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Method for treating fluoroethylene carbonate solid residues

A technology of fluoroethylene carbonate and a treatment method, which is applied in the field of solid slag treatment in the production process of fluoroethylene carbonate, can solve problems such as environmental protection problems that are difficult to solve, and reduce the yield of crude fluoroethylene carbonate and solvent recovery efficiency. , to achieve the effect of reducing environmental risks

Pending Publication Date: 2021-02-02
HUBEI HONGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the entrainment of mother liquor reduces the yield of crude fluoroethylene carbonate and the recovery efficiency of the solvent in the synthesis process; on the other hand, in the presence of a large amount of organic matter, it is difficult to solve the environmental protection problem when the by-product potassium chloride is present.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In embodiment 1 and embodiment 2, solid residue is that chloroethylene carbonate and potassium fluoride are reacted in acetonitrile solvent and obtained by filtration and separation. In embodiment 3, solid residue is chloroethylene carbonate and potassium fluoride in diethyl carbonate. After reacting in an ester solvent, it is obtained by filtration and separation. The mass ratios of chloroethylene carbonate, potassium fluoride, and solvent in Examples 1, 2, and 3 are consistent.

[0033] Example 1:

[0034] The solid residue is obtained by reacting chloroethylene carbonate and potassium fluoride in acetonitrile solvent and then separating by filtration.

[0035] Weigh 625 g of fluoroethylene carbonate solid residue and dry it under vacuum at -80kPa and 90°C for 3 hours to recover 133 g of organic solvent acetonitrile. When the pressure dropped to -95kPa and the temperature was 120°C, the drying was continued for 2 hours, and 108g of crude fluoroethylene carbonate was ...

Embodiment 2

[0037] The solid residue is obtained by reacting chloroethylene carbonate and potassium fluoride in acetonitrile solvent and then separating by filtration.

[0038] Weigh 847g of fluoroethylene carbonate solid residue and dry it under vacuum at -75kPa and 90°C for 2 hours to recover 170g of organic solvent acetonitrile. When the pressure dropped to -95kPa and the temperature was 118°C, the drying was continued for 2 hours, and 144g of crude fluoroethylene carbonate was recovered. Add 2500 g of water to the above waste residue, stir and dissolve at a stirring speed of 200 rpm for 1 h, and add 25% potassium hydroxide solution while stirring to adjust the pH value to 9. After stirring and dissolving, filter and dry the filter residue at 105°C for 2 hours, and then detect its components as potassium fluorosilicate, sodium fluoride and a small amount of potassium chloride. 60 g of activated carbon was added to the above-mentioned filtrate, and the stirring speed was 200 rpm for st...

Embodiment 3

[0040] The solid residue is obtained by reacting chloroethylene carbonate and potassium fluoride in diethyl carbonate solvent and then separating by filtration.

[0041] Weigh 542g of fluoroethylene carbonate solid residue and vacuum-dry for 5 hours under the pressure of -80kPa and 100°C to recover 120g of organic solvent diethyl carbonate. When the pressure dropped to -98kPa and the temperature was 120°C, the drying was continued for 1 hour, and 99g of crude fluoroethylene carbonate was recovered. Add 1100 g of water to the above waste residue, stir and dissolve at a stirring speed of 200 rpm for 1 h, and add 30% potassium hydroxide solution while stirring to adjust the pH value to 8. After stirring and dissolving, filter and dry the filter residue at 105°C for 2 hours, and then detect its components as potassium fluorosilicate, sodium fluoride and a small amount of potassium chloride. 33g of activated carbon was added to the above filtrate, and the stirring speed was 100rpm...

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PUM

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Abstract

The invention discloses a method for treating fluoroethylene carbonate solid residues. The method comprises the following steps: (1) drying fluoroethylene carbonate reaction solid residues under primary vacuum, and recovering a solvent; (2) heating the solid residues after the solvent is recovered in the step (1) under secondary vacuum, continuing drying, and recovering a fluoroethylene carbonatecrude product; (3) adding water into the solid residues after the fluoroethylene carbonate crude product is recovered in the step (2), performing stirring for dissolving, adding a potassium hydroxidesolution in the dissolving process to adjust the pH value until the solution is completely dissolved, and performing filtering; (4) drying the filter residues obtained in the step (3); (5) adding activated carbon into filtrate obtained in the step (3) for stirring adsorption treatment, and performing filtering after the treatment is finished; and (6) taking the filtrate obtained in the step (5), determining fluorine ion concentration, adding calcium chloride into the filtrate in proportion, performing stirring for a period of time, performing filtering, separating, washing and drying filter residues to obtain calcium fluoride, and evaporating and crystallizing the filtrate to obtain byproduct potassium chloride. The recovery efficiency of the product and the solvent is improved, the process is simple, and the treatment cost is low.

Description

technical field [0001] The invention relates to the technical field of electrolyte additives for lithium batteries, in particular to a method for treating solid residue in the production process of fluoroethylene carbonate. Background technique [0002] Fluoroethylene carbonate can not only be used as an additive of lithium-ion battery electrolyte, but also as an intermediate of medicine and pesticide, so it has a broad market prospect. The current production method of fluoroethylene carbonate is mainly prepared by chloroethylene substitution reaction with metal fluorides, followed by purification. When this method produces fluoroethylene carbonate, a large amount of potassium chloride will be produced as a by-product. Potassium chloride can be used in inorganic industry, but also as agricultural and medical raw materials. [0003] However, during the synthesis reaction of fluoroethylene carbonate, a large amount of synthetic mother liquor will be entrained by chlorides in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42C01D3/04C07C68/08C07C69/96C07C255/03C07C253/34
CPCC07D317/42C01D3/04C07C68/08C07C253/34C07C69/96C07C255/03
Inventor 金桥张响飞邱敏芳贾雪枫舒伟锋李福
Owner HUBEI HONGYUAN PHARMA