Synthesis method of tetraethylene silane

A technology of tetraethylene silane and synthesis method, which is applied in the direction of silicon organic compounds, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., and can solve incomplete substitution, low yield and purity, and difficulty in carrying out, etc. problem, to achieve the effect of less reaction steps, simple operation and improved yield

Pending Publication Date: 2022-05-13
SHIJIAZHUANG SAN TAI CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the preparation of tetraethylenesilane, vinylmagnesium chloride and silicon tetrachloride are mainly reacted in tetrahydrofuran solvent at present, but this reaction has problems such as difficulty in the late stage of substituti...

Method used

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  • Synthesis method of tetraethylene silane
  • Synthesis method of tetraethylene silane
  • Synthesis method of tetraethylene silane

Examples

Experimental program
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Embodiment 1

[0021] The synthetic method of tetraethylene silane, its synthetic steps are as follows:

[0022] 1) Preparation of vinylmagnesium chloride solution

[0023] Under the protection of nitrogen, take 9.724g (0.4mol) of magnesium chips and add them to 145.86mL of tetrahydrofuran, stir and heat to 65°C, pass in excess vinyl chloride gas, and keep stirring at 65°C to react until the magnesium chips completely disappear to obtain ethylene base magnesium chloride solution.

[0024] 2) Preparation of Tetraethylenesilane

[0025] Dissolve 16.7g (0.1mol) of tetrachlorosilane in 130mL of methyl tert-butyl ether, add 0.1g of catalyst magnesium iodide, control the temperature of the resulting system at 20°C, and slowly add All the above-mentioned vinylmagnesium chloride solutions (dropping time is 2h), after the dropwise addition, maintain 20°C and continue to stir for 2h for Grignard reaction, then slowly add 75mL of water dropwise to quench the reaction, and directly separate the phases...

Embodiment 2

[0028] The synthetic method of tetraethylene silane, its synthetic steps are as follows:

[0029] 1) Preparation of vinylmagnesium chloride solution

[0030] Under the protection of nitrogen, take 9.724g (0.4mol) of magnesium chips and add them to 155.58mL of tetrahydrofuran, stir and heat to 68°C, pass in excess vinyl chloride gas, and keep stirring at 68°C to react until the magnesium chips completely disappear to obtain ethylene base magnesium chloride solution.

[0031] 2) Preparation of Tetraethylenesilane

[0032] Dissolve 16.7g (0.1mol) of tetrachlorosilane in 133.6mL of methyl tert-butyl ether, add 0.05g of catalyst magnesium iodide, control the temperature of the resulting system at 24°C, and slowly drop Add all the above-mentioned vinylmagnesium chloride solutions (dropping time is 2.5h). After the dropwise addition, keep stirring at 24°C for 3h for Grignard reaction, and then slowly add 80mL of water dropwise to quench the reaction. After the reaction is completed...

Embodiment 3

[0034] The synthetic method of tetraethylene silane, its synthetic steps are as follows:

[0035] 1) Preparation of vinylmagnesium chloride solution

[0036] Under the protection of nitrogen, take 10.21g (0.42mol) of magnesium chips and add them to 158.26mL of tetrahydrofuran, stir and heat to 70°C, pass in excess vinyl chloride gas, and keep stirring at 70°C to react until the magnesium chips completely disappear to obtain ethylene base magnesium chloride solution.

[0037] 2) Preparation of Tetraethylenesilane

[0038] Dissolve 16.7g (0.1mol) of tetrachlorosilane in 116.9mL of methyl tert-butyl ether, add 0.08g of catalyst magnesium iodide, control the temperature of the resulting system at 25°C, and slowly drop Add all the above-mentioned vinylmagnesium chloride solutions (dropping time is 2.3h). After the dropwise addition, maintain 25°C and continue stirring for 2.5h for Grignard reaction, then slowly add 78mL of water dropwise to quench the reaction. After the reaction...

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Abstract

The invention discloses a synthesis method of tetraethylene silane, and relates to the technical field of battery electrolyte additives, and the synthesis method comprises the following steps: under the protection of an inert gas, dissolving tetrachlorosilane in methyl tert-butyl ether, adding a catalyst magnesium iodide, slowly dropwise adding a vinyl magnesium chloride solution into the obtained system, carrying out a Grignard reaction, and after the reaction is completed, carrying out a reaction to obtain the tetraethylene silane. And adding water for quenching, performing phase splitting, and performing vacuum concentration on the obtained organic phase to obtain the tetraethylene silane. The synthesis method provided by the invention is simple to operate, few in reaction steps and easy to purify, the product yield and the product purity in the production process are ensured to be maximized by controlling reaction conditions in each stage, and the product yield is further improved by reasonably controlling the dosage of reaction raw materials and the reaction process.

Description

technical field [0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of tetraethylenesilane. Background technique [0002] Tetraethylenesilane, as an important silane additive in lithium battery electrolyte, plays an important role in improving the stability of lithium batteries. It can improve the consistency of voltage when lithium batteries are shipped and screened, and reduce self-discharge. [0003] For the preparation of tetraethylenesilane, vinylmagnesium chloride and silicon tetrachloride are mainly used to react in tetrahydrofuran solvent, but this reaction has problems such as difficulty in the late stage of substitution reaction, resulting in incomplete substitution, and difficulty in subsequent purification. [0004] Therefore, the current preparation and purification methods for tetraethylenesilane are not perfect enough, which leads to low yield and purity. Contents of the invention [0005...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0805C07F7/0827
Inventor 刘鹏田丽霞张茜张民彭鹏鹏郝俊侯荣雪王军葛建民武利斌闫彩桥许晓丹闫朋飞杨世雄赵光华高山林胜赛李庆占邢艳召李晓辉牛庾鑫
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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