first stage at least one silane of the formula R.sub.a Si (OR.sup.1).sub.4-a (I) in which a is 0, 1, 2 or 3, R is a monovalent organic radical, R 1 is a monovalent organic radical, and/or a partial hydrolyzate thereof, with the proviso that at least one silane of formula (I) in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is present, and, optionally, an organo(poly)siloxane selected from the group consisting of R.sup.2.sub.3 Si--O--SiR.sup.2.sub.3 (II) in which R 2 is the same as R, (R.sup.3.sub.2 SiO).sub.b (III) in which R 3 is the same as R, and b is an integer with a value of from 3 to 8, and mixtures thereof, with water in the presence of acid and optionally a polymerization inhibitor, in a second stage reacting the reaction mixture obtained in the first stage with a base and in a third stage adding with agitation the reaction mixture obtained in the second stage into water and precipitate the organopolysiloxane resin.
Claim 3
Dependent Claim
38 words
The process of claim 1, wherein a mixture containing an organo(poly)siloxane of formula (II) and a silane of formula (I) in which a is equal to 0, and/or a partial hydrolyzate thereof, is present in the first stage.
Claim 4
Dependent Claim
63 words
The process of claim 1, wherein a mixture of silanes of formula (I), and/or partial hydrolyzates thereof, with the proviso that at least one silane in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is present in the first stage, in which at least 20% of the total number of radicals R in said mixture are aromatic radicals.
Claim 5
Dependent Claim
26 words
The process of claim 1, wherein the acid present in the first stage is selected from the group consisting of HCl, p-toluenesulfonic acid and dodecylbenzenesulfonic acid.
Claim 6
Dependent Claim
20 words
The process of claim 1, wherein the second stage is carried out at a pH of between 8.0 and 14.0.
Claim 7
Dependent Claim
36 words
The process of claim 1, wherein water is present in the third stage in an amount of from 500 to 1000% by weight, based on the total weight of the reaction mixture of the second stage.
Claim 8
Dependent Claim
133 words
The process of claim 1, wherein in a first stage a silane of formula (I) in which a is equal to 0, and/or a partial hydrolyzate thereof, and an organo(poly) siloxane of formula (II) are mixed with water and acid and reacted at the boiling point of the reaction mixture and at a pressure of between 900 and 1100 hPa, in a second stage the reaction mixture obtained in the first stage is reacted in the presence of base and a polar, water-soluble organic solvent at the boiling point of the reaction mixture and at a pressure of between 900 and 1100 hPa, and in a third stage the reaction mixture obtained in the second stage is stirred into water at room temperature and at a pressure of between 900 and 1100 hPa.
Claim 9
Dependent Claim
39 words
An organopolysiloxane resin containing [R 4 3 Sio 1/2 ] and [Sio 4/2 ] units, in which R 4 is a monovalent organic radical with the proviso that at least one radical R 4 is a SiC-bonded n-5-hexenyl radical.
Claim 10
Dependent Claim
39 words
An organopolysiloxane resin containing [R 4 3 Sio 1/2 ] and [Sio 4/2 ] units, in which R 4 is a monovalent organic radical with the proviso that at least one radical R 4 is a SiC-bonded n-5-hexenyl radical.
Claim 11
Dependent Claim
200 words
A process for preparing an organopolysiloxane resin powder which comprises reacting in a first stage at least one silane of the formula R.sub.a Si(OR.sup.1).sub.4-a (I) in which a is 0, 1, 2 or 3, R a monovalent organic radical, R 1 is a monovalent organic radical, and/or a partial hydrolyzate thereof, with the proviso that at least one silane of formula (I) in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is present, and optionally, an organo(poly)siloxane selected from the group consisting of R.sup.2.sub.3 Si--O--SiR.sup.2.sub.3 (II) in which R 2 is the same as R, (R.sup.3.sub.2 SiO).sub.b (III) in which R 3 is the same as R, and b is an integer with a value of from 3 to 8, and mixtures thereof, with water in the presence of an acid and optionally a polymerization inhibitor, in a second stage reacting the reaction mixture obtained in the first stage with a base and in a third stage adding with agitation the reaction mixture obtained in the second stage into water, and in a fourth stage filtering off the precipitated organopolysiloxane resin obtained in the third stage and thereafter washing with water if necessary and drying.
Claim 12
Dependent Claim
200 words
A process for preparing an organopolysiloxane resin powder which comprises reacting in a first stage at least one silane of the formula R.sub.a Si(OR.sup.1).sub.4-a (I) in which a is 0, 1, 2 or 3, R a monovalent organic radical, R 1 is a monovalent organic radical, and/or a partial hydrolyzate thereof, with the proviso that at least one silane of formula (I) in which a is equal to 0 or 1, and/or a partial hydrolyzate thereof, is present, and optionally, an organo(poly)siloxane selected from the group consisting of R.sup.2.sub.3 Si--O--SiR.sup.2.sub.3 (II) in which R 2 is the same as R, (R.sup.3.sub.2 SiO).sub.b (III) in which R 3 is the same as R, and b is an integer with a value of from 3 to 8, and mixtures thereof, with water in the presence of an acid and optionally a polymerization inhibitor, in a second stage reacting the reaction mixture obtained in the first stage with a base and in a third stage adding with agitation the reaction mixture obtained in the second stage into water, and in a fourth stage filtering off the precipitated organopolysiloxane resin obtained in the third stage and thereafter washing with water if necessary and drying.
Claim 13
Dependent Claim
24 words
The process of claim 1, wherein the reaction mixture obtained in the second stage is neutralized before the reaction mixture is added to water.
Claim 14
Dependent Claim
28 words
The process of claim 1, wherein the reaction mixture obtained in the second stage is added with agitation to water containing sufficient acid to neutralize the reaction mixture.
Claim 15
Dependent Claim
19 words
The process as claimed in claim 1, wherein a polar water-soluble organic solvent is added in the second stage.
Claim 16
Dependent Claim
30 words
The process as claimed in claim 1, wherein a silane of formula (I) in which some of the radicals R are acid-sensitive organic radicals are added in the second stage.
Claim 17
Dependent Claim
23 words
The process as claimed in claim 1, wherein acid is added in the third stage in an amount sufficient to neutralize the base.
Claim 18
Dependent Claim
17 words
The process as claimed in claim 1, wherein a flocculation aid is added in the third stage.
Claim 19
Dependent Claim
30 words
The process as claimed in claim 12, wherein a silane of formula (I) in which some of the radicals R are acid-sensitive organic radicals are added in the second stage.
Claim 20
Dependent Claim
17 words
The process as claimed in claim 14, wherein a flocculation aid is added in the third stage.
References Cited (Backward Citations)
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