Synthesis process of hexamethyldisilane

A technology of hexamethyldisilane and a synthesis method, applied in directions such as organic silicon compounds, can solve problems such as unfavorable industrialized production, flammability and explosion, and shortage of raw materials, and achieve the effects of convenient industrialized production, simple process, and easy control.

Active Publication Date: 2009-02-04
扬州三友合成化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There are currently two synthesis techniques for hexamethyldisilane reported in the literature: one is to react with lithium metal and trimethylchlorosilane, but it needs high temperature and high pressure, and hardly reacts under normal temperature and pressure, which is not conducive to industrial production; the other is Reaction with metal potassium and trimethylchlorosilane, although the yield is about 75%, but metal potassium is very expensive, and the raw materials are in short supply. In addition, metal potassium is very active, extremely flammable and explosive, and the process is difficult to control. Domestic fresh There is industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0014] Pump about 200kg of xylene and 550kg (2.5kmol) of 15-crown-5 into a dry 1500L stainless steel reactor with a condensing reflux system in sequence, and replace the closed system with nitrogen for 3 to 5 times. Add nitrogen to the kettle to a state slightly higher than normal pressure (0.01-0.02Mpa), then open the vent valve, and quickly add 28.8kg (1.25kmol) of metal sodium into the kettle through the manhole under the purging of a slight nitrogen flow , cover the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a state of under the protection of nitrogen atmosphere.

[0015] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours, after the metallic sodium i...

example 2

[0021] Pump about 300kg of xylene and 440kg (2kmol) of 15-crown-5 into a dry 1500L stainless steel reaction kettle with a condensing reflux system in sequence, and replace the closed system with nitrogen for 3 to 5 times. Supplement nitrogen to the state slightly higher than normal pressure (0.01~0.02Mpa), then open the vent valve, and under the purging of slight nitrogen flow, quickly add 30kg (1.30kmol) of metal sodium into the kettle through the manhole at one time, cover Put on the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a nitrogen atmosphere under the protection of

[0022] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours, after the metallic so...

example 3

[0027] Pump about 250kg of xylene and 550kg (2.5kmol) of 15-crown-5 into a dry 1500L stainless steel reactor with a condensing reflux system, and replace the closed system with nitrogen for 3 to 5 times. Supplement nitrogen in the kettle to a state slightly higher than normal pressure (0.01-0.02Mpa), then open the vent valve, and quickly add 23kg (1kmol) of metal sodium into the kettle through the manhole under the purging of a slight nitrogen flow, cover Put on the manhole cover, replace the closed system with nitrogen for 5 times, add nitrogen to the kettle for the last time to a state slightly higher than normal pressure (0.01-0.02Mpa), open the open system, so that the entire material and its reaction process are in a nitrogen atmosphere under the protection of

[0028] Heating through the jacket steam, slowly raising the temperature to 95°C-100°C (the heating process takes 1 hour), and keeping it at this temperature for 0.5 hours. First drop a small amount of trimethylch...

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Abstract

The synthesis process of hexamethyldisilane is one kind of chemical technological process. The process includes the following steps: throwing xylene, crown ether and metal sodium into reaction kettle in oxygen free condition; heating via stirring and dropping trimethylchlorosilane to react under controlled temperature; maintaining the temperature after reaction for certain time and lower the temperature inside the reaction kettle to 50 deg.c; dropping water into the kettle and settling to delaminate; and distilling in an oil-water separator to obtain crude hexamethyldisilane product. The present invention makes crown ether to participate the reaction of metal sodium and trimethylchlorosilane, and this can alter the potential of metal sodium, raise the activity of metal sodium and raise the crude hexamethyldisilane product yield to 73.17 %.

Description

technical field [0001] The invention relates to a chemical process, in particular to a method for chemically synthesizing hexamethyldisilane. Background technique [0002] There are currently two synthesis techniques for hexamethyldisilane reported in the literature: one is to react with lithium metal and trimethylchlorosilane, but it needs high temperature and high pressure, and hardly reacts under normal temperature and pressure, which is not conducive to industrial production; the other is Reaction with metal potassium and trimethylchlorosilane, although the yield is about 75%, but metal potassium is very expensive, and the raw materials are in short supply. In addition, metal potassium is very active, extremely flammable and explosive, and the process is difficult to control. Domestic fresh There is industrial production. Contents of the invention [0003] The object of the present invention is to invent a synthetic method of hexamethyldisilane, which is easy to produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
Inventor 张才山陆灯宏孙健韦善美
Owner 扬州三友合成化工有限公司
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