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Preparation method of high-purity difluoroethylene carbonate

A technology of difluoroethylene carbonate and dichloroethylene carbonate, which is applied in the field of preparation of difluoroethylene carbonate, can solve the problems of non-recyclable catalyst, long reaction time, troublesome handling, etc., and improve the utilization rate of atoms , high atomic utilization rate, and the effect of reducing solid waste

Inactive Publication Date: 2020-01-14
江苏瀚康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are disadvantages such as long reaction time, many side reactions, troublesome post-reaction treatment, and non-recyclable catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 161.21g (1.0mol) triethylamine trihydrofluoride and 350mL dimethyl carbonate to a 1L three-necked flask successively, add 207.44g (2.05mol) triethylamine to the three-necked flask, stir to make it uniform, and test Its pH is 5, 238.68g (1.45mol) of high-purity (98.35%) dichloroethylene carbonate is added dropwise into a three-necked flask, reacted at 45°C for 3.5h, and the content of dichloroethylene carbonate is 0.08 %, the reaction is terminated. Then the reaction solution was suction filtered, washed 3 times with dimethyl carbonate, and 177.22 g of crude product was obtained after distillation under reduced pressure, wherein the content of difluoroethylene carbonate in the crude product was 98.15%, and the molar yield was 96.74%. Finally, triethylamine can be recovered from the filter cake.

Embodiment 2

[0022] Add 169.27g (1.05mol) triethylamine trihydrofluoride and 350mL dimethyl carbonate successively into a 1L three-necked flask, add 217.56g (2.15mol) triethylamine into the three-necked flask, stir to make it uniform, and test Its pH is 5, and 247.66g (1.55mol) of high-purity (98.23%) dichloroethylene carbonate is added dropwise into a three-necked flask, reacted at 35°C for 5h, and the content of dichloroethylene carbonate is 0.09%. , the reaction terminates. Then the reaction solution was suction filtered, washed 3 times with dimethyl carbonate, and 189.54 g of crude product was obtained after distillation under reduced pressure, wherein the content of difluoroethylene carbonate in the crude product was 98.25%, and the molar yield was 96.89%. Finally, triethylamine can be recovered from the filter cake.

Embodiment 3

[0024] Add 145.09g (0.9mol) triethylamine trihydrofluoride and 300mL dimethyl carbonate successively into a 1L three-necked flask, add 187.20g (1.85mol) triethylamine into the three-necked flask, stir to make it uniform, and test Its pH is 6, and 207.46g (1.3mol) of high-purity (98.35%) dichloroethylene carbonate is added dropwise into a three-necked flask, reacted at 40°C for 4h, and the content of dichloroethylene carbonate is 0.13%. , the reaction terminates. Then the reaction solution was suction filtered, washed 3 times with dimethyl carbonate, and 159.38 g of crude product was obtained after distillation under reduced pressure, wherein the content of difluoroethylene carbonate in the crude product was 98.17%, and the molar yield was 97.06%. Finally, triethylamine can be recovered from the filter cake.

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PUM

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Abstract

The invention discloses a preparation method of high-purity difluoroethylene carbonate, which comprises the following steps: 1) adding a certain amount of triethylamine trihydrofluoride into a container at room temperature, and adding a proper amount of a solvent; 2) adding a certain amount of triethylamine into an obtained solution until the pH value reaches 4-7, and stirring uniformly; 3) dropwise adding a certain amount of high-purity dichloroethylene carbonate into the solution, reacting at a certain reaction temperature, and monitoring the reaction process by using gas chromatography; 4)performing suction filtration and washing after the reaction is finished, and performing reduced pressure distillation to obtain difluoroethylene carbonate, and 5) recovering a generated filter cake to obtain triethylamine. The preparation method of high-purity difluoroethylene carbonate provided by the invention is simple in process, low in reaction temperature, low in energy consumption, environment-friendly, less in solid waste, high in atom utilization rate, high in yield and suitable for large-scale production of enterprises.

Description

technical field [0001] The invention relates to the field of electrolyte additives for lithium ion batteries, in particular to a preparation method of difluoroethylene carbonate which can be used as an additive for electrolytes of lithium ion batteries. Background technique [0002] Difluoroethylene carbonate (DFEC) is an important electrolyte additive for lithium-ion batteries, which can improve the low-temperature performance of the electrolyte, increase the flash point of the electrolyte, enhance the cycle performance of the electrolyte, and have good flame retardancy. [0003] The synthesis method of difluoroethylene carbonate in traditional technology (CN106905290A, CN107903240A) is to obtain difluoroethylene by dichloroethylene carbonate (DCEC) and solid fluoride (fluoride metal) under the condition of catalyst catalysis. Vinyl carbonate. However, there are disadvantages such as long reaction time, many side reactions, troublesome post-reaction treatment, and non-recy...

Claims

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Application Information

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IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 王海明翟涛纪加明傅圣超孔令文林涛
Owner 江苏瀚康新材料有限公司