Method for preparing high-purity vinylene carbonate

A technology of vinylene carbonate and ethylene carbonate is applied in the field of preparation of high-purity electronic grade vinylene carbonate to achieve the effect of improving the degree of reaction and improving the purity

Active Publication Date: 2017-05-10
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

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preparation example Construction

[0017] The preparation method of high-purity vinylene carbonate of the present invention comprises the following steps: (a) chlorinating dry chlorine gas and ethylene carbonate under the irradiation of ultraviolet light to obtain chloroethylene carbonate; (b) preparing the The chloroethylene carbonate is dispersed in methyl silicone oil, and then an organic amine is added for elimination reaction to generate vinylene carbonate; the molar ratio of the chloroethylene carbonate to the organic amine is 1:1.1~1.5; ( c) The product obtained in step (b) is filtered and refined under reduced pressure. By carrying out the elimination reaction of chloroethylene carbonate and organic amine in methyl silicone oil, and controlling the ratio of chloroethylene carbonate and organic amine, the reaction degree can be improved, and the separation of each product can be facilitated to improve the purity of the product .

[0018] The organic amine is preferably a mixture of one or more of trieth...

Embodiment 1

[0021] The present embodiment provides a kind of preparation method of high-purity vinylene carbonate, and it comprises the following steps:

[0022] (a) Perform chlorination reaction between dry chlorine gas and ethylene carbonate under the irradiation of ultraviolet light to obtain chloroethylene carbonate. Please refer to the Chinese invention patent with application number 201510994430.4, specifically: drying Chlorine and ethylene carbonate with a flow rate of 30 L / h under ultraviolet light (100~200nm, 7.5 w / cm 2 ) under the irradiation of 35°C for chlorination reaction for 3 hours; followed by rectification at 130°C and a reflux ratio of 1:1 to obtain chloroethylene carbonate;

[0023] (b) Disperse 10 mol of chloroethylene carbonate prepared in step (a) in 10 L of methyl silicone oil, then add 6.125 g of hydroquinone and 11 mol of triethylamine and react at 30°C for 10 hours to form vinylene carbonate ;

[0024] (c) The product obtained in step (b) is subjected to sucti...

Embodiment 2

[0026] The present embodiment provides a kind of preparation method of high-purity vinylene carbonate, and it comprises the following steps:

[0027] (a) Perform chlorination reaction between dry chlorine gas and ethylene carbonate under the irradiation of ultraviolet light to obtain chloroethylene carbonate. Please refer to the Chinese invention patent with application number 201510994430.4, specifically: drying Chlorine and ethylene carbonate with a flow rate of 30 L / h under ultraviolet light (100~200nm, 7.5 w / cm 2 ) under the irradiation of 35°C for chlorination reaction for 3 hours; followed by rectification at 130°C and a reflux ratio of 1:1 to obtain chloroethylene carbonate;

[0028] (b) Disperse 10 mol of chloroethylene carbonate prepared in step (a) in 50 L of methyl silicone oil, then add 12.25 g of p-benzoquinone and 15 mol of ethanolamine to react at 55°C for 5 hours to generate vinylene carbonate;

[0029] (c) Suction filter the product obtained in step (b), take...

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Abstract

The present invention relates to a method for preparing high-purity vinylene carbonate. The method comprises the steps of (a) carrying out a chlorination reaction between ethylene carbonate and dry chlorine under the irradiation of ultraviolet light to produce chloroethylene carbonate; (b) dispersing chloroethylene carbonate into methylsilicone oil, then, adding an organic amine, and carrying out an elimination reaction to obtain vinylene carbonate, wherein the mole ratio of chloroethylene carbonate to the organic amine is 1: (1.1-1.5); and (c) refining the products obtained in the step (b) under reduced pressure. Through carrying out the elimination reaction between chloroethylene carbonate and the organic amine in the methylsilicone oil, and controlling the ratio of chloroethylene carbonate to the organic amine, the extent of the reaction can be improved, and the separation of each product can be facilitated, so as to increase the product purity.

Description

technical field [0001] The invention relates to a production method of vinylene carbonate, in particular to a preparation method of high-purity electronic grade vinylene carbonate. Background technique [0002] Vinylene carbonate is an important additive material for lithium battery electrolyte, which can form a dense and stable organic film on the surface of the battery. The organic film produces a polyalkyl lithium carbonate compound without loss of electrical conductivity and without increasing the internal resistance of the battery. This compound can effectively inhibit the insertion of solvent molecules and solvated lithium ions in graphite, reduce the decomposition of the electrolyte, and improve The stability of the graphite negative electrode improves the charge and discharge performance of the lithium battery. The lithium battery industry needs high-purity vinylene carbonate. [0003] Vinylene carbonate (VC for short) is a colorless transparent liquid. It is an or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 王小龙管国锋陆觉明万辉顾乃刚
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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