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A kind of preparation technology of methyltrimethoxysilane

A technology for the preparation of methyltrimethoxysilane, which is applied in the field of preparation of methyltrimethoxysilane, can solve problems such as ineffective treatment or utilization, increased pressure in storage containers, hidden safety hazards, etc., and achieve circular supply chain, high utilization rate and low production cost

Active Publication Date: 2018-11-23
浙江中天东方氟硅材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the substance has a low boiling point, and when the temperature is high in summer, it is easy to vaporize and generate pressure, which leads to an increase in the pressure of the storage container, and there are potential safety hazards for long-term storage
Therefore, monomethylhydrogendichlorosilane cannot be effectively processed or utilized. Due to market fluctuations, its value is currently low, and it is usually sold to manufacturers in need at a lower price

Method used

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  • A kind of preparation technology of methyltrimethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Follow the steps below to prepare methyltrimethoxysilane:

[0028] A. Alcoholysis dechlorination dehydrogenation

[0029] At room temperature, use a metering pump to continuously pump 200kg of methanol into the reactor filled with 249kg of monomethylhydrodichlorosilane, and the feeding time is 2h; 3 The speed of / h is passed into N 2 , keep the temperature of the reaction solution at 25±2° C., and carry out the alcoholysis dechlorination and dehydrogenation reaction. After 4 hours of reaction, no obvious acid gas escaped, and the reaction was completed, and nitrogen flow was stopped.

[0030] B. Post-processing

[0031] Add the sodium methoxide methanol solution with a mass fraction of 29% into the reaction kettle to stir and carry out the neutralization reaction until the pH of the reaction solution reaches 7; filter and remove the sodium chloride salt generated by the neutralization reaction, and the filtrate is the crude methyltrimethoxysilane . The crude methyl...

Embodiment 2

[0034] Follow the steps below to prepare methyltrimethoxysilane:

[0035] A. Alcoholysis dechlorination dehydrogenation

[0036] At room temperature, use a metering pump to continuously pump 207kg of methanol into a reaction kettle filled with 250kg of monomethylhydrodichlorosilane, and the feeding time is 4h; 3 The speed of / h is passed into N 2 , heat up, make the temperature of the reaction solution reach 35±2°C, and carry out the alcoholysis dechlorination and dehydrogenation reaction. After reacting for 3 hours, no obvious acid gas escaped, and the reaction was completed, and nitrogen flow was stopped.

[0037] B. Post-processing

[0038] The sodium methoxide methanol solution with a mass fraction of 29% was added to the reactor and stirred for neutralization reaction until the pH of the reaction solution reached 8; the sodium chloride salt generated by the neutralization reaction was removed by filtration, and the filtrate was crude methyltrimethoxysilane. The crude ...

Embodiment 3

[0041] A. Alcoholysis dechlorination dehydrogenation

[0042] At room temperature, respectively pump 213kg of methanol and 249kg of monomethylhydrodichlorosilane into the reaction tower continuously with a metering pump at a rate ratio of 1:1.2. The feeding time is 6 hours, and the temperature of the reaction tower is kept at 35°C. The stripping tower is then sent to the neutralization tank, and the temperature of the stripping tower is 65-70°C.

[0043] B. Post-processing

[0044]Add the sodium methoxide methanol solution with a mass fraction of 29% into the neutralization tank containing the alcoholysis product and stir for neutralization reaction until the pH of the reaction solution reaches 8; the sodium chloride salt generated by the neutralization reaction is removed by filtration, and the filtrate is formazan crude trimethoxysilane. The crude methyltrimethoxysilane is rectified at atmospheric pressure, and the fraction at 103°C is collected to obtain high-purity methy...

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Abstract

The invention discloses a preparation technique of methyltrimethoxy silane. By using monomethylhydrodichlorosilane and methanol as raw materials, the technique comprises the steps of alcoholysis dechlorination and dehydrogenation and after-treatment. The technique specifically comprises the following steps: carrying out alcoholysis reaction on the methanol and monomethylhydrodichlorosilane; and after the reaction finishes, neutralizing the reaction solution to the pH value of 6-8 by using a neutralizer, filtering to remove salts so as to obtain a methyltrimethoxy silane crude product, and carrying out atmospheric rectification on the filtrate to obtain the high-purity methyltrimethoxy silane. The low-value monomethylhydrodichlorosilane is converted into the high-added-value product methyltrimethoxy silane which can be directly sold; and the technique effectively reduces the storage danger of the monomethylhydrodichlorosilane, enhances the production safety, and conforms to the requirements for green clean production.

Description

technical field [0001] The invention relates to a preparation process of organosilane, in particular to a preparation process of methyltrimethoxysilane. Background technique [0002] Methyltrimethoxysilane is mainly used as a crosslinking agent for room temperature vulcanized silicone rubber, a hydrophobic treatment agent for glass fiber surfaces and a treatment agent for reinforced plastic laminates; the amount added to the product is only 0.5% to 4%. It can greatly improve the heat distortion temperature of the product, improve the mechanical properties, electrical properties and processing properties of the product, so it is an important additive in aviation, aerospace, military, medical and health, and civil use. [0003] The traditional preparation process of methyltrimethoxysilane is prepared by the alcoholysis reaction of methyltrichlorosilane and methanol, and hydrochloric acid gas is generated at the same time. However, methyltrichlorosilane is expensive, and its c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/1804C07F7/188C07F7/20
Inventor 邵向东杨庆红席先峰祝爱娟朱雪锋吉兰平
Owner 浙江中天东方氟硅材料股份有限公司
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