Preparation process of fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of preparation technology of fluoroethylene carbonate, can solve problems such as difficult refining and removal, increased equipment investment, troublesome production control, etc., and achieves reduction of by-product generation, Reduction of reaction time and improvement of efficiency

Pending Publication Date: 2022-06-14
内蒙古源宏精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are coking and decomposition phenomena in fluoroethylene carbonate in the rectification process, and vinylene carbonate (VC) that is difficult to separate is generated, which is not easy to be refined and removed, and rectification is carried out under relatively high temperature conditions, and the material deteriorates more, resulting in a higher yield. Low; at the same time, rectification needs to use high vacuum unit and rectification tower, which greatly increases equipment investment and high cost
However, the use of organic solvents for recrystallization not only introduces additional solvents, but also requires re-removal of solvents, making production control more troublesome
In addition, it is also reported that higher purity (98%) chloroethylene carbonate can be directly used to improve the purity of fluoroethylene carbonate crude product, but on the one hand, high-purity chloroethylene carbonate also needs to be obtained by rectification , the market price is relatively expensive; on the other hand, even the crude product of fluoroethylene carbonate prepared from high-purity chloroethylene carbonate as a raw material also requires rectification and recrystallization to obtain electronic grade products

Method used

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  • Preparation process of fluoroethylene carbonate
  • Preparation process of fluoroethylene carbonate
  • Preparation process of fluoroethylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] S1: Pretreatment: Distillation pretreatment of 80% grade of chlorinated vinyl carbonate (81.2%) of commercially available raw materials, after removing low boiling, collect fractions at 200-300Pa and temperature 80-90 °C, and the purity of chlorinated vinyl carbonate reaches 94.7%;

[0044] S2: Fluoridation: 500g of diethyl carbonate, 170g of potassium fluoride, 0.6g of hexamethyl fluoride into the reactor, dehydrated at atmospheric pressure at 120-130 °C to ≤ 0.1% of the distilled water, cooled to 70-80 °C to start adding 300g of chlorinated vinyl carbonate (according to the purity of chlorinated vinyl carbonate, the same below), about 2 hours of dropwise addition, insulation reaction for 3 hours, filtration, dissolution to obtain fluorovinyl carbonate; from Figure 1 The results of the reaction solution analysis can be seen that the purity of fluorovinyl carbonate is 93.6% (6.3min), the content of chlorinated vinyl carbonate is < 0.5% (9.5min), and the basic unparalleled f...

Embodiment 2

[0050] S1: pretreatment: 80% of the raw material grade of chlorovinyl carbonate (same as Example 1) distillation pretreatment, after removing low boiling, collect 200-300Pa, temperature 80-90 °C distillate, chlorovinyl carbonate purity of 94.6%;

[0051] S2: Fluorination: 500g diethyl carbonate, 170g potassium fluoride, 0.75g hexamethyl fluoride into the reactor, dehydrated at atmospheric pressure at 120-130 °C to ≤ 0.1% of the distilled water, cooled to 70-80 °C to start the titration treatment of 300g of chlorovinyl carbonate, about 2 hours of drop-added end, insulation reaction for 3 hours, filtration, dissolution to obtain a purity of 94.4% of fluorinated carbonate, chlorinated vinyl carbonate content of <0.5%;

[0052] S3: Refining:

[0053] S3-1 put the concentrate into the treatment kettle, cool down to -10 °C at a speed of 5 °C / hour, stop cooling, open the bottom valve of the kettle, flow out of the non-condensate, the kettle gradually heats up to 15 °C, about 2 hours la...

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Abstract

The invention provides a preparation process of fluoroethylene carbonate. The purity of the fluoroethylene carbonate crude product is practically improved by adopting various effective means in the fluorination process of the chloroethylene carbonate, and various process parameters are strictly controlled in the refining process, so that the chloroethylene carbonate with the purity of 99.95% or above can be obtained. According to the preparation process disclosed by the invention, under the condition of not using rectification, particularly not rectifying the fluoroethylene carbonate, the utilization of the cheap low-purity chloroethylene carbonate is realized, the equipment investment is reduced, another feasible route is provided for the synthesis of the fluoroethylene carbonate, and the economic value is very high.

Description

Technical field [0001] The present invention relates to the field of fluorovinyl carbonate synthesis technology, specifically to a fluorovinyl carbonate preparation process. Background [0002] Fluoroethylene carbonate (FEC) is an important fine chemical material, mainly used as a film-forming additive and explosion-proof solvent for lithium battery electrolytes. The addition of fluorovinyl carbonate to the electrolyte can form a solid electrolyte interface (SEI membrane) with excellent performance on the electrode. The compact structure of the membrane can reduce the impedance of the battery and effectively inhibit the decomposition of part of the electrolyte, thereby improving the specific capacity of the battery and improving the safety and life of the battery. In addition, fluoroethylene carbonate can also be used as an intermediate in medicine and pesticides. [0003] In the past, the industrial production of fluorovinyl carbonate was mostly direct fluorinated substitution. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 王兵波张森王伟张晓弟宋立雪
Owner 内蒙古源宏精细化工有限公司
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