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Synthesis method for co-production of 1-fluoro-2-chloroethylene carbonate and 1, 2-difluoroethylene carbonate

A technology for difluoroethylene carbonate and chloroethylene carbonate is applied in the field of co-production of 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate, and can solve the problem of production The problems of low yield, complex process and low yield can achieve the effect of improving comprehensive competitiveness, simple reaction conditions and high production yield.

Pending Publication Date: 2022-01-07
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to provide a synthetic method for the co-production of 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate to solve the current problem of co-production of 1-fluoro-2-chloro The synthesis methods of ethylene carbonate and 1,2-difluoroethylene carbonate have complex processes and low production yields, especially at present, a single method for preparing fluoroethylene carbonate lacks a co-production mode of production, and Unable to recycle reactants, leading to technical problems of low yields

Method used

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Examples

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preparation example Construction

[0019] Specifically, the embodiment of the present application provides a synthetic method for the co-production of 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate, including the steps of: The heavy component at the bottom of the tower is distilled under reduced pressure, and the 1,2-dichloroethylene carbonate component within a specific temperature range is collected, and the 1,2-dichloroethylene carbonate is mixed with the fluoride, at the fluorination reaction temperature, The fluorination reaction is carried out under normal pressure conditions. After the reaction is completed, the chloride by-products of the reaction is removed by filtration; 1,2-dichloroethylene carbonate and 1-fluoro-2-chloroethylene carbonate are separated by three-column rectification ester and 1,2-difluoroethylene carbonate, 1,2-dichloroethylene carbonate is recycled back to the fluorination reaction to obtain 1-fluoro-2-chloroethylene carbonate and 1,2-difluorocarbonic acid Vi...

Embodiment 1

[0031] Weigh 500g of vinylene carbonate crude retort column bottom heavy components for vacuum distillation, keep the vacuum at -0.099MPa, collect 1,2-dichloroethylene carbonate components in the range of 105-110°C, transfer to fluorinated Reactor, after adding 125g of magnesium fluoride, start stirring, carry out nitrogen replacement until the oxygen content is less than 0.3%, raise the temperature to 120°C for fluorination reaction, after 15 hours of reaction, vacuum filter to remove the reaction by-product magnesium chloride. Separation of 1,2-dichloroethylene carbonate, 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate, 1,2-dichloroethylene carbonate by three-column rectification Cycle back to the fluorination reaction to obtain 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate products.

Embodiment 2

[0033] Weigh 500g of vinylene carbonate crude retort column bottom heavy components for vacuum distillation, keep the vacuum at -0.099MPa, collect 1,2-dichloroethylene carbonate components in the range of 105-110°C, transfer to fluorinated Reactor, after adding 145g of calcium fluoride, start stirring, carry out nitrogen replacement until the oxygen content is less than 0.3%, raise the temperature to 140°C for fluorination reaction, after 15 hours of reaction, vacuum filter to remove the reaction by-product magnesium chloride. Separation of 1,2-dichloroethylene carbonate, 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate, 1,2-dichloroethylene carbonate by three-column rectification Cycle back to the fluorination reaction to obtain 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate products.

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Abstract

The invention discloses a synthesis method for co-production of 1-fluoro-2-chloroethylene carbonate and 1, 2-difluoroethylene carbonate. The synthesis method comprises the following steps: mixing 1, 2-dichloroethylene carbonate with a fluoride, carrying out fluorination reaction at a fluorination reaction temperature under normal pressure, and after the reaction is finished, filtering to remove chloride which is a byproduct of the reaction; and separating 1, 2-dichloroethylene carbonate, 1-fluoro-2-chloroethylene carbonate and 1, 2-difluoroethylene carbonate through three-tower rectification, and recycling 1, 2-dichloroethylene carbonate to a fluorination reaction to obtain 1-fluoro-2-chloroethylene carbonate and 1, 2-difluoroethylene carbonate products. According to the invention, 1, 2-dichloroethylene carbonate is a heavy component in a vinylene carbonate synthesis process and accounts for about 9-15% of a chlorination reaction product, the dichloroethylene carbonate byproduct is subjected to resource utilization, and the 1-fluoro-2-chloroethylene carbonate is co-produced, so that the production yield is increased.

Description

technical field [0001] The invention relates to the technical field of production methods of fluoroethylene carbonate, in particular to a synthesis method for co-producing 1-fluoro-2-chloroethylene carbonate and 1,2-difluoroethylene carbonate. Background technique [0002] 1-Fluoro-2-chloroethylene carbonate is a high-boiling component at the bottom of the tower during the production of vinylene carbonate VC. If it cannot be further processed and utilized, it will become a hazardous waste. Fluoroethylene 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 electrolyt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36
CPCC07D317/36
Inventor 谢传欣吴杰
Owner QINGDAO UNIV OF SCI & TECH