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Method for preparing methyl phenyl ring siloxane

A technology of methylphenylcyclosiloxane and methylphenyldichlorosilane, which is applied in the direction of silicon organic compounds, can solve the problems of low production efficiency, large amount of solvent usage, high energy consumption, etc., to reduce products and improve Productivity, the effect of realizing pollution-free discharge

Inactive Publication Date: 2009-08-12
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the amount of solvent used is large, the production efficiency is low, and the energy consumption is high.
[0006] In previous hydrolysis techniques, a single solvent or no solvent was used, resulting in low yields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 180mL (10.0mol) of distilled water, 60mL (1.48mol) of methanol, and 150mL (1.42mol) of toluene into a 1000mL four-necked flask equipped with mechanical stirring, reflux condenser, dropping funnel and thermometer. Under stirring, 160 mL (1.0 mol) of methylphenyldichlorosilane and 200 mL (1.42 mol) of toluene were gradually added dropwise into the bottle, maintaining the reaction temperature at 20°C. 2h dropwise, continue to react for 3h. The lower acidic aqueous phase was separated, and the organic phase was washed with water until neutral. Dry and filter. The toluene was distilled off, and 108 g of colorless and transparent methylphenylcyclosiloxane was obtained by distillation under reduced pressure, with a yield of 80%.

Embodiment 2

[0023] Add 90mL (5.0mol) of distilled water, 70mL (1.25mol) of ethanol, and 220mL (2.5mol) of benzene into a 1000mL four-necked flask equipped with mechanical stirring, reflux condenser, dropping funnel and thermometer. Under stirring, 160 mL (1.0 mol) of methylphenyldichlorosilane and 160 mL (1.8 mol) of benzene were gradually added dropwise into the bottle, maintaining the reaction temperature at 25°C. 1.5h dropwise, continue to react for 2h. The lower acidic aqueous phase was separated, and the organic phase was washed with water until neutral. Dry and filter. The benzene was evaporated, and 106 g of colorless and transparent methylphenyl cyclosiloxane was obtained by distillation under reduced pressure, with a yield of 78%.

Embodiment 3

[0025] Add 54mL (3.0mol) of distilled water, 25mL (0.27mol) of n-butanol and 360mL (3.0mol) of xylene into a 1000mL four-neck flask equipped with mechanical stirring, reflux condenser, dropping funnel and thermometer. Under stirring, 160 mL (1.0 mol) of methylphenyldichlorosilane and 190 mL (1.58 mol) of xylene were gradually added dropwise into the bottle, maintaining the reaction temperature at 30°C. 2h dropwise, continue to react for 4h. The lower acidic aqueous phase was separated, and the organic phase was washed with water until neutral. Dry and filter. Xylene was distilled off, and 115.6 g of colorless and transparent methylphenylcyclosiloxane was obtained by distillation under reduced pressure, with a yield of 85%.

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Abstract

The invention relates to the field of synthesizing technology in organic chemical engineering, in particular to a method for directly preparing methyl phenyl cyclosiloxane through hydrolyzing dichloromethyl phenylsilane in a multiphase solvent. The method comprises the steps of mixing the dichloromethyl phenylsilane with aromatic hydrocarbon, dripping the mixture into a mutually mixed multiphase mixed solvent system, stirring, carrying out hydrolysis reaction at a temperature of 0-30 DEG C, continuing the reaction for 2-4 h after dripping is finished, and removing the solvent by evaporation to obtain the methyl phenyl cyclosiloxane and linear polymethyl phenyl siloxane product. The invention can realize no pollutant discharge, reduce generation of useless reaction byproducts and improve the product yield rate. The invention is widely used in the production field.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for directly preparing methylphenylcyclosiloxane by hydrolyzing methylphenyldichlorosilane in a heterogeneous mixed solvent. Background technique [0002] Methylphenylcyclosiloxane is an important organosilicon raw material, which can be polymerized under the catalysis of anion (or cation) to obtain polymethylphenylsiloxane with excellent high and low temperature resistance and radiation resistance. oxane. There are three main methods for the preparation of methylphenylcyclosiloxane. The first is the hydrolysis method of methylphenyldichlorosilane; the second is the alkali-catalyzed thermal cracking method of methylphenylpolysiloxane; the third is the dechlorination method of methylphenyldichlorosilane and metal oxides. [0003] For the first method, R.N.Lewis et al. reported in J.Amer.Chem.Soc. (1948) 70,1115-1117 that direct hydrolysis of methylphe...

Claims

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Application Information

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IPC IPC(8): C07F7/21C08G77/04
Inventor 来国桥李美江蒋剑雄邱化玉汪嫣苏丽
Owner HANGZHOU NORMAL UNIVERSITY
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