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Industrial production method for electronic-grade fluoro-ethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, applied in the field of electrolyte additives, can solve the problems of many side reactions, poor selectivity, increase production cost, etc., to improve the purity of finished products, improve the quality level, and improve the reaction rate. Effect

Inactive Publication Date: 2017-07-04
SHANDONG YINGHUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Electrochemical fluorination and addition methods are currently limited to the laboratory development stage, and have disadvantages such as poor selectivity, high cost, and difficult control of the reaction. At present, the only industrial production method is the fluorine source replacement method
[0007] In the existing patented technology of fluorine source replacement: fluorine gas as a fluorine source has many side reactions, and the product purity is difficult to meet the standard; the acid value content of the product obtained by using hydrogen fluoride as a fluorine source cannot meet the requirements of electronic grade products, and subsequent processing is required to increase production costs; The use of fluosilicic acid or organic amine hydrofluoride as a fluorine source is limited to laboratory research and development, and industrialization is still early; in addition, although other technologies can improve reaction efficiency by adding initiators and catalysts, they are changed to increase subsequent rectification preparation The Difficulty of Electronic Grade Products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Feed industrial-grade chloroethylene carbonate with a purity of about 75% into the rectification kettle through a flow meter. The rectification kettle is rectified under negative pressure at 65°C and a pressure of 500Pa, and the light components and still residues are temporarily stored , when the purity of the positive fraction is greater than 99.5%, start to receive and enter the middle tank for collection;

[0025] (2) Replace the enamel reaction kettle with argon, and detect that the oxygen content is ≤50ppm and the moisture content is less than 0.3ppm. Then, the high-purity chloroethylene carbonate obtained by rectification is poured into the enamel reaction kettle through a metering pump, and the steam enamel reaction kettle is turned on. Valve and stirring switch, rotating speed 400r / min, raise the temperature of the material in the kettle to 60°C, then gradually add sodium bicarbonate and potassium fluoride with a purity greater than 99% and a moisture conten...

Embodiment 2

[0029] (1) Feed industrial-grade chloroethylene carbonate with a purity of about 75% into the rectification kettle through a flow meter. The rectification kettle is rectified under negative pressure at 65°C and a pressure of 500Pa, and the light components and still residues are temporarily stored , when the purity of the positive fraction is greater than 99.5%. Start to receive and enter the middle slot for collection;

[0030] (2) Replace the enamel reaction kettle with argon, and detect that the oxygen content is ≤50ppm and the moisture content is less than 0.3ppm. Then, the high-purity chloroethylene carbonate obtained by rectification is poured into the enamel reaction kettle through a metering pump, and the steam enamel reaction kettle is turned on. Valve and stirring switch, rotating speed 400r / min, raise the temperature of the material in the kettle to 60°C, then gradually add sodium carbonate and sodium fluoride with a purity greater than 99% and a moisture content of...

Embodiment 3

[0034] (1) Feed industrial-grade chloroethylene carbonate with a purity of about 75% into the rectification kettle through a flow meter. The rectification kettle is rectified under negative pressure at 65°C and a pressure of 500Pa, and the light components and still residues are temporarily stored , when the purity of the positive fraction is greater than 99.5%. Start to receive and enter the middle slot for collection;

[0035](2) Replace the enamel reaction kettle with argon, and check that the oxygen content is ≤50ppm and the moisture content is 50 ≤3μm, D max ≤10μm. The molar ratio of high-purity cesium fluoride and high-purity chloroethylene carbonate is 1:1.3, and the amount of potassium bicarbonate is 0.1% of the mass of high-purity chloroethylene carbonate; gradually add the reaction kettle, and control the temperature to ≤70°C. After all the cesium fluoride was added, the system reacted at 95°C for 8 hours, the reaction stopped when the content of chloroethylene car...

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Abstract

An industrial production method for electronic-grade fluoro-ethylene carbonate. The invention belongs to the technical field of electrolyte additives. The industrial production method includes the steps of: a) rectifying industrial-grade chloro-ethylene carbonate to increase purity; b) under protection of argon, adding high-purity fluoride salt, high-purity fluoro-ethylene carbonate and an inorganic deacidifier into a reaction kettle, so that the high-purity fluoride salt and the high-purity fluoro-ethylene carbonate are subjected to a halogen replacement reaction at 35-130 DEG C for 8-15 h, wherein molar ratio of the high-purity fluoride salt to the high-purity fluoro-ethylene carbonate is 1:1.1-1.3; and c) performing pressure-reduced rectification, water removal and re-crystallization to the product to obtain the electronic-grade product. The industrial production method achieves stable, high-effective and high-yield halogen replacement without usage of a solvent, an initiator and a catalyst.

Description

technical field [0001] The invention discloses an industrial production method of electronic-grade fluoroethylene carbonate, which belongs to the technical field of electrolyte additives. Background technique [0002] At present, lithium battery is one of the focuses of daily life that is well known and concerned by people, and the safety problem of lithium battery is one of the main obstacles hindering its development. The use of electrolyte additives can effectively improve the safety of the battery, increase the number of charge and discharge, and prolong the life of the battery. [0003] Fluoroethylene carbonate (hereinafter referred to as F-EC) is an important electrolyte additive for lithium-ion batteries. While inhibiting the decomposition of the electrolyte, it can significantly improve the safety and stability of lithium batteries, such as: cycle charging efficiency, high and low temperature resistance and stability. As people pay more and more attention to batter...

Claims

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Application Information

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IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 牛会柱
Owner SHANDONG YINGHUAN CHEM
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