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Chemical method for separating and purifying methylphenyldichlorsilane

A technology of methylphenyldichlorosilane and phenyltrichlorosilane, which is applied in the field of chemical purification of methylphenyldichlorosilane, can solve problems such as phenylchlorosilane pollution, and achieve improved yield, purity and yield High, strong actionable effect

Inactive Publication Date: 2008-07-16
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that due to the high boiling point of the added solvent, the phenylchlorosilane to be separated is polluted by the impurities entrained by the external solvent, which requires further purification treatment, and at least two additional distillation towers are required in addition to the own distillation tower of the distillation system. Fractionation column for separation of individual phase mixtures

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment one. In a 500ml three-necked reactor equipped with stirring, reflux condenser and constant pressure dropping funnel, add 200g of a mixture containing 15% of phenyltrichlorosilane and 85% of methylphenyldichlorosilane, then add 100g of toluene, and Place in a chilled brine bath at -8°C. After the liquid in the reaction kettle dropped to a constant temperature, slowly add a mixture of 2.0 g of water and 20 g of dioxane dropwise from a constant pressure dropping funnel, so that the temperature of the reaction system was not higher than 4°C. After the dropwise addition, the solvent was distilled off under normal pressure, and then the fraction at 205°C was received to obtain 161.7 g of the target product, methylphenyldichlorosilane, with a purity of 99.2% and a yield of 95.1%.

Embodiment 2

[0016] Embodiment two. In a 500ml three-port reaction kettle equipped with stirring, reflux condenser and constant pressure dropping funnel, add 200g of a mixture containing 10% of phenyltrichlorosilane and 90% of methylphenyldichlorosilane, then add 125g of benzene, and Place in a frozen brine bath at -15°C. After the liquid in the reaction kettle dropped to a constant temperature, slowly add a mixture of 3.0 g of water and 30 g of dioxane dropwise from a constant pressure dropping funnel, so that the temperature of the reaction system was not higher than 4°C. After the dropwise addition, the solvent was distilled off under normal pressure, and then the fraction at 205°C was received to obtain 162.9 g of the target product, methylphenyldichlorosilane, with a purity of 99.9% and a yield of 90.5%.

Embodiment 3

[0017] Embodiment three. In a 500ml three-necked reaction kettle equipped with stirring, reflux condenser and constant pressure dropping funnel, add 200g of a mixture containing 10% of phenyltrichlorosilane and 90% of methylphenyldichlorosilane, then add 50g of benzene, and Place in a frozen brine bath at -6°C. After the liquid in the reaction kettle dropped to a constant temperature, slowly add a mixture of 2.5 g of water and 10 g of tetrahydrofuran dropwise from a constant pressure dropping funnel, so that the temperature of the reaction system was not higher than 4°C. After the dropwise addition, the solvent was distilled off under normal pressure, and then the fraction at 205° C. was received to obtain 175.5 g of the target product, methylphenyldichlorosilane, with a purity of 99.1% and a yield of 97.5%.

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Abstract

This invention relates to a method for chemically purifying methylphenyldichlorosilane, characterizing of overcoming the deficit of the background technology and providing a high purity and recovery purifying method for methylphenyldichlorosilane. The process comprises: slowly add the mixture of water and water-soluble solvent into the mixture of methylphenyldichlorosilane and phenyltrichlorosilane with organic solvent already added, and then after finishing the reaction obtain the high purity methylphenyldichlorosilane by distillation. The distillation raffinate can be directly used in the production of organosilicon resin and the organic solvent can be reused.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for chemically purifying methylphenyldichlorosilane. Background technique [0002] When the thermal condensation method is used to produce methylphenyldichlorosilane, not only the main product methylphenyldichlorosilane but also the by-product phenyltrichlorosilane are obtained simultaneously, both of which are important organic silicon monomer raw materials, but Due to the similar boiling points of 205.0°C (101.3kPa) and 201.0°C (101.3kPa) respectively, it is difficult to obtain high-purity methylphenyl dichloride with high efficiency to separate components with high boiling point temperatures and such similar components by means of ordinary distillation separation silane. [0003] For phenylchlorosilane produced by the direct method, the main components of phenylchlorosilane are: PhSiCl 3 , Ph 2 SiCl 2 and Ph 3 For SiCl, their boiling points are 210.0°C, 305.0°C, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12C07F7/20
Inventor 李美江来国桥蒋剑雄邬继荣吕素芳
Owner HANGZHOU NORMAL UNIVERSITY
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