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Method for preparing a polyorganosiloxane and a polyorganosiloxane

a polyorganosiloxane and polyorganosiloxane technology, applied in the field of polyorganosiloxane and polyorganosiloxane, can solve the problems of low adhesion, limited synthesis method of polyorganosiloxane having a hydrosilyl group, and peeling of a subject material

Inactive Publication Date: 2014-07-31
SHIN ETSU CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present inventors have discovered that certain organic silicon compounds can react with each other to create desired hydrogenpolyorganosiloxanes without losing a hydrosilyl group. The reaction occurs in the presence of a specific catalyst. This discovery solves issues that previously existed with the production of these compounds.

Problems solved by technology

However, in the field of encapsulation of semiconductor devices and sealing, the adhesiveness is low, so that peeling from a subject material occurs often.
As stated above, the hydrosilyl group is hydrolyzed to dehydrogenate in the presence of the catalyst such as a strong alkali and, therefore, the synthesis method of the polyorganosiloxane having a hydrosilyl group is limited and a desired polyorganosiloxane has been not obtained yet.

Method used

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  • Method for preparing a polyorganosiloxane and a polyorganosiloxane
  • Method for preparing a polyorganosiloxane and a polyorganosiloxane
  • Method for preparing a polyorganosiloxane and a polyorganosiloxane

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Experimental program
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first embodiment

of the Present Method

[0040]In the first embodiment of the present method, the component (A) is at least one organic silicon compound having at least one silanol group in the molecule and the component (B1) is at least one organic silicon compound having at least one —OX′ group bonded to a silicon atom in the molecule, wherein X′ is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms or an alkoxyalkyl group having 2 to 10 carbon atoms. The organic silicon compound may be a monomer, dimer, oligomer or polymer. When the organic silicon compound is an oligomer or a polymer, its structure may be linear, branched or linear with a branched part. Particularly, a linear structure is preferred. In a case where a condensate having a high molecular weight is desired, it is preferred that the polyorganosiloxane has two or more silanol or —OX groups in each molecule. When X′ in the component (B1) is a hydrogen atom, the component (A) may be same as the component (B1).

[0041]The component (...

second embodiment

of the Present Method

[0053]In the second embodiment of the present method, the component (B2) is one or more organic silicon compounds having at least one —OX group bonded to a silicon atom in the molecule, wherein X is an alkyl group having 1 to 10 carbon atoms or an alkoxyalkyl group having 2 to 10 carbon atoms. The organic silicon compound may be a monomer, dimer, oligomer and polymer. When the organic silicon compound is an oligomer or a polymer, its structure may be linear, branched or linear with a branched part. Particularly, a linear structure is preferred. In a case where a condensate having a high molecular weight is desired, the polyorganosiloxane preferably has two or more —OX groups in the molecule.

[0054]The component (B2) may be represented by the following general formula:

(R1aSiO(4-a-c) / 2(OX)c)n

wherein, R1 is, independently of each other, a hydrogen atom or a monovalent hydrocarbon group having 1 to 18, preferably 1 to 10 carbon atoms, and optionally having an oxygen...

example 1

[0093]216.31 g (1.0 mol) of diphenyl silane diol (DPS), 484.77 g (4.0 mols) of trimethoxysilane (TMS), 200 g of toluene and 60 g of methanol were mixed, and heated to 30 degrees C. with stirring. Then, 0.02 mol of Mg(OH)2 was added to the mixture and heated at 30 degrees C. for 8 hours to react. Mg(OH)2 was removed by filtration, and toluene, methanol and the unreacted TMS were distilled off under a reduced pressure to obtain a polyorganosiloxane mainly comprising a compound represented by the following formula (10):

Its Mw was 507, an amount of the Si—H group was 0.50 mol / 100 g, and an amount of the alkoxy group was 0.99 mol / 100 g. The 1H-NMR spectrum and GPC chart of the product obtained are as shown in FIGS. 1 and 2. The ratios of the integration values of the functional groups obtained by analyzing the 1H-NMR spectrum are as follows.

—OCH3:6.0 (3.3 to 3.8 ppm)

—SiH:1.0 (4.3 to 4.6 ppm)

—C6H5:5.1 (7.2 to 8.0 ppm)

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Abstract

A method for preparing a polyorganosiloxane represented by the following general formula (1): (R3SiO1 / 2)l(R2SiO2 / 2)m(RSiO3 / 2)n(SiO4 / 2)o (1) wherein the method includes a step of condensation reacting at least one organic silicon compound having at least one hydrogen atom and at least one —OX′ group in the molecule, wherein X′ is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms or an alkoxyalkyl group having 2 to 10 carbon atoms, in the presence of a catalyst, wherein the catalyst is at least one selected from the group consisting of hydroxides of elements in Group 2 of the periodic table, hydrates of hydroxides of elements in Group 2 of the periodic table, oxides of elements in Group 2 of the periodic table, and hydroxides and oxides of metal elements in Groups 3-15 of the periodic table.

Description

CROSS REFERENCE[0001]This application claims the benefits of Japanese Patent application No. 2013-014750 filed on Jan. 29, 2013 and Japanese Patent application No. 2013-253999 filed on Dec. 9, 2013, the contents of which are incorporated by reference.[0002]The present invention relates to a method for preparing a polyorganosiloxane, specifically a polyorganosiloxane having one or more hydrosilyl groups, i.e., SiH group and, one or more alkoxysilyl groups, i.e., SiOR group, in a molecule by subjecting one or more organic silicon compounds having a silanol group, i.e., —SiOH, and / or an alkoxysilyl group, i.e., —SiOR, to a condensation reaction with each other. Further, the present invention relates to a polyorganosiloxane thus obtained.BACKGROUND OF THE INVENTION[0003]Recently, polyorganosiloxanes are attracting attention as a material having good light permeability, good heat resistance, low gas permeability and good chemical stability. Polyorganosiloxanes having various properties a...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C07F7/18
CPCC07F7/1808C07F7/188C07F7/1804C07F7/025C08G77/045C08G77/12C08G77/80
Inventor KUSUNOKI, TAKAYUKIKASHIWAGI, TSUTOMU
Owner SHIN ETSU CHEM IND CO LTD
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