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Method for purifying fluoroethylene carbonate

A technology of ethylene carbonate and a purification method, which is applied in the field of preparation of fluoroethylene carbonate, can solve problems such as unsatisfactory fluoroethylene carbonate, and achieve the effect of simple operation

Active Publication Date: 2009-12-09
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the distillation purification method commonly used in industry cannot obtain fluoroethylene carbonate that meets the requirements of lithium-ion electrolyte additives

Method used

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  • Method for purifying fluoroethylene carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] According to the preparation method of fluoroethylene carbonate of this embodiment, the specific process is as follows:

[0018] Add 880 grams of ethylene carbonate (content 99wt%) into a 2000ml stainless steel pressure vessel, install a 5W ultraviolet lamp, connect a stainless steel air duct and exhaust gas absorption device, heat up to 40°C, and feed 660g in a volume ratio of 1: 1 fluorine / nitrogen mixed gas, after the gas is introduced, 1011 g of crude fluoroethylene carbonate is obtained, wherein the content of fluoroethylene carbonate is 52.30 wt%, and the acidity of the crude product is 0.23%.

Embodiment 2

[0020] According to the preparation method of fluoroethylene carbonate of this embodiment, the specific process is as follows:

[0021] In a 5000ml four-necked flask, equipped with a stirrer and condenser, add 1680g of sodium fluoride, 3000ml of dimethyl carbonate and 5g of tetrabutylammonium bromide, stir, heat to 60℃, and drop 1225g of dimethyl carbonate. After the reaction is completed, the dimethyl carbonate is removed by distillation under reduced pressure to obtain 980 g of crude fluoroethylene carbonate, wherein the content of fluoroethylene carbonate is 75.62 wt%, and the acidity of the crude product is 1.3%.

Embodiment 3

[0023] According to the following unified method, 50g of the crude fluoroethylene carbonate obtained in Example 1 was recrystallized in a mixed solvent of different proportions of toluene and n-hexane at a temperature of -10°C, and then reduced under a vacuum of 665Pa-1064Pa Pressure distillation, collect the 84-85 ℃ fluoroethylene carbonate fraction as the product, the ratio of the mixed solvent, the amount, and the purity and acidity value of the product are shown in Table 1 on page 3 of the manual.

[0024] Table 1

[0025] Toluene (g)

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Abstract

The invention relates to a method for purifying fluoroethylene carbonate. The method ensures that fluoroethylene carbonate performs recrystallization in a mixed solvent of toluene and normal hexane at a temperature of between 30 DEG C below zero and 0 DEG C; and in the mixed solvent, the weight ratio of toluene to normal hexane is 1:1-10. After purification by the method, the content of the fluoroethylene carbonate is over 99.5 weight percent, and the acidity is below 0.005 percent, the fluoroethylene carbonate meets the requirement of lithium ion electrolyte additives, and the method has simple operation.

Description

Technical field [0001] The invention belongs to the technical field of preparation of fluoroethylene carbonate. Background technique [0002] Fluorinated ethylene carbonate, melting point 17-19℃, boiling point 200℃, structural formula: [0003] [0004] When fluoroethylene carbonate is used as a lithium ion battery electrolyte additive, its content is required to be above 99.5% by weight and acidity below 0.005%. At present, the distillation and purification methods commonly used in the industry cannot obtain fluoroethylene carbonate that meets the requirements of lithium ion electrolyte additives. Summary of the invention [0005] The technical problem to be solved by the present invention provides a purification method of fluoroethylene carbonate, which has good purification effect. [0006] In order to solve the above technical problems, the present invention adopts the following technical solutions: [0007] A method for purifying fluoroethylene carbonate. The method inclu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
Inventor 王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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