Ladder-like silicone polymers
First Claim
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1. A method for producing a polymer comprising the steps of:
- (i) reacting an organic solution of at least one monomer having the formula;
R1—
Si(OR2)(OR3)(OR4)wherein R1, R2, R3 and R4 are each independently selected from the group consisting of;
hydrogen, alkyl, alkoxy, alkenyl, alkynyl, aryl, cycloalkyl, heteroaryl and heterocyclyl,with a solution of an acid dissolved in water having a specific resistance of at least 18.2 MΩ
-cm, at a temperature below about 25°
C., to give a prepolymer;
(ii) reacting a solution of the prepolymer with a solution of an alkaline catalyst at a temperature above about 25°
C. to give a polymer; and
(iii) reacting a proportion of the free Si—
OH groups of the polymer with a predetermined sub-stoichiometric amount of a blocking agent to give a partially blocked polymer.
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Abstract
There is disclosed a three stage method for the preparation of ladder-like silicone polymers. The first stage comprises hydrolysis and polymerization of alkyltrialkoxylsilane-like monomers to give relatively low molecular weight prepolymers. The second stage comprises dehydrated condensation polymerization of the prepolymers to give high molecular weight polymers. The third stage comprises partial blocking of a proportion of the pendant Si—OH (silanol) groups with a pre-determined sub-stoichiometric amount of a blocking agent. Also disclosed are the prepolymers, polymers and partially blocked polymers so produced.
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Citations
46 Claims
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1. A method for producing a polymer comprising the steps of:
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(i) reacting an organic solution of at least one monomer having the formula;
R1—
Si(OR2)(OR3)(OR4)wherein R1, R2, R3 and R4 are each independently selected from the group consisting of; hydrogen, alkyl, alkoxy, alkenyl, alkynyl, aryl, cycloalkyl, heteroaryl and heterocyclyl, with a solution of an acid dissolved in water having a specific resistance of at least 18.2 MΩ
-cm, at a temperature below about 25°
C., to give a prepolymer;(ii) reacting a solution of the prepolymer with a solution of an alkaline catalyst at a temperature above about 25°
C. to give a polymer; and(iii) reacting a proportion of the free Si—
OH groups of the polymer with a predetermined sub-stoichiometric amount of a blocking agent to give a partially blocked polymer. - View Dependent Claims (2, 3, 4, 5, 6, 7, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46)
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8. A method for producing a polymer comprising the steps of:
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(i) reacting an organic solution of at least one monomer, the solution comprising at least one solvent selected from the group consisting of benzene, toluene, xylene, methyl isobutyl ketone, methyl ethyl ketone, diethyl ether and isopropyl ether, the at least one monomer having the formula;
R1—
Si(OR2)(OR3)(OR4)wherein R1, R2, R3 and R4 are each independently selected from the group consisting of hydrogen, alkyl, alkoxy, alkenyl, alkynyl, aryl, cycloalkyl, heteroaryl and heterocyclyl, with a solution of an acid dissolved in water having a specific resistance of at least 18.2 MΩ
-cm, at a temperature below about 25°
C., to give a prepolymer;(ii) reacting a solution of the prepolymer with a solution of an alkaline catalyst at a temperature above about 25°
C. to give a polymer; and(iii) reacting a proportion of the free Si—
OH groups of the polymer with a predetermined stoichiometric amount of a blocking agent to give a partially blocked polymer. - View Dependent Claims (9, 10, 11, 12, 13, 14)
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15. A method for producing a polymer comprising the steps of (i) reacting an organic solution of at least one monomer having the formula:
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R1—
Si(OR2)(OR3)(OR4)wherein R1, R2, R3 and R4 are each independently selected from the group consisting of; hydrogen, alkyl, alkoxy, alkenyl, alkynyl, aryl, cycloalkyl, heteroaryl and heterocyclyl, with a solution of an acid dissolved in water having a specific resistance of at least 18.2 MΩ
-cm at a temperature below about 25°
C., to give a prepolymer, the molar ratio of the water to the at least one monomer being from about 3 to 1 to about 20 to 1;(ii) reacting a solution of the prepolymer with a solution of an alkaline catalyst at a temperature above about 25°
C. to give a polymer; and(iii) reacting a proportion of the free Si—
OH groups of the polymer with a predetermined sub-stoichiometric amount of a blocking agent to give a partially blocked polymer. - View Dependent Claims (16, 17, 18, 19, 20)
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Specification