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Phenyl alkoxy silane prepared by sodium condensation method

A technology of phenylalkoxysilane and sodium condensation, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as low production efficiency and long reaction cycle, Achieve the effects of fast reaction speed, shortened reaction cycle, and reasonable process formula design

Inactive Publication Date: 2007-11-28
盐城市华业医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction cycle is as long as more than 15 hours, and the production efficiency is low

Method used

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  • Phenyl alkoxy silane prepared by sodium condensation method
  • Phenyl alkoxy silane prepared by sodium condensation method
  • Phenyl alkoxy silane prepared by sodium condensation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 50g of n-octane and 11.5g of metallic sodium into a three-necked flask, heat to melt the sodium, start stirring and beat it into sodium sand, and then at 104°C, mix ClSi(OMe) 3 The mixed solution of 42g and 28.5gPhCl was gradually dropped into a three-necked flask within 2h, and then kept at reflux temperature for 3h. After vacuum distillation, 89g of crude product was evaporated, and the sample was analyzed by gas chromatography to measure phenyltrimethoxy 16.37 g of silane, 7.99 g of diphenyldimethoxysilane, and 1.2 g of triphenylmethoxysilane, and the conversion rate of benzene was 64%.

Embodiment 2

[0033] Add 164g of methyl orthosilicate and 23g of metal sodium into a three-necked flask, heat and stir to beat the metal sodium into sodium sand, and then mix 57g of PhCl and 83g of ClSi(OMe) at 120°C 3 The mixed solution was added dropwise within 2 hours, after the drop was completed, it was kept at reflux temperature for another 1 hour, and then the crude product was evaporated under reduced pressure, and analyzed by gas chromatography, the content of phenyltrimethoxysilane was 58.8g, diphenyldimethoxysilane The base silane was 10.6g, and the conversion rate of benzene was calculated to be 89%.

Embodiment 3

[0035] Add 164g of tetraethyl orthosilicate and 23.5 g of sodium metal into the three-necked flask, beat the metal sodium into sodium sand under heating and stirring, and mix 56 g of PhCl and 24 g of SiCl at 110 ° C 4The mixed solution was dripped into a three-necked flask within 2 hours, and after dropping, it was kept at reflux temperature for 2 hours, and then the crude product was evaporated by distillation under reduced pressure, and analyzed by gas chromatography, the amount of phenyltriethoxysilane was 58.2g, two The phenyldiethoxysilane was 19.4g, the triphenylsilane was 2.1g, and the conversion rate of benzene was calculated to be 81%.

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PUM

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Abstract

The present invention relates to sodium condensation process for synthesizing phenyl alkoxyl silane. Chlorobenzene and MeaSiXb(OR)4-(a+b), where, X is Cl or Br, R is Me or Et, a is 0 or1 and b is 1, 2, 3 or 4, are made to produce sodium condensation reaction in solvent at 98-130 deg.c for 0.5-8 hr. The process has complete reaction of metal sodium, simple operation, short reaction period, benzene converting rate up to 70-80 %, and MePhSi(OR)2 selectivity up to 50 %.

Description

Technical field [0001] The present invention relates to the synthesis of phenylalkoxysilane by sodium condensation method. Background technique [0002] In polymer materials such as silicone oil, silicone rubber, and silicone resin, when the main chain silicon atom has a phenyl group, it can be endowed with excellent high and low temperature resistance, high energy radiation resistance and physical and mechanical properties, and it can also be improved. The compatibility of organic compounds (or polymers) and inorganic fillers increases the refractive index of polysiloxane. When the phenyl-containing polysiloxane matches the refractive index of the selected filler, a transparent material can be obtained. Phenyl-containing alkoxysilane Me a Ph b Si(OR) 4-(a+b) (wherein, a=0 or 1; b=1, 2 or 3; R is Me or Et) (Me is CH 3 -, Et is CH 3 CH 2 -, Ph is C 6 h 5 -, the same below) is the basic monomer for synthesizing phenyl silicone oil, phenyl silicone rubber, and phenyl s...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 张银华王一璐
Owner 盐城市华业医药化工有限公司
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