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Preparation process of ethylene sulfate

A technology for the preparation of vinyl sulfate, which is applied in the direction of organic chemistry, can solve the problems of low yield and difficulty in fully carrying out the reaction, and achieve the effects of increased product yield, short reaction route, low cost of raw and auxiliary materials and low manufacturing cost

Inactive Publication Date: 2021-10-29
河北津宏化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because vinyl sulfate is easily hydrolyzed to form a strong acidic substance, sodium bicarbonate needs to be added during the oxidation process for neutralization, and the pH range must be strictly controlled. Because the reaction system of this manufacturing method is heterogeneous, it is difficult to fully carry out the reaction. The yield is low and needs to be solved urgently

Method used

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  • Preparation process of ethylene sulfate
  • Preparation process of ethylene sulfate

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Experimental program
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Effect test

Embodiment 1

[0037] A kind of preparation technology of vinyl sulfate, comprises the following steps:

[0038] S1. Add 100kg of ethylene glycol weighed into the synthesis reaction kettle, then add 180kg of sodium ethoxide into the synthesis reaction kettle, then stir for 2 hours to mix evenly, and control the temperature in the reaction kettle to 0°C;

[0039] S2. Feed 120 kg of sulfuryl chloride into the reaction solution in S1. The speed of sulfuryl chloride feeding is 22 mL / min, and the pressure of feeding is 0.3-0.4 MPa. After reacting for 2 hours, blow nitrogen gas for 1 hour, and stir again for 2.5 hours. After standing still for 0.5h, the mixture of vinyl sulfate and metal chloride salt generated was separated to obtain crude vinyl sulfate, and the crude product of vinyl sulfate was dehydrated with anhydrous magnesium sulfate, and after dehydration, dichloroethane was used to dehydrate the crude product of vinyl sulfate. The crude product of vinyl sulfate is recrystallized, wherein ...

Embodiment 2

[0041] S1. Add 100kg of ethylene glycol weighed into the synthesis reaction kettle, then add 180kg of sodium ethoxide into the synthesis reaction kettle, then stir for 2 hours to mix evenly, and control the temperature in the reaction kettle to 5°C;

[0042] S2, feed 160 kg of sulfuryl chloride into the reaction solution in S1, the feed rate of sulfuryl chloride is 22mL / min, the pressure of feed is 0.3-0.4MPa, after reacting for 2h, blow nitrogen gas for 1h, and stir again for 2.5h, After standing still for 0.5h, the mixture of vinyl sulfate and metal chloride salt generated was separated to obtain crude vinyl sulfate, and the crude product of vinyl sulfate was dehydrated with anhydrous magnesium sulfate, and after dehydration, dichloroethane was used to dehydrate the crude product of vinyl sulfate. The crude product of vinyl sulfate is recrystallized, wherein the weight ratio of ethylene dichloride and vinyl sulfate is 1.5:1, and finally vacuum-dried to obtain high-purity viny...

Embodiment 3

[0044] S1. Add 100kg of ethylene glycol weighed into the synthesis reaction kettle, then add 215kg of sodium ethoxide into the synthesis reaction kettle, then stir for 2 hours to mix evenly, and control the temperature in the reaction kettle to 5°C;

[0045]S2. Introduce 160kg of sulfuryl fluoride into the reaction liquid in S1. The rate of introduction of sulfuryl fluoride is 22mL / min, and the pressure of introduction is 0.3-0.4MPa. After 2.5h of reaction, blow nitrogen gas for 1.5h and stir again React for 3h, after standing for 1h, separate the mixture of vinyl sulfate and metal fluoride salts to obtain the crude vinyl sulfate, use anhydrous magnesium sulfate to dehydrate the crude vinyl sulfate, and use dichloroethane to dehydrate the crude product after dehydration The vinyl sulfate crude product after dehydration carries out recrystallization, and wherein the weight ratio of ethylene dichloride and vinyl sulfate is 1.5:1, carries out vacuum drying at last and obtains high...

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Abstract

The invention relates to the technical field of lithium ion battery electrolyte additives, and particularly discloses a preparation process of ethylene sulfate. The preparation process comprises the steps of S1, taking ethylene glycol as an initial raw material, and performing exchange reaction with alkali metal alkoxide to generate alkali metal diol salt and lower alcohol; and S2, carrying out condensation reaction on the alkali metal diol salt and sulfuryl chloride or sulfuryl fluoride to generate ethylene sulfate and metal halide salt, and then refining to obtain ethylene sulfate. The method has the advantage of improving the product yield of ethylene sulfate.

Description

technical field [0001] The application relates to the technical field of lithium ion battery electrolyte additives, more specifically, it relates to a kind of preparation technology of vinyl sulfate. Background technique [0002] With the continuous advancement of lithium-ion battery technology, the requirements for electrolyte additives in lithium-ion batteries are also getting higher and higher. It is necessary for electrolyte additives to suppress the decline in the initial capacity of the battery, increase the initial discharge capacity, and reduce high temperature. The battery expansion caused by the environment also needs to improve the charge and discharge performance and cycle times of the battery. Electrolyte additives are an important part of lithium secondary batteries. Excellent electrolyte additives have positive electrochemical effects in lithium secondary batteries, which can improve the kinetic characteristics of the battery, thereby significantly improving t...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 刘康王宏义
Owner 河北津宏化工有限公司
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