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Preparation method of fluoroethylene sulfate

The technology of vinyl fluorosulfate and vinyl monofluorosulfate is applied in the preparation field of preparing vinyl fluorosulfate by an electrolytic fluorination method, and can solve the problems of complicated reaction and operation, high toxicity of fluorination reagents and resource utilization rate. It can achieve the effect of environmental friendliness, avoiding the production of intermediate products, and low cost

Active Publication Date: 2021-08-06
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +2
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned existing technologies all adopt the traditional chemical fluorination method, the reaction and operation are relatively complicated, and there are problems such as poor resource utilization, large equipment investment, high production cost, and serious environmental pollution, and the toxicity of the fluorinated reagent is high or extremely low. stable, expensive

Method used

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  • Preparation method of fluoroethylene sulfate
  • Preparation method of fluoroethylene sulfate
  • Preparation method of fluoroethylene sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Mix 0.8 mol of vinyl sulfate and 35 mol of anhydrous hydrogen fluoride (moisture content 20000ppm) to obtain anhydrous hydrogen fluoride solution of vinyl sulfate, put it into a 1L electrolytic cell, control the voltage to 5V and the current to 45A at room temperature, and perform electrolytic dehydration . After removing water for 8 hours, electrolytic fluorination was carried out under normal pressure. The reaction tank temperature was controlled at 0°C, the electrolysis voltage was 5.5V, the electrolysis current was 80A, and the reaction time was 10h. After the reaction is completed, the reaction solution is discharged from the bottom of the electrolytic cell, and an acid scavenging agent calcium oxide is added to obtain a crude product of vinyl fluorosulfate. After rectification, a vinyl fluorosulfate product with a purity higher than 99.5% is obtained. After calculation, the conversion rate of vinyl sulfate is 82.43%, and the selectivity of vinyl fluorosulfate is ...

Embodiment 2

[0031] Mix 0.6mol vinyl sulfate and 35mol anhydrous hydrogen fluoride (moisture content 35000ppm) to obtain anhydrous hydrogen fluoride solution of vinyl sulfate, put it into a 1L electrolytic cell, control the voltage to 7V and current to 50A at room temperature, and perform electrolytic dehydration . After removing water for 10 hours, electrolytic fluorination was carried out under normal pressure. The reaction tank temperature was controlled at 40°C, the electrolysis voltage was 7.5V, the electrolysis current was 75A, and the reaction time was 11h. After the reaction is completed, the reaction solution is discharged from the bottom of the electrolytic cell, and the acid scavenger aluminum oxide is added to obtain the crude product of vinyl fluorosulfate. After rectification, the product of vinyl fluorosulfate with a purity higher than 99.5% is obtained. After calculation, the conversion rate of vinyl sulfate is 81.99%, and the selectivity of vinyl fluorosulfate is 93.46%. ...

Embodiment 3

[0033] Mix 2 mol of vinyl sulfate and 25 mol of anhydrous hydrogen fluoride (moisture content 40000ppm) to obtain anhydrous hydrogen fluoride solution of vinyl sulfate, put it into a 1L electrolytic cell, control the voltage to 4.5V and the current to 35A at room temperature, and perform electrolytic dehydration . After removing water for 11 hours, electrolytic fluorination was carried out under normal pressure. The reaction tank temperature was controlled at 25°C, the electrolysis voltage was 5V, the electrolysis current was 120A, and the reaction time was 7h. After the reaction is completed, the reaction solution is discharged from the bottom of the electrolytic cell, and the acid scavenger aluminum oxide is added to obtain the crude product of vinyl fluorosulfate. After rectification, the product of vinyl fluorosulfate with a purity higher than 99.5% is obtained. According to calculation, the conversion rate of vinyl sulfate is 79.71%, and the selectivity of vinyl fluorosu...

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Abstract

The invention discloses a preparation method of fluoroethylene sulfate. The preparation method comprises the following steps: A1, adding anhydrous hydrogen fluoride and ethylene sulfate into an electrolytic bath, and mixing to obtain an anhydrous hydrogen fluoride solution of ethylene sulfate; A2, under normal pressure, a controlled voltage of 5-8 V and a current of 30-120 A, carrying out an electrolytic fluorination reaction at a reaction temperature of -5-50 DEG C for 5-25 h; and A3, removing hydrogen fluoride in a reaction liquid, and rectifying to obtain the fluoroethylene sulfate. The method has the advantages of simple process, low cost, high current efficiency, good reaction conversion rate and selectivity, stable product quality and the like.

Description

technical field [0001] The invention relates to an electrolyte additive for a lithium ion battery, in particular to a preparation method for preparing fluoroethylene sulfate by an electrolytic fluorination method. Background technique [0002] Vinyl sulfate is a new type of lithium battery electrolyte additive, which is used to inhibit the decrease of the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after high temperature storage, and improve the charge and discharge performance and cycle times of the battery. Its fluorinated product, fluoroethylene sulfate, can form a solid electrolyte interface (SEI film) with better performance on the electrode. The film has a tight structure, which can effectively reduce the impedance of the battery and inhibit the separation of part of the electrolyte, which is more obvious The specific capacity of the battery can be greatly improved, and the safety and service life of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/28C25B3/11C25B15/00C07D327/10
CPCC25B15/00C07D327/10Y02E60/10
Inventor 章祺倪航
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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