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Preparation method of 1,3-divinyl-1,1,3,3-tetramethyldisilazane

A technology of tetramethyldisilazane and dimethylvinylchlorosilane, applied in the field of battery electrolyte additives, can solve problems such as unsatisfactory effect, loss of environment, pollution, etc., so as to prevent serious losses and environmental pollution, improve Productivity, the effect of avoiding complex operations

Inactive Publication Date: 2019-05-21
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although conventional battery additives have a certain effect, the amount of addition used is large and the effect is not ideal. Therefore, it is urgent to seek a new battery additive to improve and solve battery performance problems.
[0003] 1,3-divinyl-1,1,3,3-tetramethyldisilazane with CAS No. 7691-02-3, molecular weight 185.414, currently synthesized 1,3-divinyl-1,1 , The method of 3,3-tetramethyldisilazane mainly uses dimethylvinylchlorosilane as raw material, feeds ammonia gas into it for reaction, and adds salt-dissolving agent for extraction, with high yield and high purity , but the complex operation of filtering and desalting after adding the salt-dissolving agent will cause serious losses and environmental pollution, especially the high content of ammonium chloride and tetramethyldivinyldisiloxane impurities, which seriously restricts the 1,3 -Application promotion of divinyl-1,1,3,3-tetramethyldisilazane

Method used

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  • Preparation method of 1,3-divinyl-1,1,3,3-tetramethyldisilazane
  • Preparation method of 1,3-divinyl-1,1,3,3-tetramethyldisilazane

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Experimental program
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Effect test

Embodiment 1

[0021] Add 2mol of dimethylvinyl chlorosilane to the reaction kettle, feed ammonia to it for reaction, the amount of ammonia is controlled to be 2:3.4 molar ratio of dimethyl vinyl chlorosilane and ammonia, within 2 hours Access 99%,

[0022] A. Control the reaction pressure to 5 kg NH 3 Pressure, 130 ° C reaction, the reaction time is 6h, after the reaction, add dichloroethane to dissolve the product;

[0023] B. Adding the above product into hydroquinone, tert-butylcatechol and copper naphthenate in a total amount of 0.05% of the product mass, carry out molecular distillation at a temperature of 160-163° C. and 760 mmHg to obtain a colorless transparent liquid. The product content is 98.95%, and the yield is 98%. The tested product density is 0.819g / cm 3 , ammonium chloride is 0, tetramethyldivinyldisiloxane content is 0.1%, the 1H NMR of the product: 400MHz, CDCl 3 Such as figure 1 Shown, 13C NMR: CDCl 3 Such as figure 2 As shown, the infrared spectrum is as image...

Embodiment 2

[0025] Add 2mol of dimethylvinyl chlorosilane to the reaction kettle, feed ammonia to it for reaction, the amount of ammonia is controlled to be the molar ratio of dimethyl vinyl chlorosilane to ammonia 2:3.3, within 2 hours Access 99%,

[0026] A. Control the reaction pressure to 3 kg NH 3 Pressure, 150 ° C reaction, the reaction time is 1h, after the reaction, add dichloroethane to dissolve the product;

[0027] B. Add the above product into hydroquinone, tert-butylcatechol and copper naphthenate in a total amount of 0.08% of the product mass, carry out molecular distillation at a temperature of 160-163° C. and 760 mmHg to obtain a colorless transparent liquid. The product content is 98.83%, and the yield is 97.6%. The tested product density is 0.82g / cm 3 , ammonium chloride is 0, and the content of tetramethyldivinyldisiloxane is 0.12%.

Embodiment 3

[0029] Add 2mol of dimethylvinyl chlorosilane to the reactor, feed ammonia to it for reaction, the amount of ammonia is controlled to be 2:3.1 molar ratio of dimethyl vinyl chlorosilane to ammonia, within 2 hours Access 99%,

[0030] A. Control the reaction pressure to 2 kg NH 3 Pressure, 140 ° C reaction, the reaction time is 4h, after the reaction is completed, add dichloroethane to dissolve the product;

[0031] B. Add the above product into hydroquinone, tert-butylcatechol and copper naphthenate in a total amount of 0.1% of the product mass, carry out molecular distillation at a temperature of 160-163° C. and 760 mmHg to obtain a colorless transparent liquid. The product content is 98.86%, and the yield is 98.2%. The tested product density is 0.821g / cm 3 , ammonium chloride is 0, and the content of tetramethyldivinyldisiloxane is 0.11%.

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Abstract

The invention relates to a preparation method of 1,3-divinyl-1,1,3,3-tetramethyldisilazane and belongs to the technical field of battery electrolyte additives. The preparation method takes trimethyl-vinyl chlorosilane as a raw material, and ammonia is introduced into trimethyl-vinyl chlorosilane for reaction. The preparation method comprises the following steps: A, controlling pressure to 2-5 kg NH3 pressure, performing the reaction at 80-150 DEG C for 1-6 hours, and after the reaction ends, adding a dichloroethane digestion product, and B, adding the product into a polymerization inhibitor, and performing molecular distillation under the condition of a temperature of 35-85 DEG C and a vacuum degree of 1-5 Pa to obtain colorless and clear liquid. The preparation method is simple; through combination of temperature control and post-treatment operation, and prepared 1,3-divinyl-1,1,3,3-tetramethyldisilazane is high in yield and purity and more suitable for the battery electrolyte additives.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, and relates to the use of 1,3-divinyl-1,1,3,3-tetramethyldisilazane as an additive for electrolytes to improve the performance of electrolytes and batteries , specifically relates to a preparation method of 1,3-divinyl-1,1,3,3-tetramethyldisilazane. The preparation method of the present invention is simple, and the 1,3-divinyl-1,1,3,3-tetramethyldisilazane prepared by temperature control combined with post-treatment operation has high yield and high purity, and is more suitable for use in Additives for battery electrolytes. Background technique [0002] With the development of my country's electronic information industry, the demand for chemical power is increasing, and its performance requirements are getting higher and higher. Lithium-ion batteries are widely used in various electronic devices such as notebook computers, mobile phones, and MP4s because of their advantage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10H01M10/0567
CPCY02E60/10
Inventor 武利斌刘鹏郝俊
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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