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Synthesis method for fluoro-ethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate is applied in the field of battery stabilizers, which can solve the problems of reduced production efficiency, long production time, and many side reactions, and achieves reduced production time, convenient separation, and fewer side reactions. Effect

Active Publication Date: 2017-07-04
山东永浩新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing fluoroethylene carbonate preparation methods mainly include: electrochemical fluorination, displacement fluorination, addition fluorination, etc. Among these methods, electrochemical fluorination and addition fluorination have poor selectivity and many side reactions. Disadvantages such as higher cost
The current industrial method is to replace fluoride with fluorine source. The fluorine source is generally potassium fluoride, sodium fluoride, silver fluoride, antimony trifluoride, antimony pentafluoride, calcium fluoride, etc. The yield is generally about 70%, which is mainly due to the occurrence of side reactions leading to low yield. At the same time, due to the intense heat release of the reaction, the fluorinating agent needs to be added in batches for multiple times, which leads to longer production time and lower production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Replace the enamel reaction kettle with nitrogen, and detect that the oxygen content is ≤50ppm and the moisture content is less than 10ppm, then add anhydrous high-purity mixed fluoride into the reaction kettle through the hand hole, and the mixed fluoride is tripropyltin fluoride and fluoride Potassium is uniformly mixed at a mass ratio of 25:1; the chloroethylene carbonate and solvent are injected into the enamel reaction kettle through a metering pump, and the solvent is a mixed solvent of methyl tert-butyl ether and acetonitrile at a mass ratio of 3:17 The molar ratio of chloroethylene carbonate to mixed fluoride is 1:1.05, and the mass ratio of chloroethylene carbonate to solvent is 1:1.1; open the steam valve and stirring switch of the enamel reaction kettle, and the speed is 500r / min. Raise the temperature of the material in the kettle to 81°C and react for 3 hours. When the content of chloroethylene carbonate is less than or equal to 2%, the reaction stops, a...

Embodiment 2

[0023] (1) Replace the enamel reaction kettle with nitrogen, and detect that the oxygen content is ≤50ppm and the moisture content is less than 10ppm, then add anhydrous high-purity mixed fluoride into the reaction kettle through the hand hole, and the mixed fluoride is tripropyltin fluoride and fluoride Potassium is uniformly mixed at a mass ratio of 23:1; and the chloroethylene carbonate and solvent are injected into the enamel reaction kettle through a metering pump, and the solvent is a mixture of methyl tert-butyl ether and acetonitrile at a mass ratio of 2:19 Solvent; the molar ratio of chloroethylene carbonate to mixed fluoride is 1:1.1, and the mass ratio of chloroethylene carbonate to solvent is 1:0.9; open the steam valve and stirring switch of the enamel reaction kettle, and the speed is 500r / min , raise the temperature of the material in the kettle to 78°C for 3.5 hours, the reaction will stop when the content of chloroethylene carbonate is ≤2%, and the temperature ...

Embodiment 3

[0025] (1) Replace the enamel reaction kettle with nitrogen, and detect that the oxygen content is ≤50ppm and the moisture content is less than 10ppm, then add anhydrous high-purity mixed fluoride into the reaction kettle through the hand hole, and the mixed fluoride is diisopropyl tin fluoride and fluorine Potassium chloride is uniformly mixed by mass at 27:1; and chloroethylene carbonate and solvent are injected into the enamel reaction kettle through a metering pump, and the solvent is a mixture of methyl tert-butyl ether and acetonitrile at a mass ratio of 7:15 Solvent; the molar ratio of chloroethylene carbonate to mixed fluoride is 1:1.1, and the mass ratio of chloroethylene carbonate to solvent is 1:1.2; open the steam valve and stirring switch of the enamel reaction kettle, and the speed is 500r / min , after heating the material in the kettle to 83°C for 3 hours, the reaction stops when the content of chloroethylene carbonate is ≤2%, and the temperature is lowered to 40°...

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PUM

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Abstract

A synthesis method for fluoro-ethylene carbonate. The invention belongs to the technical field of battery stabilizers. The synthesis method includes the steps of: 1) under protection of inert gas, adding chloro-ethylene carbonate, a tetraalkyl halogenated amine catalyst, a solvent and a fluoride mixture into a reaction kettle with stirring and mixing, and controlling the temperature to be 60-100 DEG C to perform a halogen exchange reaction for 3-6 h to produce a crude product containing fluoro-ethylene carbonate, wherein molar ratio of the chloro-ethylene carbonate to the fluoride mixture is 1:1.0-1.1, and the mass ratio of the chloro-ethylene carbonate to the solvent is 1:0.9-1.2; and 2) purifying the crude product containing fluoro-ethylene carbonate to produce the fluoro-ethylene carbonate. The method is characterized by one-time addition of the fluorinating agent, mild reaction, high yield, convenient separation and simple operations.

Description

technical field [0001] A method for synthesizing fluoroethylene carbonate belongs to the technical field of battery stabilizers. Background technique [0002] At present, lithium batteries are widely used in mobile phones, tablet computers, electric vehicles and other neighborhoods. With the country's advocacy of green energy and people's increasing concern for the environment, the lithium battery industry will usher in rapid development. However, the safety and life of lithium batteries have always been a technical difficulty in the industry. After research, it is found that the proper use of electrolyte additives can effectively improve the safety of batteries, increase the number of charge and discharge times, and prolong battery life. Among them, fluoroethylene carbonate is an important battery stabilizer. [0003] Existing fluoroethylene carbonate preparation methods mainly include: electrochemical fluorination, displacement fluorination, addition fluorination, etc. A...

Claims

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Application Information

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IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 牛会柱
Owner 山东永浩新材料科技有限公司
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