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Synthetic method of fluoro ethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of catalytic synthesis, can solve problems such as the need to increase the yield, and achieve the effects of easy realization, high reaction yield, and abundant sources of raw materials

Active Publication Date: 2013-03-27
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Improve the conversion rate to 78.5%, but the yield still needs to be improved

Method used

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  • Synthetic method of fluoro ethylene carbonate
  • Synthetic method of fluoro ethylene carbonate
  • Synthetic method of fluoro ethylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 500g of chloroethylene carbonate and 1000g of N,N-dimethylformamide (DMF) to a 2000ml four-neck round bottom flask equipped with mechanical stirring, thermometer and reflux condenser, stir and mix well, then add 357g of KF solid and 1.5 g β-cyclodextrin. Heat up to 30°C in an oil bath. After 3 hours of heat preservation and reaction, filter. After washing the filter cake with DMF, 1632g of filtrate was obtained. The solution was analyzed, and the mass of fluorinated ethylene carbonate (FEC) in the filtrate was measured by gas chromatography to be 404.7g, and the yield of FEC reached 93.5%.

Embodiment 2

[0031] In the 2000ml four-necked round-bottom flask that is equipped with mechanical stirring, thermometer, reflux condenser, add 500g chloroethylene carbonate and 500g N,N-dimethylformamide (DMF) and 500g acetonitrile, after stirring and mixing, 476 g of KF solids were added along with 5.0 g of α-butyl-cyclodextrin. Heat up to 40°C in an oil bath. After 3 hours of heat preservation and reaction, filter. This solution was analyzed, and the quality of FEC contained in the filtrate was 406.6g as measured by gas chromatography. The yield of the final product FEC reached 93.9%.

Embodiment 3

[0033] Add 500g of chloroethylene carbonate and 1000g of tetrahydrofuran to a 2000ml four-necked round-bottomed flask equipped with mechanical stirring, a thermometer, and a reflux condenser. After stirring and mixing, add 288g of potassium fluoride solid and 4.5g of γ-ethane base-cyclodextrin. Heat up to 50°C in an oil bath. After 2.5 hours of heat preservation reaction, it was filtered. The solution was analyzed, and the content of fluoroethylene carbonate (FEC) measured by gas chromatography was 402.9g, and the conversion rate of FEC reached 93.1%.

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Abstract

The invention relates to a synthetic method of fluoro ethylene carbonate. The synthetic method is characterized by comprising the following steps: carrying out halogen exchange reaction of fluoro ethylene carbonate as a starting material and a potassium fluoride fluridizer in an organic solvent; and using cyclodextrin as a phase transfer catalyst and quickly converting the mixture into the fluoro ethylene carbonate in the reaction. The synthetic method provided by the invention is simple in process and high in selectivity, and the yield can reach over 93%.

Description

[0001] technical field [0002] The invention relates to the technical field of catalytic synthesis, and relates to a method for synthesizing fluoroethylene carbonate, in particular to a method for synthesizing fluoroethylene carbonate through phase transfer catalysis. Background technique [0003] The market for secondary lithium-ion batteries has developed rapidly in recent years, and they are increasingly used in mobile phones, notebook computers, digital imaging equipment, hand-held electric tools, electric bicycles, and electric vehicles. Therefore, higher requirements are placed on the performance of the battery. Improving the safety and stability of batteries and improving the cycle life have become the primary tasks to be solved urgently. [0004] Electrolyte additives have attracted much attention because of their small addition amount and obvious improvement in the performance of lithium-ion batteries. Fluoroethylene carbonate can improve the performance o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
Inventor 刘红光张洪源叶学海周立山郭西凤吴巍
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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