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Preparation method of bis-fluoro-ethylene carbonate

A technology of bisfluoroethylene carbonate and bischloroethylene carbonate, which is applied in the field of preparation of electrolyte additive bisfluoroethylene carbonate, can solve the problems of using a large amount of solvents, solid waste, solid-liquid separation, etc. To achieve the effect of simple process route, easy to obtain raw materials and cheap raw materials

Active Publication Date: 2013-05-22
ZHANGJIAGANG HICOMER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the following methods are mainly used to prepare difluoroethylene carbonate: dichloroethylene carbonate and fluoride are reacted in an organic solvent to produce a solution containing difluoroethylene carbonate, followed by filtration and separation, precipitation and rectification, etc. To obtain high-purity bisfluoroethylene carbonate, the above method has the following disadvantages: the reaction solution needs to be separated from the solid and liquid, and because there are many solid wastes, a large amount of solvent needs to be used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Add 209 g of dichloroethylene carbonate (purity: 75%, 1 mol) into a three-necked flask equipped with stirring, thermometer, condenser and tail gas absorption device; The hydrogen fluoride gas is continuously fed in at a speed of 0.5 L / min, and the nitrogen gas is continuously fed in at a speed of 0.5 L / min. The waste gas hydrogen fluoride and hydrogen chloride gas generated during the reaction are absorbed with lye. After 6 hours of heat preservation reaction, sampling analysis showed that dichloroethylene carbonate was 12.3%, and difluoroethylene carbonate was 60.1%; after heat preservation reaction for 12 hours, sampling analysis showed that dichloroethylene carbonate was 0.9%, and difluoroethylene carbonate was 0.9%. Substituted ethylene carbonate was 74.7%, and the reaction was over; (3) Rectification under reduced pressure, collecting 120g of 60-90°C / 100mmHg fraction (96.7% content), the yield was 93.6%.

Embodiment 2

[0022] (1) Add 184.7g of dichloroethylene carbonate (purity: 85%, 1mol) into a three-neck flask equipped with stirring, thermometer, condenser and tail gas absorption device, (2) Stir and heat up to 60°C, at 0.2L / min Continuously feed hydrogen fluoride gas at a speed of 1L / min, and at the same time continuously feed nitrogen gas at a speed of 1L / min. The waste gas hydrogen fluoride and hydrogen chloride gas generated during the reaction are absorbed with lye. After 4 hours of heat preservation reaction, sampling analysis showed that dichloroethylene carbonate was 7.6%, and difluoroethylene carbonate was 70.5%; after heat preservation reaction for 9 hours, sampling analysis showed that dichloroethylene carbonate was 0.5%, difluoroethylene Ethylene carbonate was 88.5%, and the reaction was over; (3) Rectification under reduced pressure, collecting fraction 118 at 60-90°C / 100mmHg (content: 97.8%), and the yield was 93.1%.

Embodiment 3

[0024] (1) Add 165.3 g of dichloroethylene carbonate (95% purity, 1 mol) into a three-necked flask equipped with stirring, thermometer, condenser and tail gas absorption device, (2) Stir and heat up to 60°C, at 0.3L / min Continuously feed hydrogen fluoride gas at a speed of 1L / min, and at the same time continuously feed nitrogen gas at a speed of 1L / min. The waste gas hydrogen fluoride and hydrogen chloride gas generated during the reaction are absorbed with lye. After 3 hours of heat preservation reaction, sampling analysis showed that dichloroethylene carbonate was 10.6%, and difluoroethylene carbonate was 83.3%; after heat preservation reaction for 6 hours, sampling analysis showed that dichloroethylene carbonate was 0.8%, difluoroethylene Substituted ethylene carbonate was 93.2%, and the reaction was over; (3) Rectification under reduced pressure, collecting 60-90°C / 100mmHg fraction 118 (content: 98.9%), the yield was 94.1%.

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Abstract

The invention discloses a preparation method of bis-fluoro-ethylene carbonate as an electrolyte additive. The preparation method comprises the following steps of: with bis-chloro-ethylene carbonate and hydrogen fluoride as raw materials, under the protection of nitrogen, carrying out reaction to obtain a mixture containing the bis-fluoro-ethylene carbonate by controlling the reaction temperature at 40-120 DEG C; and then carrying out distillation and purification on the mixture to obtain the bis-fluoro-ethylene carbonate as a needed product. The preparation method has the beneficial effects that the raw materials are cheap and easy to obtain, a process route is simple, no solid waste is generated, the yield is above 90 percent, and hydrogen fluoride as waste gas and hydrogen chloride gas are absorbed through alkali liquor without environmental pollution basically.

Description

technical field [0001] The invention relates to a method for preparing electrolyte additive bisfluoroethylene carbonate. Background technique [0002] Difluoroethylene carbonate is mainly used in the lithium ion electrolyte of lithium batteries. Difluoroethylene carbonate can effectively improve the high and low temperature resistance of lithium ion electrolyte and improve the flame retardancy of lithium ion electrolyte. Difluoroethylene carbonate has two structural formulas - cis and trans, and its structural formula is as follows: [0003] or [0004] At present, the following methods are mainly used to prepare difluoroethylene carbonate: dichloroethylene carbonate and fluoride are reacted in an organic solvent to produce a solution containing difluoroethylene carbonate, followed by filtration and separation, precipitation and rectification, etc. To obtain high-purity bisfluoroethylene carbonate, the above method has the following disadvantages: the reaction liquid...

Claims

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Application Information

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IPC IPC(8): C07D317/42
Inventor 刘冬许国荣姚双开钱裕佳
Owner ZHANGJIAGANG HICOMER CHEM CO LTD