A kind of preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane

A technology of divinyltetramethyldisiloxane and tetramethyltrisiloxane, which is applied in the field of synthesis of organosilicon compounds, and achieves the effects of high yield, high efficiency and easy operation

Active Publication Date: 2022-03-04
新元化学(山东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the deficiencies in the prior art, the present invention provides a preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane, the method It does not use chlorosilane as a reaction raw material, which solves the problems of environmental protection and poor selectivity caused by chlorosilane in the prior art, and has the advantages of simple operation, high catalytic efficiency, high yield, and good safety.

Method used

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  • A kind of preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane
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  • A kind of preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane

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Effect test

Embodiment 1

[0039] A preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane, comprising the steps of:

[0040] (1) Under nitrogen protection, add 216g (1.0mol) diphenylsilanediol, 204.6g (1.1mol) divinyl Tetramethyldisiloxane and 409.2g n-hexane, then slowly add 4.2g p-toluenesulfonic acid to it and stir to form milky white suspension;

[0041] (2) Turn on the heating, and slowly raise the temperature of the suspension to 70-80°C for reflux reaction. During the reaction, use a water separator to reflux and separate the water generated by the reaction. As the reaction progresses, the system gradually changes from milky white to clear and transparent. Maintain the reaction for 2h;

[0042] (3) After the reaction is complete, the system is lowered to room temperature, and 5% aqueous sodium bicarbonate solution is added to the flask to neutralize the catalyst, then the layers are left to stand, and the organic phase is washed with water at 50-60°C for 0.5h until The s...

Embodiment 2

[0046] A preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane, comprising the steps of:

[0047] (1) Under nitrogen protection, add 216g (1.0mol) diphenylsilanediol, 204.6g (1.1mol) divinyl Tetramethyldisiloxane and 409.2g n-hexane, then slowly add 8.4g p-toluenesulfonic acid therein and stir to form milky white suspension;

[0048] (2) Turn on the heating, and slowly raise the temperature of the suspension to 70-80°C for reflux reaction. During the reaction, use a water separator to reflux and separate the water generated by the reaction. As the reaction progresses, the system gradually changes from milky white to clear and transparent. Maintain the reaction for 2h;

[0049] (3) After the reaction is complete, the system is lowered to room temperature, and 5% aqueous sodium carbonate solution is added to the flask to neutralize the catalyst. Become neutral, obtain upper layer organic phase crude product;

[0050] (4) Collect the organic phase, carry ...

Embodiment 3

[0052] A preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane, comprising the steps of:

[0053] (1) Under nitrogen protection, add 216g (1.0mol) diphenylsilanediol, 204.6g (1.1mol) divinyl Tetramethyldisiloxane and 511.5g n-hexane, then slowly add 12.6g p-toluenesulfonic acid to it and stir to form milky white suspension;

[0054] (2) Turn on the heating, and slowly raise the temperature of the suspension to 70-80°C for reflux reaction. During the reaction, use a water separator to reflux and separate the water generated by the reaction. As the reaction progresses, the system gradually changes from milky white to clear and transparent. Maintain the reaction for 2h;

[0055] (3) After the reaction is complete, the system is lowered to room temperature, and 5% potassium bicarbonate aqueous solution is added to the flask to neutralize the catalyst, then the layers are left to stand, and the organic phase is washed with water at 50-60°C for 0.5h until T...

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Abstract

The invention relates to a preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane, which comprises: under the protection of protective gas, the The organic solvent, diphenylsilanediol, divinyltetramethyldisiloxane and catalyst are mixed in proportion, the temperature is raised for reflux reaction, and the water generated by the reaction is separated by reflux with a water separator. After the reaction is completed, the temperature is lowered, Neutralize and wash with water to obtain the organic phase, and rectify under negative pressure to obtain the product. The invention avoids the problems of environmental protection and low selectivity caused by using chlorosilane as a reaction raw material, and has the advantages of simple and convenient operation, high catalytic efficiency, high yield, good safety and the like.

Description

technical field [0001] The invention belongs to the field of synthesis of organosilicon compounds, and specifically refers to a preparation method of 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane. Background technique [0002] 1,5-divinyl-3,3-diphenyl-1,1,5,5-tetramethyltrisiloxane is an important organosilicon intermediate and belongs to the category of phenyl silicone oil. Its molecular main chain has only three silicon-oxygen chain links, two phenyl groups are connected to the silicon in the middle, and a lively vinyl group is connected to the silicon at both ends. Because of its special molecular structure, it has many unique functions. The vinyl group at the end of its molecule can be used for addition reaction with a compound containing a silicon hydrogen group, and a phenyl group is introduced into the obtained product, which endows the product with excellent high and low temperature resistance, aging resistance, and radiation resistance. As an intermediate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C07F7/20
CPCC07F7/0874C07F7/20
Inventor 于鹏飞解乐福杜辉邵军强侯志伟田志钢
Owner 新元化学(山东)股份有限公司
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