Preparation method of methyldimethoxysilane

A technology of methyldimethoxyhydrogensilane and methylhydrogendichlorosilane, which is applied in the field of preparation of methyldimethoxyhydrogensilane, can solve the problem of uneven reaction, non-release of chlorosilane, and influence on the use of downstream products, etc. problem, to achieve the effect of improving product quality

Active Publication Date: 2017-05-31
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The first method is the esterification method: that is to use methylhydrogendichlorosilane and methanol as raw materials, and carry out esterification reaction under the action of solvent and hydrochloric acid absorbent to synthesize methyldimethoxyhydrogensilane products. Both are in the stage of small laboratory tests, but because the selected hydrochloric acid adsorbent forms a complex with chlorosilane, the absorbent forms a precipitate with HCl on the one hand, and complexes with methyldichlorohydrogensilane on the other hand. Chlorosilane cannot be released from the complex well, and due to the generation of precipitation, the reaction complex product is wrapped, making the reaction uneven. Therefore, the product yield decreases after the absorbent is used, r

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  • Preparation method of methyldimethoxysilane

Examples

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Embodiment 1

[0031] Add 250g methanol to the constant pressure dropping funnel A on the upper part of the esterification packed tower, add 292g methanol to the constant pressure dropping funnel B in the three-necked flask, and add 1000g methylhydrogendichlorosilane to the constant pressure dropping funnel C in the middle of the packed tower After the material preparation is completed, turn on the magnetic stirrer, and turn on the oil margin heating device outside the three-necked flask. After the oil margin temperature reaches 70°C, start to drop methanol from the upper part of the packed tower into the packed tower at a rate of 25.0g / h. Hydrogen dichlorosilane is dripped into the middle part of the packed tower at a speed of 90g / h, and the methanol in the lower part of the packed tower is dripped into a three-necked flask at a speed of 29.2g / h to carry out the esterification reaction, and the hydrogen chloride by-product is absorbed into hydrochloric acid by tap water. To avoid overflow of...

Embodiment 2

[0033] Add 280g methanol to the constant pressure dropping funnel A on the upper part of the esterification packed tower, add 250g methanol to the constant pressure dropping funnel B in the three-necked flask, and add 1000g methylhydrogendichlorosilane to the constant pressure dropping funnel C in the middle of the packed tower After the material preparation is completed, turn on the magnetic stirrer, and turn on the oil margin heating device outside the three-necked flask. After the oil margin temperature reaches 75°C, start to drop methanol from the upper part of the packed tower into the packed tower at a rate of 28.0g / h. Hydrogen dichlorosilane is dripped into the middle part of the packed tower at a speed of 100g / h, and the methanol in the lower part of the packed tower is dripped into a three-necked flask at a speed of 25.0g / h to carry out esterification reaction, and the by-product hydrogen chloride is absorbed into hydrochloric acid by tap water. To avoid the overflow o...

Embodiment 3

[0035] Add 265g of methanol to the constant pressure dropping funnel A on the upper part of the esterification packed tower, add 270g of methanol to the constant pressure dropping funnel B of the three-necked flask, and add 1000g of methylhydrogendichlorosilane to the constant pressure dropping funnel C in the middle of the packed tower , after the material preparation is completed, turn on the magnetic stirrer, and turn on the oil margin heating device outside the three-necked flask. After the oil margin temperature reaches 80°C, start to drop methanol from the upper part of the packed tower into the packed tower at a rate of 26.5g / h. Hydrogen dichlorosilane is dripped into the middle part of the packed tower at a speed of 110g / h, and the methanol in the lower part of the packed tower is dripped into the three-necked flask at a speed of 27.0g / h to carry out the esterification reaction, and the by-product hydrogen chloride is absorbed into hydrochloric acid by tap water. To avo...

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Abstract

The invention relates to the technical field of fine chemical engineering, and in particular relates to a preparation method of methyldimethoxysilane. The preparation method disclosed by the invention is characterized in that methyldichlorosilane and methanol sufficiently react in a packed tower by adopting a one-step esterification process, and Si-Cl bonds of methylhydrochlorosilane are completely converted into Si-O bonds, and the reaction efficiency is high; after the reaction is ended, a crude product is neutralized by hexamethylenetetramine, and then is filtered and distilled and the like to obtain a methyldimethoxysilane product with the mole yield of 99.5 percent or above. The mole yield of a product prepared by the preparation method disclosed by the invention reaches 95.0 percent or above, and the product is neutral, so the use of downstream customers is not affected; in addition, a used neutralizer does not react with the methylhydrochlorosilane or the methyldimethoxysilane product; by-produced hexamethylene tetramine hydrochloride does not cake, is proper in particle size and easy to filter, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of methyldimethoxyhydrogensilane. Background technique [0002] Methyldimethoxyhydrogensilane contains both hydrolyzed alkoxy linkages (Si-OCH 3 ), which also contains active silicon-hydrogen bonds (Si-H), where Si-OCH 3 The bonds are converted into siloxanes through hydrolysis and condensation; reacting with Grignard reagents can generate organoalkoxysilanes; Si-H bonds can undergo hydrosilylation with a series of unsaturated compounds such as alkenes and alkynes under platinum catalysts Synthetic reaction to obtain various silicone coupling agents, silicone-terminated and cured polyethers, polyacrylate sealants and adhesives, etc., and is suitable for the preparation of many high-purity silicone compounds, such as modified silanes Sealants, anti-fogging agents, water repellents, silane coupling agents such as vinyl, epoxy and methacryloxy derivativ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/188
Inventor 刘明锋吴兵兵陈圣云杨龙安甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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