Preparation method of methyl triethoxysilane

A technology of methyltriethoxysilane and methyldichlorosilane, which is applied in the field of preparation of methyltriethoxysilane, can solve the problems of high price, large hydrogen chloride, high production cost, etc., achieve high cost and reduce raw materials The effect of low cost and selling price

Active Publication Date: 2015-12-09
ZHEJIANG QUZHOU GUIBAO CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages are: the price of methyltrichlorosilane is high, resulting in high production cost; using methyltrichlorosilane as raw materi...

Method used

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  • Preparation method of methyl triethoxysilane
  • Preparation method of methyl triethoxysilane

Examples

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Embodiment

[0028] A preparation method of methyltriethoxysilane, the preparation method steps are as follows:

[0029] (1) Methyldichlorosilane and catalyst (anhydrous nickel chloride, according to the weight of methyldichlorosilane, the consumption of anhydrous nickel chloride is 200-2000ppm) are added in the reactor, heated to reflux, Under the condition of stirring, add absolute ethanol dropwise from the bottom of the reaction kettle, and the dropwise addition of absolute ethanol is carried out in two steps: first, add absolute ethanol with a total weight of 30-35% of absolute ethanol dropwise, and control the reaction temperature at 42±1°C. Then the temperature was raised and kept at 60±1°C, and the remaining absolute ethanol was continued to be added dropwise. During the whole process, nitrogen protection is continued, and the molar ratio of methyldichlorosilane to absolute ethanol is 1:3-3.6.

[0030] (2) After all the anhydrous ethanol has been added dropwise, control the reactio...

specific example 1

[0032] Add 1000kg of methyldichlorosilane and 1kg of anhydrous nickel chloride to a 3000L top reactor with a condenser (cooled by -15°C frozen brine) and a stirring tower, and heat to reflux under nitrogen protection . 1440kg of absolute ethanol was added dropwise from the bottom of the kettle. First add 1 / 3 of absolute ethanol, keep the reaction temperature at 42±1°C, then raise the temperature and keep it at 60±1°C, and continue to add the remaining absolute ethanol dropwise. After all the dropwise addition was completed, the reaction was maintained at 60°C for 3 hours. During the reaction, the reaction kettle was controlled to maintain a slight negative pressure environment, and the pressure was kept at -1KPa. Sampling, gas chromatography detection, does not contain methyldiethoxysilane in the product. Then evacuate to -0.08Mpa in the kettle, and keep the top condenser at -15°C and keep full reflux. After 4 hours of reflux, stop vacuuming. During the reflux process, the i...

specific example 2

[0034] Add 1000kg of methyldichlorosilane and 0.7kg of anhydrous nickel chloride to a 3000L top reactor with a condenser (cooled by -15°C frozen brine) and a stirred tower, and heat to reflux under nitrogen protection state. 1380kg of absolute ethanol was added dropwise from the bottom of the kettle. First add 1 / 3 of absolute ethanol, keep the reaction temperature at 42±1°C, then raise the temperature and keep it at 60±1°C, and continue to add the remaining absolute ethanol dropwise. After all the dropwise addition was completed, the reaction was maintained at 60°C for 3 hours. During the reaction, the reaction kettle was controlled to maintain a slight negative pressure environment, and the pressure was kept at -1KPa. Sampling, gas chromatography detection, does not contain methyldiethoxysilane in the product. Then evacuate to -0.08Mpa in the kettle, keep the top condenser at -15°C and maintain total reflux, stop vacuuming after 4 hours of reflux, during the reflux process,...

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Abstract

The invention discloses a preparation method of methyl triethoxysilane. The method includes the following steps that 1, methyl dichloresilane and a catalyst are added to a reaction still and heated to flow back, and absolute ethyl alcohol is added dropwise from the bottom of the reaction still under the stirring condition; 2, after all absolute ethyl alcohol is added dropwise, the reaction temperature is controlled to be 60+/-1 DEG C, the reaction is continued for more than 2 hours, backflow deacidification is conducted, sodium ethoxide is neutralized and rectified, and methyl triethoxysilane with the content of more than 99.0% is obtained. Methyl dichloresilane serves as the raw material to prepare methyl triethoxysilane, and the price of methyl dichloresilane is far lower than that of methyl trichlorosilane, so that production cost is remarkably reduced, meanwhile, by-product chlorine hydride can be greatly reduced, by-product treatment cost is reduced, the method is simple, easy to carry out and suitable for industrial production, and the product yield is high.

Description

technical field [0001] The invention relates to the field of synthesis of silane crosslinking agents, in particular to a preparation method of methyltriethoxysilane. Background technique [0002] Methyltriethoxysilane is used in the rubber and pharmaceutical industries, and is used as a raw material for organosilicon polymers. This product is an important raw material for the production of silicone resin, phenylmethyl silicone oil and waterproofing agent. At the same time, it is easy to hydrolyze and can form alkali metal silicon alkoxide with alkali metal hydroxide. And it can also be used as a crosslinking agent for room temperature vulcanized silicone rubber. [0003] The traditional preparation process of methyltriethoxysilane is to react methyltrichlorosilane with ethanol through alcoholysis to obtain crude methyltriethoxysilane, then deacidify, neutralize and rectify to obtain methyltriethoxysilane Silane products (such as CN102079754A). The disadvantages are: the ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 李冲合洪璞王伟王燕锋
Owner ZHEJIANG QUZHOU GUIBAO CHEM
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