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A kind of preparation method of methylphenylsiloxane ring

A methyl phenyl siloxane ring body and solid technology, which is applied in the direction of silicon organic compounds, can solve the problems of hydrolyzed oil that needs to be washed many times, and achieve the goal of reducing environmental pollution and labor intensity, simplifying the process, and reducing environmental pollution. Effect

Inactive Publication Date: 2015-09-16
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the hydrolyzed oil needs to be washed many times in the process of preparing the methylphenylsiloxane ring body in the prior art, the present invention provides a method using MePhSiCl 2 A method for preparing methylphenylsiloxane rings by hydrolysis of solid complexes. Using this type of solid complexes can ensure that the HCl produced during the hydrolysis process is absorbed in a timely and quantitative manner, and ensure that the hydrolyzed oil is neutral during the entire reaction process. Or weak alkalinity, so that the hydrolyzed oil can be used for cracking and rearrangement without water washing, and at the same time, it also suppresses the breaking of Si-Ph bond to the greatest extent, reduces the generation of cross-linked by-products, and improves the yield of the target product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 246 g (3.12 mol) of pyridine and 246 g of toluene into a 2 L three-necked flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and use a refrigeration system to lower the temperature in the reaction flask to –40 After °C, slowly add 250 mL (1.56 mol) MePhSiCl dropwise through a constant pressure dropping funnel 2 , as the dropwise addition process begins, white precipitates are formed in the reaction bottle immediately. After the dropwise addition, the refrigeration system is removed, and stirring is continued. When the temperature in the reaction bottle reaches room temperature, the reaction mixture is filtered, and the white solid is collected to obtain the six compound compound.

[0024] (2) Transfer the hexa-coordination compound to a 1 L three-necked flask, and slowly add 56.2 g (3.12 mol) of deionized water dropwise under stirring. With the addition of water, the white solid is gradually hydrolyzed, and the temper...

Embodiment 2

[0027] (1) Add 436 g (4.68 mol) of 2-picoline and 1000 g of benzene into a 3 L three-neck flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and use a refrigeration system to lower the temperature in the reaction flask under stirring. After cooling down to 10°C, slowly add 250 mL (1.56 mol) MePhSiCl dropwise through a constant pressure dropping funnel 2 The mixture with 60 mL of benzene, with the beginning of the dropwise addition process, a white precipitate was formed in the reaction bottle immediately, after the dropwise addition was completed, the refrigeration system was removed, and the stirring was continued. When the temperature in the reaction bottle reached room temperature, the reaction mixture was filtered and collected. The white solid is the hexa-coordination compound.

[0028] (2) Transfer the hexa-coordination compound to a 1 L three-necked flask, and slowly add 112.4 g (6.24 mol) of distilled water dropwise under st...

Embodiment 3

[0031] (1) Add 1453 g (15.6 mol) of 3-picoline and 347 g of xylene into a 5 L three-necked flask equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and raise the temperature in the reaction flask to After 30°C, slowly drop 250 mL (1.56 mol) MePhSiCl through a constant pressure dropping funnel 2 With the mixture of 600 mL xylene, as the dropwise addition process begins, a white precipitate is formed in the reaction bottle immediately. After the dropwise addition, the refrigeration system is removed and the stirring is continued. When the temperature in the reaction bottle reaches room temperature, the reaction mixture is filtered. Collect the white solid to obtain the hexa-coordination compound.

[0032] (2) Transfer the hexa-coordination compound to a 3 L three-necked flask, and slowly add 1406 g (78 mol) of deionized water dropwise under stirring. With the addition of water, the white solid is gradually hydrolyzed, and the temperature in...

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Abstract

The present invention relates to the technical field of organosilicone industry, and is to solve the problem in the prior art that the hydrolysis oil requires repeated water washing in the process of synthetizing methylphenylsiloxane ring. The present invention provides a preparation method for methylphenylsiloxane ring. By the method, hydrolysis-generated HCl can be quantitatively absorbed to ensure that the hydrolysis oil is neutral or weakly alkaline. The oil can be used for cracking and rearrangement without special washing with water, at the same time the Si-Ph bond rupture is restrained maximally, the production of crosslinking byproducts are reduced, and the yield of the target product is improved.

Description

technical field [0001] The invention relates to the technical field of organosilicon industry, in particular to a method for preparing a methylphenylsiloxane ring body. Background technique [0002] As a special silicone material, polymethylphenylsiloxane, due to the introduction of phenyl in the structural unit, the material has excellent temperature resistance, radiation resistance, refractive index, damping, and compatibility with traditional organic materials. It is superior to polydimethylsiloxane in other aspects, and is widely used in aerospace, electronics, transportation and other industrial fields, and has increasingly become an important new type of organic silicon polymer material in the national economy. [0003] Methylphenyl siloxane ring is the necessary raw material for the preparation of high-viscosity methyl phenyl silicone oil and high-temperature vulcanized methyl phenyl silicone rubber, and it is also the most important raw material. The methylphenylsil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
Inventor 胡应乾邬继荣来国桥胡承刚张国栋蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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