A preparation method for methyl phenyl siloxane unit-containing organosilicone ring bodies

A technology of methyl phenyl silicon and methyl phenyl dimethoxy, which is applied in the field of preparation of methyl phenyl silicon oxygen rings, can solve the problems of easy hydrolysis, excessive waste, unstable raw materials, etc., and achieve low cost , stable process and short reaction steps

Inactive Publication Date: 2012-10-03
SUZHOU BAILINGWEI HYPERFINE MATERIAL
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The raw materials used in this method are uns

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  • A preparation method for methyl phenyl siloxane unit-containing organosilicone ring bodies
  • A preparation method for methyl phenyl siloxane unit-containing organosilicone ring bodies

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[0019] Example 1

[0020] The first reaction: preparation of intermediate methyl phenyl dimethoxy silane

[0021] Under nitrogen protection, add Mg (1.07kg, 44.64mol), 300ml of tetrahydrofuran, 4 grains of iodine, and heat to 70°C. After 40 minutes, slowly add chlorobenzene (5kg, 44.64mol) and The solution prepared by 14L tetrahydrofuran was added dropwise while keeping the reflux state, the internal temperature was kept at 65°C, and the dripping was completed for about 7 hours. After dripping, the solution was kept refluxed. After the reaction for 3 hours, it was naturally cooled to room temperature.

[0022] Under nitrogen protection, add methyltrimethoxysilane (18.24kg, 133.9mol) to a dry 50L reaction kettle, keep the temperature at about 10℃, and add phenylmagnesium chloride format reagent dropwise for about 6 hours and react at room temperature for 3 hours .

[0023] 15L of petroleum ether was added to the reaction kettle for extraction three times, the organic layers were combi...

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Abstract

The invention relates to a preparation method for organosilicone ring bodies. The method comprises that the organosilicone ring bodies are obtained via synthesis and purification processes of synthesis, hydrolysis, pyrolysis and distillation after Grignard reaction of chlorobenzene (bromobenzene). The method has the advantages of readily available and low-price raw materials, stable technology, high security and no environmental pollution, short reaction steps and low cost, and is suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of organic silicon, and particularly relates to a method for preparing a methylphenyl silicone ring body used for silicone rubber, silicone resin and silicone oil. The ring body is 2,4,6-trimethyl-2,4,6-triphenylcyclotrisiloxane (hereinafter referred to as tricyclic) and 1,3,5,7-tetramethyl-1, A mixture of 3,5,7-tetraphenylcyclotetrasiloxane (hereinafter referred to as tetracyclic) (the crude product contains a small amount of pentacyclics). Color is colorless to light yellow viscous liquid, total purity: >99%, wherein the ratio of tricyclic to tetracyclic ring is controllable between 1:7 and 7:1. Background technique: [0002] Methyl phenyl siloxane is a key monomer for the synthesis of high polymers such as functional silicone rubber, silicone resin and silicone oil, and has a wide range of application values. For example, the methyl vinyl phenyl silicone rubber synthesized from this monomer is suitable for the manu...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 宋绍兴邹增龙顾扬
Owner SUZHOU BAILINGWEI HYPERFINE MATERIAL
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