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Preparation method of methyl phenyl silanediol

A technology of methyl phenyl silicon diol and phenyl methyl cyclotetrasiloxane, which is applied in the field of preparation of methyl phenyl silicon diol, can solve the problems of poor storage stability, can not meet market demands and the like, and achieves stable performance. High performance, good gloss, good lubricity

Inactive Publication Date: 2021-12-17
仙桃市格瑞化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing methylphenylsilanediol used in silicone rubber has poor storage stability and cannot meet market demand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A preparation method of methylphenylsilanediol, comprising the steps of:

[0014] 1) Add 20 parts of phenylmethylcyclotetrasiloxane and 20 parts by weight of tetramethyldivinyldisiloxane into a vacuum stirring jacketed tank with a vent valve at the bottom, stir and mix well and then heat up to 70°C Stir and dehydrate for 1 hour under the conditions of ~85°C and -0.11~-0.13MPa; raise the temperature of the reaction solution to 95~100°C, add 1 weight part of lower alcohol for washing, 15 weight parts of alkali solution, 1 weight part of dimethyl sulfoxide and 3 parts by weight of potassium hydroxide, stirred and reacted for 1 hour under the condition of -0.11~-0.13MPa; then added 15 parts by weight of methylphenyldimethoxysilane, stirred and reacted for 2 hours at 110-120°C; then raised the temperature Keep warm at 150°C for 1 hour, then remove small molecules at 180-200°C and -0.11-0.13MPa for 1 hour; after removing small molecules, hydrogen-containing silicone oils with...

Embodiment 2

[0017] A preparation method of methylphenylsilanediol, comprising the steps of:

[0018] 1) Add 50 parts of phenylmethylcyclotetrasiloxane and 25 parts by weight of tetramethyldivinyldisiloxane into a vacuum stirring jacketed tank with a vent valve at the bottom, stir and mix well and heat up to 70°C Stir and dehydrate for 1 hour under the conditions of ~85°C and -0.11~-0.13MPa; raise the temperature of the reaction solution to 95~100°C, add 1 weight part of lower alcohol for washing, 25 weight parts of alkali solution, 1 weight part of dimethyl sulfoxide and 4 parts by weight of potassium hydroxide, stirred and reacted for 1 to 2 hours under the condition of -0.11 to -0.13MPa; then added 15 to 25 parts by weight of methylphenyldimethoxysilane, and stirred and reacted at 110-120°C ~3 hours; then raise the temperature to above 150°C for 1~2 hours, and then remove small molecules at 180~200°C and -0.11~-0.13MPa for 1~2 hours; after removing small molecules, you can get different...

Embodiment 3

[0021] A preparation method of methylphenylsilanediol, comprising the steps of:

[0022] 1) Add 80 parts of phenylmethylcyclotetrasiloxane and 30 parts by weight of tetramethyldivinyldisiloxane into a vacuum stirring jacketed tank with a vent valve at the bottom, stir and mix well and heat up to 70°C Stir and dehydrate for 2 hours under the conditions of ~85°C and -0.11~-0.13MPa; raise the temperature of the reaction solution to 95~100°C, add 2 parts by weight of lower alcohol for washing, 30 parts by weight of alkali solution, and 2 parts by weight of dimethyl sulfoxide and 5 parts by weight of potassium hydroxide, stirring and reacting for 1 to 2 hours under the condition of -0.11 to -0.13MPa; ~3 hours; then raise the temperature to above 150°C for 1~2 hours, and then remove small molecules at 180~200°C and -0.11~-0.13MPa for 1~2 hours; after removing small molecules, you can get different Hydrogen-containing silicone oil with hydrogen content and viscosity;

[0023] 2) Ad...

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PUM

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Abstract

The invention relates to a preparation method of methyl phenyl silanediol, which comprises the following steps of: adding phenyl methyl cyclotetrasiloxane and tetramethyl divinyl disiloxane into a reduced pressure stirring jacket tank with a vent valve at the bottom, stirring and mixing well, heating to 70-85 DEG C, stirring and dehydrating under the conditions of -0.11 to -0.13 MPa, separating out an upper-layer product by a decanting method, and carrying out reduced pressure distillation and filtration to obtain phenyl methyl silanediol. The method is simple in process and suitable for industrial popularization. As low alcohol is used for washing, the proportion of small molecules can be further reduced by 5%. The phenyl methyl silanediol is obtained through equilibrium polymerization of a base catalyst, and the phenyl methyl silanediol is high in stability, good in lubricity and good in glossiness.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymers, in particular to a method for preparing methylphenylsilanediol. Background technique [0002] Methylphenylsilanediol can be regarded as a product in which some of the methyl groups in dimethyl silicone oil are replaced by phenyl groups. It has excellent lubricity, high and low temperature resistance, and radiation resistance, and has broad application prospects. Therefore, the synthesis and application research of polymethylphenylsiloxane has aroused widespread attention at home and abroad. At present, commercially available methyl phenyl silicone oils are roughly divided into five grades according to their structure and phenyl mole fraction, namely: 1) low phenyl silicone oil with 5% to 10% phenyl content; 2) low phenyl silicone oil with phenyl content 25% medium phenyl silicone oil; 3) high phenyl silicone oil with 45% phenyl content; 4) high phenyl low polymerization degree sil...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/06C08G77/08C08G77/10
CPCC08G77/12C08G77/06C08G77/08C08G77/10C08G77/80
Inventor 熊永春
Owner 仙桃市格瑞化学工业有限公司