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Method for preparing fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate is applied in the field of preparation of fluoroethylene carbonate, and can solve the problems of side reaction tar and fluoroethylene carbonate being difficult to meet the requirements for use, low yield and the like

Inactive Publication Date: 2011-05-18
ZHEJIANG HUAJING FLUORINE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] But above-mentioned reaction has obvious side reaction and tar generation, and this also is the reason that most patents describe low yield
In addition, excessive post-reaction treatment steps are easy to introduce moisture, making it difficult for the moisture content of the obtained product fluoroethylene carbonate to meet the usage requirement of less than 20ppm
[0010] In summary, this area lacks a preparation method that suppresses side reactions and tar generation, increases yield, and reduces product moisture

Method used

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  • Method for preparing fluoroethylene carbonate
  • Method for preparing fluoroethylene carbonate

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preparation example Construction

[0042] Preparation method of fluoroethylene carbonate

[0043] The invention provides a kind of preparation method of fluoroethylene carbonate, the method comprises the following steps,

[0044] A mixture of fluorinated reagents and solvents is provided, and the solvent for the reaction is a high-boiling organic solvent with bp>200°C; raw materials for chloroethylene carbonate are provided;

[0045] The mixture is warmed up, and the chloroethylene carbonate is added dropwise to the mixture when the mixture is warmed up to the required temperature;

[0046] The reaction system is distilled under reduced pressure at the same time as or after the dropwise addition to obtain crude fluoroethylene carbonate.

[0047] The method described is as follows:

[0048]

[0049] The "MF" stands for a fluorinating agent; the "solvent" stands for a solvent.

[0050] In a preferred example, the method includes the following steps:

[0051] Add fluorinated reagent and solvent into reactio...

Embodiment 1

[0085] Preparation of Fluoroethylene Carbonate

[0086] Put 4.8 moles of KF and 800 g of tetraethylene glycol dimethyl ether in a 2L reaction flask, heat to an internal temperature of 80-100°C, and dehydrate under reduced pressure until the water content of the solution is less than 50 ppm. Start to add 4.0 moles of chloroethylene carbonate dropwise, and the dropwise addition is completed in about 6 hours. The dropwise addition is carried out with vacuum distillation at the same time, and a total of 600 g of the solution is distilled out, and the reaction conversion rate is 97%. This solution was subjected to rectification under reduced pressure to obtain 381.6 g of fluoroethylene carbonate with a GC content of 99.95%, a yield of 90%, a water content of 8 ppm, and a total chlorine content of 12 ppm.

[0087] MP: 19-20°C.

Embodiment 2

[0089] Preparation of Fluoroethylene Carbonate

[0090] Put 4.8 moles of KF and 800 g of tetraethylene glycol dimethyl ether in a 2L reaction flask, heat to an internal temperature of 80-100°C, and dehydrate under reduced pressure until the water content of the solution is less than 50 ppm. Start to add 4.0 moles of chloroethylene carbonate dropwise, and the dropwise addition is completed in about 6 hours. After the dropwise addition, the stirring reaction is continued for 4 hours, and the reaction conversion rate is 85%. This solution was subjected to rectification under reduced pressure to obtain 326.5 g of fluoroethylene carbonate with a GC content of 99.90%, a yield of 77%, a water content of 12 ppm, and a total chlorine content of 15 ppm.

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Abstract

The invention discloses a method for preparing fluoroethylene carbonate, which comprises the following steps: providing a mixture of a fluorating agent and a solvent; providing a chloroethylene carbonate raw material; heating the mixture, and dripping the chloroethylene carbonate into the mixture under a constant pressure when the mixture is heated to a required temperature; and performing distillation under reduced pressure on a reaction system during dripping or after dripping to obtain a coarse fluoroethylene carbonate product. When the preparation method of the invention is used, high-purity and low-moisture content product can be obtained in a shorter period.

Description

technical field [0001] The invention relates to a preparation method of fluoroethylene carbonate. Background technique [0002] Since Sony's lithium-ion battery was launched in 1991, lithium-ion batteries have developed rapidly and have been widely used in mobile phones, notebook computers, digital products, electric bicycles and other fields; with the restrictions on traditional non-renewable resources and energy saving and emission reduction The development of new energy vehicles has risen to the height of strategic status in various countries, among which power batteries are the core of the recent development of new energy vehicles. Compared with lead-acid batteries, nickel-cadmium batteries, and nickel-metal hydride secondary batteries, lithium batteries have the advantages of high energy density, low self-discharge rate, and long cycle life. These advantages of lithium batteries will make them a new energy vehicle battery in the near future. main direction. [0003] F...

Claims

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Application Information

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IPC IPC(8): C07D317/42
Inventor 蔡国荣刘俊俞佳麟
Owner ZHEJIANG HUAJING FLUORINE CHEM TECH
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