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Polysiloxane and method for producing same

A technology of polysiloxane and manufacturing method, which is applied in the field of polysiloxane manufacturing without solvent, can solve the problems of chemical structure, molecular weight not mentioned, difficulty in controlling substituent ratio, inability to manufacture polysiloxane, etc. , to achieve the effects of process simplification, time shortening and manufacturing cost reduction

Inactive Publication Date: 2008-08-20
DOW CORNING TORAY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When there are two or more substituents, it is also difficult to control the ratio of the substituents in the product, and polysiloxanes having different combinations of mono-substituted siloxane units, di-substituted siloxane units, etc. cannot be produced in desired ratios.
In addition, there is no mention of the detailed chemical structure and molecular weight of the product
So far, no solvent-free, catalyst-free production of polysiloxanes accompanied by the formation of siloxane bonds using hydrolysis-condensation reactions has been proposed

Method used

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  • Polysiloxane and method for producing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] 10mm inner diameter and 9.6cm inner volume where the pressure sensor is installed 3 The reaction tube made of SUS316 was filled with 3ml of phenyltrimethoxysilane and 1.5ml of water, and plugged it with a stopper. The mixture was put into a sand bath heated to 250°C, heated for 15 minutes, and then rapidly cooled in a water bath, and the stopper was opened. The internal pressure of the reaction tube during heating was 3.7 MPa. The product is a phase-separated mixture of a white solid and a colorless transparent liquid. The colorless and transparent liquid is a methanol aqueous solution. In addition, the solid product was confirmed to be phenylsilsesquioxane containing an OH group and a methoxy group from the IR and NMR spectrum data summarized below. The isolation yield of this product converted from the weight of the starting material was 92%, and the molecular weight was 9,700.

[0066] IR(cm -1 ): 3,650, 3,050, 1,595, 1,420, 1,100;

[0067] 13 C-NMR (ppm): 50.9, 128.4, 1...

Embodiment 2

[0070] In Example 1, the reaction was carried out in the same manner as in Example 1, except that the reaction temperature was 300°C and the reaction time was 10 minutes. The internal pressure of the reaction tube during heating was 4.3 MPa. The same phase-separated mixture as in Example 1 was obtained, and the IR and NMR spectra of the solid product were also the same as those in Example 1. It was confirmed that the solid product was phenylsilsesquioxane containing OH groups and methoxy groups. The isolation yield was 92%, and the molecular weight was 13,600.

Embodiment 3

[0072] In Example 1, the reaction was performed in the same manner as in Example 1, except that the amount of phenyltrimethoxysilane was 4 ml, the amount of water was 2 ml, the reaction temperature was 350° C., and the reaction time was 10 minutes. The internal pressure of the reaction tube during heating was 14.3 MPa. The same phase-separated mixture as in Example 1 was obtained, and the IR and NMR spectra of the solid product were also the same as those in Example 1. It was confirmed that the solid product was phenylsilsesquioxane containing OH groups and methoxy groups. The isolation yield was 82%, and the molecular weight was 2,900.

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Abstract

A method of manufacturing a polysiloxane by subjecting a mixture of water and a silicon-containing compound represented by average structural formula (A): R 1 a (R 2 O) b SiO [(4-a-b) / 2] (where R 1 designates the same or different optionally substituted univalent hydrocarbon groups; R 2 is a univalent hydrocarbon group having four or less carbon atoms; and where 'a' and 'b' are numbers that satisfy the following conditions: 0 a 3 ; 0 < b 4 ; and 0 < a + b 4) to hydrolysis and condensation at a temperature not less than 200 DEG C and under pressure not less than 2.5 MPa: is a simplified method of manufacturing a polysiloxane with reduced amount of production wastes.

Description

Technical field [0001] The present invention relates to a method for manufacturing a polysiloxane with a simplified manufacturing method and low environmental pressure. More specifically, it relates to a solvent-free manufacturing method of polysiloxane using a condensation reaction that does not use an acid and a base catalyst. Background technique [0002] Polysiloxane materials have excellent light permeability, electrical insulation, light stability, thermal stability, cold resistance, etc., so they have been used in almost all industrial fields such as electrical and electronics, construction, automobiles, machinery, chemistry, and biochemistry. Used in. As a production method of polysiloxane, the hydrolysis-condensation reaction of chlorosilanes is known as the cheapest method, but since the system is acidic, a neutralization step of the product is required. In addition, polysiloxanes can also be produced using alkoxysilanes as starting materials. However, as described in W...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06
CPCC08G77/06C08G77/04
Inventor 小川琢哉今井纮平大岛义人
Owner DOW CORNING TORAY CO LTD
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