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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0020] Example 1

[0021] (1) Replace the enamel reactor with nitrogen, and detect that the oxygen content is ≤50ppm, and the moisture <10ppm, then add anhydrous high-purity mixed fluoride to the reaction kettle through the hand hole, the mixed fluoride is a mixture of tripropyltin fluoride and potassium fluoride in a mass ratio of 25:1 uniformly mixed; the chlorine is discharged through a metering pump The ethylene carbonate and the solvent are injected into the enamel reactor. The solvent is a mixed solvent of methyl tert-butyl ether and acetonitrile at a mass ratio of 3:17; the molar ratio of the added chloroethylene carbonate to the mixed fluoride is 1: 1.05, the mass ratio of chloroethylene carbonate to solvent is 1:1.1; turn on the steam valve and stirring switch of the enamel reactor at a speed of 500r / min, and heat the contents of the kettle to 81℃ for 3 hours. The reaction stops when the content is less than or equal to 2%, and the temperature is lowered to 40°C; (2) The...

Example Embodiment

[0022] Example 2

[0023] (1) Replace the enamel reactor with nitrogen, and detect that the oxygen content is ≤50ppm, and the moisture <10ppm, then add the anhydrous high-purity mixed fluoride into the reactor through the hand hole, the mixed fluoride is the mixture of tripropyltin fluoride and potassium fluoride in a mass ratio of 23:1; The chloroethylene carbonate and the solvent are poured into the enamel reactor. The solvent is a mixed solvent of methyl tert-butyl ether and acetonitrile in a mass ratio of 2:19; the molar ratio of the added chloroethylene carbonate to the mixed fluoride is 1 :1.1, the mass ratio of chloroethylene carbonate to solvent is 1:0.9; turn on the steam valve and stirring switch of the enamel reactor at a speed of 500r / min, and heat up the contents of the kettle to 78°C for 3.5 hours. The reaction stops when the lipid content is less than or equal to 2%, and the temperature is lowered to 40°C; (2) The materials obtained from the reaction are pumped int...

Example Embodiment

[0024] Example 3

[0025] (1) Replace the enamel reactor with nitrogen, and detect that the oxygen content is ≤50ppm, and the moisture <10ppm, then add the anhydrous high-purity mixed fluoride to the reaction kettle through the hand hole, the mixed fluoride is a mixture of diisopropyltin fluoride and potassium fluoride according to the mass 27:1 uniformly mixed; and the metering pump The chloroethylene carbonate and the solvent are poured into the enamel reactor. The solvent is a mixed solvent of methyl tert-butyl ether and acetonitrile in a mass ratio of 7:15; the molar ratio of the added chloroethylene carbonate to the mixed fluoride is 1 :1.1, the mass ratio of chloroethylene carbonate to solvent is 1:1.2; turn on the steam valve and stirring switch of the enamel reactor at a speed of 500r / min, and heat the contents of the kettle to 83℃ for 3 hours. The reaction stops when the lipid content is less than or equal to 2%, and the temperature is lowered to 40°C; (2) The materials ...

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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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