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Method for synthesizing fluoroethylene carbonate by phase-transfer catalysis

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of phase-transfer catalytic synthesis of fluoroethylene carbonate, and can solve problems such as difficult-to-control reactions, safety accidents, and unsuitability for industrial production

Inactive Publication Date: 2010-10-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

However, this method is difficult to control the progress of the reaction, has special requirements for equipment, and has very high requirements for the production process, and the post-treatment of excess fluorine gas is also very troublesome, otherwise safety accidents are likely to occur
[0006] Another synthetic method is also mentioned in the literature. Hideki Ishii et al [Tetrahedron57 (2001) 9067-9072] adopt the method of electrochemical partial fluorination, using vinylene carbonate (VC) as the starting material, and undergo a two-step reaction Synthesized fluoroethylene carbonate, but this method has low yield and high cost, and is not suitable for industrial production

Method used

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  • Method for synthesizing fluoroethylene carbonate by phase-transfer catalysis

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Effect test

Embodiment 1

[0021] Add 245 grams of chloroethylene carbonate to a dry 1000 milliliter three-necked flask, add 400 milliliters of butanone, 170 grams of potassium fluoride, and 1 gram of 18-crown-6 at the same time, react by heating, and react for 4 hours at reflux temperature. After finishing, cooling, filtering, filtrate gas chromatographic analysis, analysis result shows that 80.5% chloroethylene carbonate reacts, and the selectivity of fluoroethylene carbonate is 85.4%.

Embodiment 2

[0023] Add 245 grams of chloroethylene carbonate to a dry 1000 milliliter three-necked flask, add 350 milliliters of butanone, 170 grams of potassium fluoride, and 1.5 grams of 18-crown-6 at the same time, heat the reaction, and react at 80 ° C for 7 hours. After finishing, cooling, filtering, gas chromatographic analysis of the filtrate, analysis result shows that 85.3% of chloroethylene carbonate reacts, and the selectivity of fluoroethylene carbonate is 82.7%.

Embodiment 3

[0025] Add 375 g of chloroethylene carbonate to a dry 1500 ml three-necked flask, simultaneously add 350 ml of acetonitrile, 250 g of potassium fluoride, and 2.0 g of 18-crown-6, heat the reaction, and reflux at 90° C. for 5 hours. After the reaction was finished, it was cooled, filtered, and the filtrate was analyzed by gas chromatography. The analysis results showed that 82.6% of chloroethylene carbonate had reacted, and the selectivity of fluoroethylene carbonate was 85.3%.

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Abstract

The invention relates to a method for synthesizing fluoroethylene carbonate by phase-transfer catalysis. The fluoroethylene carbonate is produced by performing halogen exchange reaction on chloroethylene carbonate and potassium fluoride under the catalysis of crown ether serving as a phase-transfer catalyst in aprotic solvent.

Description

technical field [0001] The invention relates to a method for synthesizing fluoroethylene carbonate by phase transfer catalysis. Specifically, it relates to chloroethylene carbonate, which carries out a halogen exchange reaction with potassium fluoride in an aprotic solvent under the catalysis of a phase transfer catalyst crown ether to generate a method for fluoroethylene carbonate. The fluoroethylene carbonate can be used as an additive for the electrolyte of the lithium-ion secondary battery to improve the cycle life of the battery and improve the safety performance of the battery. Background technique [0002] The fluoroethylene carbonate referred to in the present invention is a compound having the following structure. [0003] [0004] McMillan R (J.Power Sources 1999, 81~82:20) etc. added fluoroethylene carbonate to 1mol / L LiPF 6 / PC+EC electrolyte system, the capacity retention rate of the battery after 200 cycles is 73%, and the battery current efficiency reache...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42B01J31/02H01M10/40
Inventor 吴茂祥方桂煌潘荧黄剑莹卢碧强
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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