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Process for the continuous preparation of 4-trifluoromethylethylene carbonate

A technology of trifluoromethylethylene carbonate and trifluoropropylene oxide, which is applied in the field of preparation of five-membered cyclic carbonates, can solve the problem of inconsistent high-quality requirements for battery-grade reagents, metal catalysis, high price, and residual metal tungsten in the product and other problems, to achieve the effect of high product quality, low preparation efficiency, and high space-time yield

Active Publication Date: 2021-02-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reaction yield is high, it is carried out intermittently in a high-pressure reactor, the preparation efficiency is low, and it involves metal catalysis, the price is expensive, and the product has metal tungsten residues, which does not meet the high-quality requirements of battery-grade reagents.

Method used

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  • Process for the continuous preparation of 4-trifluoromethylethylene carbonate
  • Process for the continuous preparation of 4-trifluoromethylethylene carbonate
  • Process for the continuous preparation of 4-trifluoromethylethylene carbonate

Examples

Experimental program
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Effect test

example 3

[0035] After a certain proportion of 3,3,3 trifluoropropylene oxide is mixed with bromine-containing fluoroalkanes and organic bases, it is dehydrated by molecular sieve drying treatment device D1, and then enters preheater E 1 , and the carbon dioxide that has passed through the dryer D2 is fully mixed in the mixer M, and then enters the tubular reactor R for reaction; the reaction product flow enters the gas-liquid separation tank S, and the top component of the separation tank is carbon dioxide, which enters the carbon dioxide recovery system C, recycling; the bottom material is TFPC, TFPO, bromine-containing fluoroalkanes, organic bases, carbon dioxide, etc., and enter the first rectification tower for the separation of 3,3,3-trifluoropropylene oxide; the first rectification tower The top component is the material containing 3,3,3-trifluoropropylene oxide, which is returned to the organic material recovery unit or preheater for recycling; the bottom component enters the sec...

Embodiment 1

[0037] Transport 3,3,3-trifluoropropylene oxide to the material mixing unit V1, and then add 2,3-dibromo-1,1,1, 2,3,3-Hexafluoropropene and triethylamine are transported to V1, and after starting to stir and mix evenly, they are transported to the molecular sieve drying device D1 by the pump for dehydration. After the water content of TFPO is detected to be less than 10ppm, the 3,3,3 - The trifluoropropylene oxide material is transported to the preheater E1 for preheating, the preheating temperature is 70°C, and then mixed with the CO passing through the dryer D2 2 Mix in the mixer M, the temperature of the mixer is 120°C, after mixing, it enters the tubular reactor R for reaction (specification), the reaction temperature is 120°C, the reaction pressure is 0.5MPa, the reaction residence time is 40min, and the reaction product flow enters the gas-liquid separation tank, the top component is carbon dioxide, which enters the carbon dioxide recovery system C for recycling; the bot...

Embodiment 2～6

[0044] Embodiment 2~6 prepares 4-trifluoromethylethylene carbonate according to the same method in embodiment 1, difference is that the reaction temperature in embodiment 1 is 120 ℃, and in embodiment 2~6, reaction temperature is followed by 70°C, 90°C, 100°C, 150°C, 180°C, and the temperature of the preheater was adjusted accordingly. The reaction results are shown in Table 1.

[0045] Table 1

[0046]

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Abstract

The invention discloses a method for continuously preparing 4-trifluoromethylethylene carbonate, which comprises the following steps: a. mixing a certain proportion of 3,3,3-trifluoropropylene oxide, bromine-containing fluoroalkane, and organic base After mixing evenly, it is transported to the drying device for dehydration; b. After the dried 3,3,3-trifluoropropylene oxide material is preheated by the preheater, it is efficiently mixed with the dried carbon dioxide in the mixer, and then The reaction is carried out by a tubular reactor to obtain a product stream containing 4-trifluoromethylethylene carbonate, 3,3,3-trifluoropropylene oxide and carbon dioxide; c, the product of step b flows through a gas-liquid separation tank , the first rectification tower, and the second rectification tower carry out the separation and recovery of materials, and the target product is obtained at the top of the second rectification tower. The invention has the characteristics of continuous and stable process, high space-time yield, environmental friendliness, and no metal residue in the product, and is mainly used for the continuous preparation of electrolyte solution 4-trifluoromethylethylene carbonate for lithium ion batteries.

Description

technical field [0001] The invention relates to a method for preparing five-membered cyclic carbonate, in particular to a method for continuously preparing 4-trifluoromethylethylene carbonate (TFPC). Background technique [0002] Due to the advantages of high energy density, high output voltage, long cycle life, no memory effect, and environmental friendliness, lithium-ion batteries have been widely used in various electronic products, equipment and new weapons and equipment. In recent years, lithium-ion batteries have become the The application of power energy in the automotive and aerospace fields has also attracted much attention. Electrolyte is an indispensable part of lithium-ion batteries, which directly affects the discharge and charge capacity, cycle performance and safety performance of the battery. The currently used lithium-ion battery electrolyte is the third-generation electrolyte, which is mainly composed of ethylene carbonate (EC), dimethyl carbonate (DMC), a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36C07D301/32C07D303/08
CPCC07D301/32C07D303/08C07D317/36
Inventor 马辉吕剑谷玉杰涂东怀毛伟赵波王博韩升白彦波杨志强
Owner XIAN MODERN CHEM RES INST