Supercharge Your Innovation With Domain-Expert AI Agents!

Preparation method for difluoroethylene carbonate

A technology of bisfluoroethylene carbonate and vinylene carbonate, which is applied in the field of preparation of bisfluoroethylene carbonate, can solve the problems of high processing cost, cumbersome processing, and low yield, achieve high purity and create economic benefits , the effect of high yield

Inactive Publication Date: 2018-04-13
ZHANGJIAGANG HICOMER CHEM CO LTD
View PDF6 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that there are many side reactions, the yield is too low, it is not easy to purify, and the rectification process is difficult
The disadvantages of this method are: high cost of raw materials, easy corrosion of equipment, high equipment requirements, not suitable for industrial production
[0004] At present, there is still a problem in the production: the crude product of vinylene carbonate forward distillation (the content of vinylene carbonate is 30% ~ 60%) is relatively cumbersome to deal with, and the treatment cost is high, and it is usually treated as waste liquid

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0017] The preparation method of bisfluoroethylene carbonate is described in detail below.

[0018] The preparation method of bisfluoroethylene carbonate comprises the following steps.

[0019] 1. Addition reaction: add the forward distillation of vinylene carbonate and organic solvent in the first reaction kettle, stir so that the forward distillation of vinylene carbonate and the organic solvent are completely miscible, and the vinylene carbonate in the forward distillation of vinylene carbonate The mass fraction of vinyl ester is 30% to 60%. Nitrogen is passed through. The function of nitrogen is to isolate the reactants from air and water, heat to 20-50°C, and add liquid bromine or chlorine gas to carry out the addition reaction. The dropping rate of liquid bromine is 12 drops / minute, and the flow rate of chlorine gas is 0.1 to 0.5 liters / minute when chlorine gas is introduced. After the reaction is completed, solvent removal (recover the solvent for future use), refining...

Embodiment 1

[0025] One, addition reaction: in the first reaction kettle, add the forward distillation of vinylene carbonate and organic solvent, wherein the quality of the forward distillation of vinylene carbonate is 143.42g, the massfraction of vinylene carbonate is 60%, carbonic acid Vinylene is 1 mol; the organic solvent is dimethyl carbonate, the mass is 1000 g, and the water content is 8.2 ppm. Stir to make the forward distillate of vinylene carbonate miscible with the organic solvent completely, pass nitrogen gas, heat to 25°C, add liquid bromine (1.1mol, 175.791g) dropwise, the dropping rate of liquid bromine is 12 drops / min, carry out Addition reaction. After the reaction, precipitation and refining were carried out, and the whole process of refining was under nitrogen protection to obtain pure bisbromoethylene carbonate (239.56 g, yield 97.45%, purity 99.01%). Put the pure product of bisbromoethylene carbonate into the second reaction kettle for subsequent use.

[0026] 2. Sub...

Embodiment 2

[0029] One, addition reaction: in the first reaction kettle, add the forward distillation of vinylene carbonate and organic solvent, wherein the quality of the forward distillation of vinylene carbonate is 172.10g, the massfraction of vinylene carbonate is 50%, carbonic acid Vinylene is 1 mol; the organic solvent is diethyl carbonate, the mass is 500 g, and the water content is 5.3 ppm. Stir to make the front distillation of vinylene carbonate and diethyl carbonate miscible completely, pass nitrogen gas, heat to 30°C, pass chlorine gas (1.3mol, 92.3g), and the flow rate of chlorine gas is 0.3 liters / minute to carry out addition reaction . After the reaction, precipitation and refining were carried out, and nitrogen protection was used throughout the refining process to obtain pure dichloroethylene carbonate (153.50 g, yield 97.80%, purity 99.10%). Put the pure product of dichloroethylene carbonate into the second reaction kettle for standby.

[0030] 2. Substitution reaction...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method for difluoroethylene carbonate. The method comprises the following steps: step 1, adding front cut fraction of vinylene carbonate and an organic solvent into a first reaction kettle, performing mixing and dissolving completely, introducing a nitrogen gas, wherein the mass fraction of vinylene carbonate in the front cut fraction of the vinylene carbonateis 30%-60%, performing heating to the temperature of 20-50 DEG C, adding liquid bromine dropwise or introducing a chlorine gas, performing an addition reaction, after the reaction is completed, performing desolventizing, performing refining to obtain a pure product of dibromoethylene carbonate or a pure product of dichloroethylene carbonate, and putting the pure product into a second reaction kettle for standby application; step 2, adding an organic solvent into the second reaction kettle until mixing and dissolving are performed completely, then adding a fluorinating reagent, performing a reaction, adding triethylamine to make the reaction liquid system weakly acidic, heating the second reaction kettle until the temperature is 50-70 DEG C, and keeping the temperature until a reaction isfinished, so as to obtain a crude product; and step 3, performing vacuum rectification on the crude product to obtain the target product difluoroethylene carbonate. The method provided by the invention has the advantages that the target product has high purity and a high yield, can reach an electronic grade, and fully utilizes a waste liquid.

Description

technical field [0001] The invention relates to the technical field of additives for lithium battery electrolytes, in particular to a preparation method of bisfluoroethylene carbonate. Background technique [0002] Difluoroethylene carbonate is a kind of lithium battery electrolyte additive. The addition of bisfluoroethylene carbonate can improve the cycle performance and low-temperature performance of the electrolyte, and can also significantly increase the flash point of the electrolyte. [0003] At present, the preparation methods for preparing bisfluoroethylene carbonate mainly contain the following types. 1. Using dichloroethylene carbonate as a raw material, carry out a fluorination reaction with a fluorinating reagent to obtain bisfluoroethylene carbonate. The defect of this method is: many side reactions, the yield is too low, it is not easy to purify, and the rectification process is difficult. 2. Using vinylene carbonate as raw material and fluorine gas as fluor...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 许国荣赵建庞宝华孙西船姚双开许怡荪
Owner ZHANGJIAGANG HICOMER CHEM CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More