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Method for preparing high-purity chloroethylene carbonate through continuous two-stage liquid phase reaction

A technology of chloroethylene carbonate and dichloroethylene carbonate, applied in the field of continuous two-stage liquid phase reaction to prepare high-purity chloroethylene carbonate, can solve the problem of low production efficiency, no separation process, dichlorocarbonic acid Vinyl esters are not easy to separate and other problems, to achieve the effect of improving product quality, strong selectivity, and shortening reaction time

Inactive Publication Date: 2021-09-03
重庆微而易科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] 1. Reactors are basically used for the reaction of chlorine gas and ethylene carbonate, all of which are produced intermittently, and the production efficiency is low;
[0010] 2. Dichloroethylene carbonate, a by-product produced by the reaction of chlorine gas and ethylene carbonate, is not easy to separate, and most patents do not provide a separation process

Method used

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  • Method for preparing high-purity chloroethylene carbonate through continuous two-stage liquid phase reaction

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Experimental program
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Effect test

Embodiment 1

[0036]Step 1): 1000Kg of pre-melted ethylene carbonate (including ethylene carbonate reused in the workshop section) and catalyst azobisisobutyronitrile and liquid chlorine are added to the primary chlorination reaction tower T1, wherein ethylene carbonate: The mass ratio of azobisisobutyronitrile is 10:1, the molar ratio of ethylene carbonate: liquid chlorine is 2:1, the pressure of the primary chlorination reaction tower is controlled at 3.0MPa, and the temperature is 90°C. The gas phase of the light components at the top of the tower (hydrogen chloride and a small amount of entrained ethylene carbonate, etc.) is discharged from the top of the tower, condensed by the condenser E2, and then enters the reflux tank V1, and the non-condensable gas hydrogen chloride is discharged from the top of V1, and the condensate (containing ethylene carbonate) The residence time of ethylene carbonate, catalyzer, liquid chlorine etc. added in the primary chlorination reaction tower by reflux ...

Embodiment 2

[0040] The ethylene carbonate charging capacity of embodiment 2 is identical with embodiment 1, and difference is only, each parameter is different, and in embodiment 2, in step 1), ethylene carbonate: the mass ratio of azobisisobutyronitrile is 8 : 1, ethylene carbonate: the molar ratio of liquid chlorine is 3:1, the pressure of the primary chlorination reaction tower is 2.0MPa, and the temperature is 100°C. The residence time of each component in the primary chlorination reaction tower T1 is 2 hours;

[0041] The pressure of the secondary chlorination reaction tower in step 2) is 2.0 MPa, and the temperature is 110°C. The residence time of each component in the primary chlorination reaction tower T1 is 2 hours;

[0042] In step 3), the pressure of the rectifying tower is 300 Pa, and the temperature is 70°C. The qualified product chloroethylene carbonate was 1334.00Kg, the yield was 95.89%, and the purity was 99.91%.

Embodiment 3

[0044] Embodiment 3 is identical with the ethylene carbonate charging amount of embodiment 1, and difference only is that each parameter is different, and in embodiment 3, in step 1), ethylene carbonate: the mass ratio of azobisisobutyronitrile is 12 : 1, the molar ratio of ethylene carbonate: liquid chlorine is 3:1, the pressure of the primary chlorination reaction tower is 3.5MPa, and the temperature is 70°C. The residence time of each component in the primary chlorination reaction tower T1 is 2 hours;

[0045] The pressure of the secondary chlorination reaction tower in step 2) is 3.5MPa, and the temperature is 80°C. The residence time of each component in the primary chlorination reaction tower T1 is 2 hours;

[0046] In step 3), the pressure of the rectifying tower is 600 Pa, and the temperature is 100°C. The qualified product chloroethylene carbonate was 1343.61Kg, the yield was 96.65%, and the purity was 99.92%.

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Abstract

The invention discloses a method for preparing high-purity chloroethylene carbonate through a continuous two-stage liquid phase reaction, which comprises the following step: carrying out a two-stage liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst at high temperature and high pressure to produce chloroethylene carbonate, and carrying out high-vacuum rectification on the reaction product to separate the chloroethylene carbonate, the dichloroethylene carbonate and the unreacted ethylene carbonate, thereby obtaining the high-purity chloroethylene carbonate.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction. Background technique [0002] With the development of lithium-ion batteries, the amount of electrolyte additives fluoroethylene carbonate (FEC) and vinylene carbonate (VC) is increasing rapidly. FEC can improve the cycle life of the battery, increase the safety of the battery, and can improve the low-temperature life of the battery. Chloroethylene carbonate (CEC) is mainly used to prepare lithium battery electrolyte fluoroethylene carbonate and vinylene carbonate, react with potassium fluoride to produce fluoroethylene carbonate, and under the action of catalyst to produce vinylene carbonate . High-purity chloroethylene carbonate can also be directly used as a flame retardant additive for lithium battery electrolyte to improve the cycle perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 何睿鸣彭丽华张月娥
Owner 重庆微而易科技有限公司
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