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Method for preparing hexamethyldisilane

A technology of hexamethyldisilane and trimethylchlorosilane is applied in the field of preparation of organosilicon materials, and can solve the problems that hexamethyldisilane and hexamethyldisilane are not disclosed, and the reaction is not easy to control, and the like, Achieve the effect of short reaction time and high-efficiency production

Active Publication Date: 2008-05-21
ZHEJIANG HAIZHOU PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] And another domestic patent publication number CN1974579 discloses a preparation process using sodium as a raw material. It is also mentioned in its specification that it is not feasible to prepare hexamethyldisilane by reacting with potassium as a raw material, specifically including the difficulty of the reaction. Control, economic cost, the yield after the reaction is considered to be 75%, etc., but it does not disclose how to operate and realize the preparation method of hexamethyldisilane when potassium is used as a raw material
[0012] So far, there is no domestic synthesis process for producing hexamethyldisilane using a certain proportion of potassium instead of lithium metal

Method used

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  • Method for preparing hexamethyldisilane

Examples

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Effect test

Embodiment 1

[0026] First fill nitrogen into a 1500ml reactor, pump in 2.0mol (246.5ml) of solvent o-xylene, put in 1.2mol (46.8g) of potassium metal, raise the temperature to about 80 degrees, and slowly add 1.5 mol of trimethylchlorosilane dropwise. mol (191.5ml), while raising the temperature to reflux for about 9 hours, the reaction was completed, cooled to normal temperature, added 500ml of water, stirred and separated, and then collected 113 degree fractions, the yield was 81.2%, and the conversion rate of the material was 92.17%.

Embodiment 2

[0028] According to the steps of Example 1, first fill nitrogen into a 1500ml reactor, pump in 2.0mol (246.5ml) of solvent m-xylene, put in 1.2mol (46.8g) of potassium metal, raise the temperature to about 75 degrees, and slowly drop Add 1.4 mol (178.7 ml) of trimethylchlorosilane, and raise the temperature and reflux for about 10 hours at the same time. After the reaction is completed, cool to room temperature, add 600 ml of water, stir and separate, and then collect the 113-degree fraction with a yield of 81.9%. The conversion of the material The rate is 93.0%.

Embodiment 3

[0030] According to the steps of Example 1, first fill nitrogen into a 1500ml reactor, pump in 2.0mol of trimethylbenzene as a solvent, put in 1.1mol (42.9g) of metal potassium, raise the temperature to about 65 degrees, and slowly add trimethyl chloride dropwise Silane 1.6mol (204.2ml), while raising the temperature and refluxing for about 9 hours, the reaction was completed, cooled to normal temperature, added 500ml of water, stirred and separated, and then collected the 113 degree fraction, the yield was 80.1%, and the conversion rate of the material was 92.6%.

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Abstract

The present invention discloses a preparation method of an organic silicon material and concretely indicates a preparation method of hexamethyldisilane. The present invention considers one kind of two kinds of dimethylbenzene and trimethylbenzene as solvent, wherein, the dimethylbenzene is preferential; the solvent is put in a reactor under the state without oxygen, metal potassium is put into the solvent, then solution is heated to 60 DEG C to 85 DEG C, furthermore trimethylchlorosilane is added to react for certain time, finally the product can be obtained by normal separation method. The present invention has the advantages of saving energy, short reaction time, high product yield etc. The present invention can be widely applied to almost all national economic fields of the defense and military industry, the aviation and aerospace field, the electronic and electrical field, the building field, the machinery field, the metallurgy, the automobile field, the instrument field, the weaving field, the chemical industry, the light industry, the food field, the medical and health field, the personal health care field etc.

Description

technical field [0001] A method for preparing an organosilicon material, specifically a method for preparing hexamethyldisilane. Background technique [0002] Hexamethyldisilane is a kind of organosilicon material, which can be used as a terminator for polysiloxane chains. It is a new polymer synthetic material with dual characteristics of organic materials and inorganic materials. The English name of hexamethyldisilane: Hexamethyldisilane [0003] Chemical Structure: [0004] [0005] Molecular formula and molecular weight: C 6 h 18 Si 2 , 146 [0006] Properties: Appearance is colorless transparent liquid with pleasant fruity smell. Insoluble in water, soluble in xylene, benzene, ethylene glycol, dimethyl ether and other solvents. [0007] Uses: It can be used as a polysilane chain terminator and silylating agent, widely used in pharmaceutical synthesis, mainly used in the synthesis of ribavirin, cefpirome and other antibiotics. [0008] Hexamethyldisilane mater...

Claims

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Application Information

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IPC IPC(8): C07F7/08
Inventor 陈昌略郑金星金永进管宜河
Owner ZHEJIANG HAIZHOU PHARMA CO LTD
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