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Preparation method of vinyl sulfate

A technology of vinyl sulfate and vinyl sulfite, which is applied in the field of preparation of vinyl sulfate, can solve the problems of high moisture content and acid value, low molar yield and purity, and difficult availability of raw materials, etc., and achieve low production cost , Improve the molar yield and purity, the effect of low moisture content

Active Publication Date: 2016-12-07
江苏瀚康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the disclosed preparation method of vinyl sulfate has the following disadvantages: one, the molar yield and purity of the product are not high, and the moisture content and acid value of the product are relatively high; two, the raw materials are difficult to obtain, and the preparation cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation method of vinyl sulfate, including substitution reaction and oxidation reaction, also includes refining process,

[0017] Specific steps are as follows :

[0018] (1) Substitution reaction: Thionyl chloride and ethylene glycol are used as the reaction raw materials for the substitution reaction. First, 130.0g (1mol) of ethylene glycol is added to the first reaction kettle, and then the Add 295 g (1.2 mol) of thionyl chloride dropwise for 1 hour. After the dropwise addition, keep warm at 40°C for 1 hour to obtain a reaction solution containing vinyl sulfite, and then use deionized water to dissolve the reaction solution Washing to neutrality, then the reaction solution was left to stand, layered and separated to separate vinyl sulfite 223.87g (purity is 98.72%), and then the isolated vinyl sulfite was added to the second reaction kettle for subsequent use;

[0019] (2) Oxidation reaction: first add 450 g of dichloromethane as a solvent and 8.97 g of ferr...

Embodiment 2

[0022] The preparation method of vinyl sulfate, including substitution reaction and oxidation reaction, also includes refining process,

[0023] Specific steps are as follows :

[0024] (1) Substitution reaction: Thionyl chloride and ethylene glycol are used as the reaction raw materials for the substitution reaction. First, 130.0g (1mol) of ethylene glycol is added to the first reaction kettle, and then the Add 495.6g (2mol) of thionyl chloride dropwise for 1.5h. After the dropwise addition, keep warm at 30°C for 2h to obtain a reaction solution containing vinyl sulfite, and then use deionized water to dissolve the reaction solution Washing to neutrality, then the reaction solution was left to stand, layered and separated to separate vinyl sulfite 224.55g (purity is 98.97%), then the isolated vinyl sulfite was added to the second reaction kettle for subsequent use;

[0025] (2) Oxidation reaction: first add 450 g of dichloromethane as a solvent and 49.38 g of ferric sulfate ...

Embodiment 3

[0028] The preparation method of vinyl sulfate, including substitution reaction and oxidation reaction, also includes refining process,

[0029] Specific steps are as follows :

[0030](1) Substitution reaction: Thionyl chloride and ethylene glycol are used as the reaction raw materials for the substitution reaction. First, 130.0g (1mol) of ethylene glycol is added to the first reaction kettle, and then the Add 619.5g (2.5mol) of thionyl chloride dropwise for 2 hours. After the dropwise addition, keep it warm at 50°C for 1 hour to obtain a reaction solution containing vinyl sulfite, and then distill the reaction solution with deionized water. Washing to neutrality, then the reaction solution was left to stand, layered and separated to separate vinyl sulfite 223.64g (purity is 98.85%), then the isolated vinyl sulfite was added to the second reaction kettle for subsequent use;

[0031] (2) Oxidation reaction: first add 450 g of dichloromethane as a solvent and 106.04 g of a fer...

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PUM

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Abstract

The invention discloses a preparation method of vinyl sulfate. The preparation method comprises the following steps: (1) substitution reaction: carrying out substitution reaction on thionyl chloride and ethanediol used as raw materials, washing the reaction solution with deionized water to a neutral state, standing, stratifying, and separating to obtain vinyl sulfite; (2) oxidation reaction: adding dichloromethane and a ferric sulfate solution into the vinyl sulfite, cooling to 0-5 DEG C, dropwisely adding a sodium percarbonate solution to obtain a water-phase / organic-phase-coexistent reaction solution, standing the reaction solution, stratifying, separating out the water phase, and carrying out reduced pressure distillation on the organic phase, thereby obtaining the vinyl sulfate crude product; and refinement: recrystallizing the vinyl sulfate crude product by using dichloromethane to obtain the high-purity vinyl sulfate. The preparation method has the characteristics of high mole yield, high product purity, low moisture content, low acid value and low preparation cost. The mole yield can reach 85% or above, the purity can reach 99% or above, the moisture content is less than or equal to 60 ppm, and the acid value is less than or equal to 60 ppm.

Description

technical field [0001] The invention relates to the field of electrolyte additives for lithium ion batteries, in particular to a preparation method of vinyl sulfate that can be used as an additive for electrolytes of lithium ion batteries. Background technique [0002] Vinyl sulfate is an additive that can make the electrolyte of lithium-ion batteries more effective. Adding vinyl sulfate to the lithium-ion battery electrolyte can inhibit the decline of the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after being placed at high temperature, and improve the charge-discharge performance and cycle times of the battery. At present, the disclosed preparation method of vinyl sulfate has the following disadvantages: one, the molar yield and purity of the product are not high, and the moisture content and acid value of the product are relatively high; two, the raw materials are not easy to obtain, and the preparation co...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 刘冬许国荣戴江英姚双开庞宝华丁敬敏
Owner 江苏瀚康新材料有限公司
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