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Method for preparing fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, applied in the field of preparation of fluoroethylene carbonate, can solve problems such as poor selectivity, low conversion rate, difficult control, etc., achieve mild reaction conditions, improve reaction Yield, effect of reducing reaction time

Inactive Publication Date: 2016-04-13
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) Carry out halogen exchange reaction with the fluorine in hydrogen fluoride as nucleophile: the crude product of this method gains produces a large amount of fluorine-containing waste water after washing, and the processing difficulty of fluorine-containing waste water is bigger, and the selectivity of this method is relatively low. Poor, high cost, difficult to control;
[0007] (3) Electrolytic fluorination with fluorine in hydrogen fluoride as a nucleophile: the selectivity of this reaction is poor, the reaction is difficult to control, and this method is still being explored;
[0008] (4) Halogen exchange reaction using fluorine in the fluorinating agent as a nucleophile: the reaction process of this method is relatively easy to control, relatively high in safety, and widely used, but the reaction time is long and the conversion rate is not too high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 120 g of sulfolane and 10 g of ethylene glycol dimethyl ether into a 1 L three-neck round bottom flask, then add 61 g of chloroethylene carbonate, and start stirring. After the temperature of the solvent system was raised to 79° C., 1 g of polyethylene glycol with a degree of polymerization of 400 was added to the mixture as a phase transfer catalyst, and the mixture was fully stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 125°C, and add 15g, 10g and 10g of fluorinating agent respectively when reaching this temperature, 1 hour and 2 hours later, then maintain this temperature and continue the reaction for 8 hours to obtain fluorinated ethylene carbonate mixture of esters. The yield of fluoroethylene carbonate was 85.5%.

[0023] The mixture containing fluoroethylene carbonate was recrystallized twice, and then vacuum distillation was carried out under the vacuum condition of about -1.3kPa, and the fraction at 90-110°C was col...

Embodiment 2

[0025] Add 60 g of sulfolane and 70 g of diethylene glycol dimethyl ether into a 1 L three-neck round bottom flask, then add 61 g of chloroethylene carbonate, and start stirring. After the temperature of the solvent system was raised to 76° C., 2 g of polyethylene glycol with a degree of polymerization of 1000 was added to the mixture as a phase transfer catalyst, and the mixture was thoroughly stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 132°C, and add 20g, 12g and 10g of fluorinating agent respectively when reaching this temperature, 1 hour and 2 hours later, then maintain this temperature and continue the reaction for 7 hours to obtain fluorinated ethylene carbonate mixture of esters. The yield of fluoroethylene carbonate was 88.7%.

[0026] The mixture containing fluoroethylene carbonate was recrystallized twice, and then vacuum distillation was carried out under the vacuum condition of about -1.3kPa, and the fraction at 90-110°C ...

Embodiment 3

[0028] Add 178g of triethylene glycol dimethyl ether into a 1L three-neck round bottom flask, then add 61g of chloroethylene carbonate, and start stirring. After raising the temperature of the solvent system to 72° C., 3 g of polyethylene glycol with a degree of polymerization of 800 was added to the mixture as a phase transfer catalyst, and the mixture was thoroughly stirred for 10 minutes. Then gradually raise the temperature of the reaction system to 140° C., and add 15 g, 15 g, and 10 g of fluorinating agent when reaching this temperature, 1 hour, and 2 hours later, and then maintain this temperature to continue the reaction for 6 hours to obtain fluorinated ethylene carbonate. mixture of esters. The yield of fluoroethylene carbonate was 88.5%.

[0029] The mixture containing fluoroethylene carbonate was recrystallized twice, and then subjected to vacuum distillation under a vacuum condition of about -1.3kPa to collect fractions at 90-110°C to obtain pure fluoroethylene c...

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Abstract

The invention provides a method for preparing fluoroethylene carbonate. According to the method, chloroethylene carbonate and a fluorinating agent serve as raw materials, polyethylene glycol serves as a phase transfer agent, a nonprotic organic solvent serves as a reaction medium solvent, reaction parameters are adjusted, the reaction yield is improved, the reaction time is reduced, the reaction conditions are mild, the requirements on a generating device are low, and the environmental pressure is small.

Description

technical field [0001] The present invention relates to a kind of preparation method of carbonate, especially a kind of preparation method of fluoroethylene carbonate. Background technique [0002] Fluoroethylene carbonate (FEC) is a colorless transparent liquid at room temperature and is a special kind of ethylene carbonate. Fluoroethylene carbonate is a very important fine chemical material with good development prospects. Fluoroethylene carbonate can be used as a medicine and pesticide intermediate, and because the molecular structure contains a 1,3-dioxane-2-one structure, it can be used for the synthesis of furan and oxazolone medicines and pesticides. [0003] Fluoroethylene carbonate can also be used as an excellent film-forming additive and anti-riot solvent for lithium-ion battery electrolytes. After adding fluoroethylene carbonate to the electrolyte of lithium-ion batteries, a solid electrolyte interface (Solid electrolyte interphase, SEI) film with better perfor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/38
CPCC07D317/38
Inventor 王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD