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Method for preparing fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, applied in the field of ethylene carbonate derivatives, can solve the problems of highly toxic fluorine gas, high reactivity, long reaction time, etc., and achieves lower production cost and environmental friendliness. Effect

Active Publication Date: 2008-07-02
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not use a phase transfer catalyst, resulting in a high temperature and a long reaction time for the reaction, and the conversion rate is also very low, which ultimately makes it difficult to obtain high-purity fluoroethylene carbonate products
[0005] Using the mixed gas of fluorine and nitrogen to react with ethylene carbonate is also a very important method for preparing fluoroethylene carbonate. The raw material used in this method is fluorine, and fluorine is not only highly toxic, but also highly reactive and very reactive. easily out of control
Due to the intense heat generated by the reaction, it is easy to cause the pressure in the reaction vessel to be too high, which is dangerous, and the fluorine gas is highly toxic and corrosive, so the requirements for the reaction equipment are very high.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0024] Add 44g sodium fluoride and stir in the three-neck round-bottomed flask equipped with dropping funnel, condenser, stirrer and thermometer, add 3.4g polyethylene glycol phase transfer catalyst (polymerization degree 800), then dropwise add 122.5g chlorine Substitute ethylene carbonate, and control the dropping temperature at 50-70°C. As the dropping goes on, the color of the mixture turns dark brown, and the temperature rises by itself. After the dropping is completed, the mixture is very viscous. After insulated at 100°C for 3 hours, cool the material to 30°C, and then use centrifugal suction to obtain a black filtrate, which contains 0.5% unreacted chloroethylene carbonate, 92% fluoroethylene carbonate and other raw materials with incoming impurities. The black filtrate was subjected to rectification under reduced pressure to finally obtain 59 g of a product with a purity of 99.9%.

[0025] Through the comparison of this example and Comparative Example 1, it can be fo...

Embodiment 3

[0027] In this embodiment, the order of addition of the materials in the second embodiment is reversed. That is: first add 2.8g of polyethylene glycol phase transfer catalyst (polymerization degree 800) and 122.5g of chloroethylene carbonate and mix, and then gradually add 42g of sodium fluoride powder into the above mixture through a funnel at 40°C , the addition speed should be slow, control the reaction temperature at 50-70°C, and finish adding in 2 hours. The other steps are the same as in Example 2. After 3 hours of heat preservation, the material becomes extremely viscous, cool the material to 30°C, and then use After centrifugal suction filtration, a black filtrate was obtained, which contained 4% unreacted chloroethylene carbonate, 89% fluoroethylene carbonate and impurities brought in by other raw materials. The black filtrate was subjected to rectification under reduced pressure to finally obtain 41 g of a product with a purity of 99.5%.

[0028] By comparing this e...

Embodiment 4

[0030] In this embodiment, add 42g sodium fluoride and 1.7g crown 18 ether when equipped with a dropping funnel, a three-necked round bottom flask with a condenser, agitator and thermometer, and then add 122.5g chloroethylene carbonate dropwise, The product has exothermic phenomenon, control the dropping temperature at 50-70°C, and then keep the reaction at 100°C for 3 hours. Suction filtration is carried out after the heat preservation is finished, and the filtrate is taken for chromatographic analysis. The content of chloroethylene carbonate is 1%, 91% of fluoroethylene carbonate, and the rest are unidentified impurities brought in the raw materials. Then the filtrate is decompressed and purified. Distillation finally obtained the finished product 57g with a purity of 99.8%.

[0031] Through this example, it can be found that the effect of using the polyethylene glycol phase transfer catalyst is the same as that of the crown ether transfer catalyst.

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Abstract

The invention discloses a method for preparing fluoroethylene carbonate with relatively short reaction time, relatively high yield and relatively low cost; the invention essentially comprise the following steps that: 1. fluoride and phase transfer catalyst are added into a reaction vessel; 2. chloroethylenes carbonate is added into the reaction vessel, all the reactants are subject to reaction in the reaction vessel, thus obtaining the mixture containing fluoroethylene carbonate; 3. the fluoroethylene carbonate in the mixture is solid-liquid separated and extracted by distillation, thus acquiring fluoroethylene carbonate with needed purity. By adopting the preparation method of the invention, the fluoroethylene carbonate with high yield can be obtained under a mild reaction condition and in relatively short reaction time. Additionally, the invention is more economical and more environment friendly and can use relatively cheap original materials, thus reducing production cost. The invention can be used for preparing fluoroethylene carbonate.

Description

technical field [0001] The invention relates to ethylene carbonate derivatives containing fluorine atoms, in particular to a preparation method of fluoroethylene carbonate. Background technique [0002] Fluoroethylene carbonate (F-EC), English name: Fluoroethylene carbonate, chemical name: 4-Fluoro-1, 3-dioxolan-2-one. It can be used as medicine, pesticide intermediate and lithium ion battery electrolyte additive. [0003] Introduced a kind of synthetic method of synthetic fluoroethylene carbonate in U.S. Patent Pat.No.6,010,806, the route that uses is that dimethyl carbonate and 3,3,3-trifluoro-1,2-propylene oxide are in Synthesized in the presence of sodium bicarbonate. The price of the 3,3,3-trifluoro-1,2-propene oxide used in the method is very high, and the reaction time is very long, requiring 8-40 hours, which seriously limits the industrialization of the method. [0004] International Patent Application Publication No. WO 98 / 15024 introduces a method for preparing...

Claims

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Application Information

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IPC IPC(8): C07D317/40
Inventor 陈剑戴晓兵
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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