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Preparation method and application of fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of organic synthesis, can solve problems such as difficult separation, long reaction time, and performance degradation of lithium batteries, and achieve mild reaction conditions, short reaction time, and good safety Effect

Active Publication Date: 2020-04-10
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Fluoroethylene carbonate can be used as a medicine, pesticide intermediate and applied to lithium batteries, which can effectively improve the SEI film-forming performance of lithium batteries, form a dense protective layer, reduce impedance, prevent the decomposition of the electrolyte, and improve the high temperature of the electrolyte. low temperature performance, but there are still some defects more or less about the method for preparing fluoroethylene carbonate in the prior art: for example, it is not easy to separate after the reaction, the yield and the purity are low (the low purity will cause the extremely low performance of the lithium battery. Great drop, such as purity 99.9% and 99%, two kinds of purity of fluoroethylene carbonate applied to lithium battery will cause great difference in the cycle performance of lithium battery), the reaction time is too long, not conducive to industrial applications, etc.
This method uses KF as fluorinating agent, the reaction time is long, and the yield is only 61%.

Method used

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  • Preparation method and application of fluoroethylene carbonate
  • Preparation method and application of fluoroethylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Under nitrogen protection, add 80 g of anhydrous sodium bifluoride, 0.4 g of tetraphenylphosphine bromide (TPPB), 200 ml of ethyl acetate into the reaction vessel, stir and raise the temperature to 70 ° C, and dropwise add 250 g of chloroethylene carbonate (CEC) ( The purity is 82.5%, purchased from Zhangjiagang Bairuisi), dripping in 1 hour, 77 ° C for 2 hours, cooled to 40 ° C for suction filtration, the filter residue was rinsed twice with 100 ml ethyl acetate, and the combined filtrate was decompressed to remove the solvent to obtain a Fluoroethylene carbonate crude product 168g, GC content 80.5%, yield 94.4%.

Embodiment 2

[0032] Under the protection of nitrogen, add 90 g of anhydrous potassium hydrogen fluoride, 0.6 g of tetrakis(diethylamine) phosphonium bromide (TPB), 200 ml of dimethyl carbonate into the reaction vessel, stir and raise the temperature to 80°C, and start adding monochloroethylene carbonate dropwise Ester (CEC) 250g (purity: 82.5%), dripped in 1 hour, kept at 90°C for 2 hours, cooled to 40°C for suction filtration, rinsed the filter residue twice with 100ml ethyl acetate, combined the filtrate to remove the solvent under reduced pressure to obtain monofluoro The crude ethylene carbonate was 173g, the GC content was 78.52%, and the yield was 97.1%.

Embodiment 3

[0034] Under nitrogen protection, 112 g of anhydrous potassium hydrogen fluoride, 0.9 g of tetrakis(diethylamine) phosphonium bromide (TPB), 250 ml of methyl tert-butyl ether were added to the reaction vessel, and the temperature was raised to 55°C with stirring to start adding dichloride Ethylene carbonate (DCEC) 200g (purity: 97.2%, Zhangjiagang Bairuisi), dripped in 2 hours, kept at 60°C for 2 hours, cooled to 40°C for suction filtration, rinsed the filter residue twice with 100ml ethyl acetate, combined the filtrates and reduced pressure The solvent was removed to obtain 148g of crude difluoroethylene carbonate, the GC content was 84.5%, and the yield was 96.9%.

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Abstract

The invention discloses a preparation method and an application of fluoroethylene carbonate. The preparation method comprises the following steps: adding alkali metal hydrofluoride, a quaternary phosphonium salt and an organic solvent into a reaction container in the presence of a protective gas, performing mixing, heating the obtained mixture to 45-100 DEG C, dropwisely adding chloroethylene carbonate into the reaction container, and performing a reaction to obtain the fluoroethylene carbonate, wherein the alkali metal hydrofluoride is anhydrous potassium hydrofluoride and / or anhydrous sodiumhydrofluoride. The invention also discloses the application of the prepared fluoroethylene carbonate in a lithium ion battery. The preparation method has the advantages of realization of high-yield and high-purity preparation of the fluoroethylene carbonate, mild reaction conditions, good safety, and easiness in separation of the reaction product; and high-purity fluoroethylene carbonate with thepurity reaching 99.99% or above can be prepared through coarse distillation, vacuum distillation and melt crystallization, and is particularly suitable for lithium batteries.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to fluorine-containing additive 4-fluoroethylene carbonate (FEC) and / or difluoroethylene carbonate (FEC) for lithium ion batteries 2 EC), in particular to a preparation method and application of fluoroethylene carbonate. Background technique [0002] Fluoroethylene carbonate can be used as a medicine, pesticide intermediate and applied to lithium batteries, which can effectively improve the SEI film-forming performance of lithium batteries, form a dense protective layer, reduce impedance, prevent the decomposition of the electrolyte, and improve the high temperature of the electrolyte. low temperature performance, but there are still some defects more or less about the method for preparing fluoroethylene carbonate in the prior art: for example, it is not easy to separate after the reaction, the yield and the purity are low (the low purity will cause the extremely low performance of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42H01M10/0525H01M10/0567
CPCC07D317/42H01M10/0525H01M10/0567Y02E60/10
Inventor 汪许诚王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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