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Synthesis method of hexamethyl disilane

A technology of hexamethyldisilane and a synthesis method, which is applied in the directions of organic silicon compounds, chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, etc. and other problems, to achieve the effect of facilitating industrial production, improving activity, and being easy to control

Inactive Publication Date: 2018-02-02
常州润联化工有限公司
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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 method of hexamethyldisilane relates to a chemical process. Under anaerobic conditions, the temperature is raised and stirred in a reaction kettle filled with xylene, crown ether and metal sodium, and trimethylchlorosilane is added dropwise into the reaction kettle , after the end, control the temperature in the reactor, keep warm, and then lower the temperature to 50°C ± 5°C, add water dropwise to the reactor, let it stand for stratification, and distill and dehydrate through an oil-water separator to obtain the crude product Liujia base disilane. The present invention uses metal sodium and trimethylchlorosilane to react with the participation of crown ether, changes the potential of metal sodium, improves the activity of metal sodium, and makes it react with trimethylchlorosilane, and the crude product yield can reach 73.17%; The process of the invention is simple, easy to control and convenient for industrialized production.

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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IPC IPC(8): C07F7/08
CPCC07F7/0801C07F7/0805
Inventor 言兆福
Owner 常州润联化工有限公司
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