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A kind of preparation method of methyldimethoxysilane

A technology of methyldimethoxysilane and magnetic stirring device, which is applied in the fields of chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., and can solve the problems of little significance in industrial production and difficult to handle high Problems such as boiling matter and methanol by-products are difficult to achieve the effects of reducing equipment requirements, improving product quality, and reaction process safety

Active Publication Date: 2022-01-11
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process of this method is simple, no corrosive substances are produced, and the yield can reach 86%, but the reaction will produce a large amount of high boiling substances that are difficult to handle, and there is a small amount of methanol by-product that is difficult to completely separate from the product; at the same time, due to the high temperature reaction, it can High consumption is also a problem that cannot be ignored, so industrial production is of little significance

Method used

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  • A kind of preparation method of methyldimethoxysilane
  • A kind of preparation method of methyldimethoxysilane

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 120g of 1,3,5,7-tetramethylcyclotetrasiloxane, 212g of trimethyl orthoformate, 6.64g of methanol, and phenylglycidyl ether to a 500mL three-neck flask equipped with a magnetic stirring device and a distillation device. 0.33g and concentrated sulfuric acid 1.33g. Stirring was started, and the temperature of the system was raised to 55°C for 4 hours; then the temperature was slowly raised to 80°C to continue the reaction for 1 hour. From the beginning of heating to the end of the reaction, all the distillates are collected with a receiving bottle to obtain the synthetic crude product. The crude product was then subjected to atmospheric distillation, and the fraction at 60-61°C was collected to obtain 210.2 g of methyldimethoxysilane product. Through GC analysis, the product molar yield is 98.6%, and the main content is 99.5%.

Embodiment 2

[0031] 120g of 1,3,5,7-tetramethylcyclotetrasiloxane, 212g of trimethyl orthoformate, 3.32g of methanol, methyl (ethyl ) glycidyl ether 0.33g and concentrated sulfuric acid 1.66g. Stirring was started, and the temperature of the system was raised to 60°C for 4.5 hours; then the temperature was slowly raised to 85°C to continue the reaction for 1 hour. From the beginning of heating to the end of the reaction, all the distillates are collected with a receiving bottle to obtain the synthetic crude product. The crude product was then subjected to atmospheric distillation, and the fraction at 60-61°C was collected to obtain 207.0 g of methyldimethoxysilane product. Through GC analysis, the product molar yield is 96.9%, and the main content is 99.3%. Stabilizers are epoxy compounds such as epoxy styrene, 1,2-epoxy-3-phenylpropane, and ethylene glycol glycidyl ether.

Embodiment 3

[0033] 120g of 1,3,5,7-tetramethylcyclotetrasiloxane, 212g of trimethyl orthoformate, 9.96g of methanol, ethylene glycol glycidol Ether 0.66g and p-toluenesulfonic acid 0.67g. Stirring was started, and the temperature of the system was raised to 50°C for 5 hours; then the temperature was slowly raised to 90°C to continue the reaction for 1 hour. From the beginning of heating to the end of the reaction, all the distillates are collected with a receiving bottle to obtain the synthetic crude product. The crude product was then distilled at atmospheric pressure, and the fraction at 60~61°C was collected to obtain 208.4g of methyldimethoxysilane product. Through GC analysis, the product molar yield is 97.4%, and the main content is 99.1%.

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Abstract

The invention relates to a method for preparing methyldimethoxysilane, which belongs to the technical field of preparation of silane crosslinking agents. The present invention is under the conditions of certain temperature, catalyst and initiator, 1,3,5,7-tetramethylcyclotetrasiloxane and trimethyl orthoformate are obtained through cracking chain breaking and transesterification reaction to obtain methyl dimethyl Oxysilane, while adding a stabilizer during the reaction to inhibit the disproportionation reaction. Afterwards, the 60~61°C fraction was collected by atmospheric distillation to obtain a methyldimethoxysilane product with a content of more than 99.5%. The method for preparing methyldimethoxysilane has simple process, low equipment requirements, high efficiency, no corrosive substances and high boiling substances, no free chlorine, and is a safe and environment-friendly production method.

Description

technical field [0001] The invention relates to a method for preparing methyldimethoxysilane, which belongs to the technical field of preparation of silane crosslinking agents. Background technique [0002] Methyldimethoxysilane is an important organosilicon intermediate for synthesizing modified silicone oil and modified resin. Its molecular structure contains both hydrolyzable silicon methoxy (Si-OCH 3 ), and contains active silicon-hydrogen bonds (Si-H), which can undergo hydrosilylation reactions with a series of vinyl monomers through silicon-hydrogen bonds, and can introduce different functional groups to obtain various silane coupling agents, which is conducive to accelerating Develop modified silicone products; at the same time, due to the suitable hydrolysis speed, deep curing can be realized. It is an end-capping agent with excellent performance. It can be used as polyether end-capping to obtain the basis of the current popular silicone modified polyether sealant ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
CPCC07F7/188
Inventor 文少卿甘俊甘书官陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM
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