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Preparation method and application of trimethyl silicon alkoxide

A technology of trimethylsilanol and potassium trimethylsiliconate, which is applied in the field of preparation of trimethylsiliconate, and can solve problems such as instability of trimethylsilanol, unsuitability for industrial production, and danger

Inactive Publication Date: 2017-10-10
壮铭新材料科技江苏有限公司
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the methods of this kind of potassium trimethylsiliconate mainly include: 1) Using trimethylchlorosilane, an industrial basic raw material, as raw material to prepare trimethylsilanol, and then react with metal potassium to obtain trimethylsilicon Potassium alkoxide, this method is very difficult to control when preparing trimethylsilanol, trimethylsilanol is very unstable, and if the control is not good, all hexamethyldisiloxane is produced, and the second step uses metal Potassium is very dangerous and not conducive to industrialization, and it is easy to get hexamethyldisiloxane if it is not well controlled in the second step reaction
2) Use hexamethyldisiloxane and sodium amide as raw materials to directly react to obtain the product. Although this method is simple, sodium amide is very dangerous and expensive, and is not suitable for industrial production
3) Use hexamethyldisiloxane and methyl methionine as raw materials, and directly react to obtain the product. Although this method is simple, the methionine is very dangerous and expensive. The reaction requires low temperature, no water and oxygen, and the conditions are relatively harsh. Not suitable for industrial production

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  • Preparation method and application of trimethyl silicon alkoxide
  • Preparation method and application of trimethyl silicon alkoxide
  • Preparation method and application of trimethyl silicon alkoxide

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[0020] see figure 1 , the present invention provides a technical solution: a method for preparing trimethylsiliconate, the preparation steps are as follows: put hexamethyldisiloxane and potassium hydroxide into a 10L three-necked bottle, add 10ml of alcohol preparation, Heated to reflux for 48 hours, while separating water with a water separator, cooled, filtered, and dried to obtain white solid potassium trimethylsiliconate. Alcohol preparations used were methanol, ethanol, isopropanol or ethylene glycol. High-content potassium trimethylsilanolate is prepared by using hexamethyldisiloxane (MM), a cheap industrially produced raw material, as a raw material, and heating and refluxing with various catalysts such as potassium hydroxide. These catalysts are all beneficial to the dissolving of potassium hydroxide and the carrying out of the reaction.

[0021] The process has only one step of reaction. Hexamethyldisiloxane and potassium hydroxide are heated and refluxed under cata...

Embodiment 1

[0023] Such as figure 2 As shown, put 3kg of hexamethyldisiloxane and 560g of potassium hydroxide in a 10L three-necked flask, heat 10ml of methanol, heat to reflux for 48 hours, and simultaneously use a water separator to separate water, cool, filter, and dry to obtain a purity of 91% white solid potassium trimethylsiliconate 0.95kg.

[0024] Take 1.12kg of the obtained potassium trimethylsiliconate in 2L of anhydrous tetrahydrofuran, add 1kg of dimethylchlorosilane dropwise under stirring, and react for 1h at room temperature, filter, concentrate, extract with ether, dry, and concentrate to obtain 1.2kg of pentamethyldisiloxane with a purity of more than 98%.

Embodiment 2

[0026] Such as image 3 As shown, put 3kg of hexamethyldisiloxane and 560g of potassium hydroxide in a 10L three-necked flask, heat 10ml of ethanol, heat to reflux for 48 hours, and simultaneously use a water separator to separate water, cool, filter, and dry to obtain a purity of 90% white solid potassium trimethylsiliconate 0.93kg.

[0027] Take 1.12 kg of the obtained potassium trimethylsiliconate in 2 L of anhydrous tetrahydrofuran, add 1.2 kg of chloromethyl dimethyl chlorosilane dropwise under stirring, and react for 1 h at room temperature, filter, concentrate, extract with ether, and dry , concentrated to obtain 1.8kg of chloromethylpentamethyldisiloxane with a high purity of more than 98%.

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Abstract

The invention discloses a preparation method and an application of trimethyl silicon alkoxide. The preparation method includes the preparation steps: placing hexamethyldisiloxane and potassium hydroxide into a 10L three-mouth flask; adding 10ml of alcohol preparations; performing heating reflux for 48 hours; dividing water by a water knockout trap; cooling, filtering and drying materials to obtain white solid potassium trimethylsilanolate. Inexpensive trimethyl silicon alkoxide (MM) in industrial production serves as a raw material, and the trimethyl silicon alkoxide and the potassium hydroxide are subjected to heating reflux reaction under various catalysts to prepare potassium trimethylsilanolate with high content. All the catalysts are beneficial to dissolution of the potassium hydroxide, and reaction is facilitated.

Description

technical field [0001] The invention relates to the technical field, in particular to a preparation method and application of trimethylsiliconate. Background technique [0002] Organosilicon alcohols and organosilicon alkoxides have very extensive and important significance in the field of synthetic silicone oil, resin and silicone rubber, especially in the modification of new products. In recent years, research has made great breakthroughs. Therefore, it is of great significance to study the synthesis of organosilanols and silicon alkoxides. Potassium trimethylsiliconate is one of the most important. [0003] In the prior art, the methods of this kind of potassium trimethylsiliconate mainly include: 1) Using trimethylchlorosilane, an industrial basic raw material, as raw material to prepare trimethylsilanol, and then react with metal potassium to obtain trimethylsilicon Potassium alkoxide, this method is very difficult to control when preparing trimethylsilanol, trimethyl...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0836C07F7/0838C07F7/0874
Inventor 杨绍祖韦举志王欢李长斌
Owner 壮铭新材料科技江苏有限公司
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