Diphenylcyclotrisiloxane and its preparation method and application

A technology of diphenylcyclotrisiloxane and diphenylsiloxane is applied in the field of synthesis of organosilicon compounds, and can solve the problems of inability to efficiently obtain target products, poor cyclosiloxane selectivity and the like, and achieve copolymerization. The effect of good reaction effect, less impurities and simple process

Active Publication Date: 2021-08-31
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

This method uses a variety of chlorosilanes for co-hydrolysis to obtain different cyclosiloxane mixtures. The selectivity to cyclosiloxanes with specific structures is very poor, and the product is generally a mixture of various cyclosiloxanes, which cannot be efficiently produced. get the target product

Method used

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  • Diphenylcyclotrisiloxane and its preparation method and application
  • Diphenylcyclotrisiloxane and its preparation method and application
  • Diphenylcyclotrisiloxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation method of 1,3-dimethyl-1,3-bis(3,3,3-trifluoropropyl)-5,5-diphenylcyclotrisiloxane comprises the following steps:

[0050] (1) Under nitrogen protection, add 1055g trifluoropropylmethyl dichlorosilane and 540g ethyl acetate to a 5L four-necked flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a vent tube, and dissolve 1080g acetic acid Ethyl ester, 540g of diphenylsilanediol and 555.5g of triethylamine were mixed uniformly to form a transparent solution and then added to the constant pressure dropping funnel, started stirring, and slowly added the materials in the constant pressure dropping funnel dropwise to the flask, The system is cooled by an ice-water bath, and the reaction is maintained at 0-20°C until the addition of the material is completed, and then kept at 0-20°C and continued to stir for 2h;

[0051] (2) After the reaction is complete, filter the system to remove triethylamine hydrochloride, whe...

Embodiment 2

[0057] The preparation method of 1,3-dimethyl-1,3-bis(3,3,3-trifluoropropyl)-5,5-diphenylcyclotrisiloxane comprises the following steps:

[0058] (1) Under nitrogen protection, add 1107.8g trifluoropropylmethyldichlorosilane and 540g ethyl acetate to a 5L four-necked flask equipped with mechanical stirring, a thermometer, a constant pressure dropping funnel, and a vent tube, and 1080g Ethyl acetate, 540g of diphenylsilanediol and 583.3g of triethylamine were mixed uniformly to form a transparent solution, then added to the constant pressure dropping funnel, started stirring, and slowly added the contents of the constant pressure dropping funnel to the flask , the system is cooled by an ice-water bath, and the reaction is maintained at 0-20°C until the material is added dropwise, and then kept at 0-20°C and continued to stir for 2h;

[0059] (2) After the reaction is complete, filter the system to remove triethylamine hydrochloride, wherein the filter cake is washed with 200 g ...

Embodiment 3

[0064] The preparation method of 1,3-dimethyl-1,3-bis(3,3,3-trifluoropropyl)-5,5-diphenylcyclotrisiloxane comprises the following steps:

[0065] (1) Under nitrogen protection, add 1160.5g trifluoropropylmethyldichlorosilane and 540g ethyl acetate to a 5L four-necked flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a vent tube, and 1080g Ethyl acetate, 540g of diphenylsilanediol and 611.1g of triethylamine were mixed uniformly to form a transparent solution, then added to the constant pressure dropping funnel, started stirring, and slowly dropped the contents of the constant pressure dropping funnel into the flask , the system is cooled by an ice-water bath, and the reaction is maintained at 5-15°C until the material is added dropwise, and then kept at 5-15°C and continued to stir for 2h;

[0066] (2) After the reaction is complete, filter the system to remove triethylamine hydrochloride, wherein the filter cake is washed with 2...

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Abstract

The invention relates to diphenylcyclotrisiloxane and its preparation method and application. Trifluoropropylmethyldichlorosilane and diphenylsilanediol are used to react trisiloxane with chlorine at both ends, and then The trisiloxane is hydrolyzed and condensed to make intramolecular cyclization, and the target product is directional prepared through two-step reactions. The method not only suppresses the occurrence of side reactions, but also greatly increases the yield of cyclotrisiloxane, and has the advantages of high efficiency, simple and convenient operation, high product purity and the like.

Description

technical field [0001] The invention belongs to the field of synthesis of organosilicon compounds, in particular to a 1,3-dimethyl-1,3-bis(3,3,3-trifluoropropyl)-5,5-diphenylcyclotrisilane Oxy-alkane and its preparation method and application. Background technique [0002] Fluorosilicone rubber is a special synthetic material whose main chain is silicon-oxygen structure, side chain is methyl and trifluoropropyl structure, mainly through 1,3,5-trimethyl-1,3,5-tri(3 ,3,3-Trifluoropropyl)cyclotrisiloxane (D 3 F) obtained by ring-opening polymerization. The special chemical structure of this material makes it have many unique functions. The Si-O-Si structure of the main chain gives fluorosilicone rubber flexibility and thermal stability, while the side chain structure of trifluoropropyl gives fluorosilicone rubber Good oil and solvent resistance. However, compared with methyl group, trifluoropropyl group is easy to decompose at high temperature to form fluoride, making its h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C08G77/24
CPCC07F7/21C08G77/24
Inventor 于鹏飞解乐福邵军强杜辉侯志伟田志钢
Owner 新元化学(山东)股份有限公司
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