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Method for preparing ethylene 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 unresolved purity and yield, difficult availability of product raw materials, and impossibility of industrial production, etc., to achieve reduced oxidation time and low moisture content , reduce the effect of hydrolysis

Inactive Publication Date: 2019-03-19
东营石大胜华新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The problem at present is: for a long time, many production enterprises have been researching the production process of vinyl sulfate, trying to make a breakthrough in this field, but because the raw materials of the product are not easy to get, the preparation cost is high, and the purity and yield cannot be solved. The problem is that it has not been able to be industrialized

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  • Method for preparing ethylene sulfate
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  • Method for preparing ethylene sulfate

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preparation example Construction

[0034] The preparation method of vinyl sulfate mentioned in the present invention, its detailed preparation method, comprises the following steps:

[0035] (1) Add ethylene glycol into the reaction kettle, then slowly add thionyl chloride dropwise to it, and control the reaction temperature at 25-30°C;

[0036] (2) After the dropwise addition is completed, raise the temperature to 40°C, keep it warm for 1 hour, continue to raise the temperature to 50°C, and keep it warm for 2 hours;

[0037] (3) After the heat preservation is over, cool to room temperature, add deionized water to the obtained solution for washing, and add sodium carbonate solution to adjust the pH value to neutral, let stand for a period of time, and separate vinyl sulfite after layering solution;

[0038] (4) Put the vinyl sulfite obtained above into the oxidation kettle, and add ice cubes to control the initial temperature at 0-5°C;

[0039] (5) Add buffering agent to the oxidation kettle to adjust the pH ...

Embodiment 1

[0049] Embodiment 1: the preparation method of vinyl sulfate mentioned in the present invention comprises substitution reaction, oxidation reaction and refining process, and concrete steps are as follows:

[0050] (1) Substitution reaction: Thionyl chloride and ethylene glycol are used as the reaction raw materials for the substitution reaction. First, 1325g (10mol) of ethylene glycol is added to the reaction kettle, and then chlorine is added dropwise to the first reaction kettle at room temperature. 3012g (12mol) of sulfoxide, the dropping time is 1h, and the dropping temperature is controlled at 28°C. After the dropwise addition, keep the temperature at 40°C for 1 hour, then increase the temperature to 50°C, and keep the temperature for 2 hours. Thereby obtain the reaction solution containing vinyl sulfite, wash the reaction solution with deionized water, then leave the reaction solution, layered and separate vinyl sulfite 2413g (purity is 98.92%), then separate the Vinyl ...

Embodiment 2

[0053] Embodiment 2: a kind of vinyl sulfate preparation method is: comprise substitution reaction, oxidation reaction and refining process, concrete steps are as follows:

[0054] (1) Substitution reaction: Thionyl chloride and ethylene glycol are used as reaction raw materials for substitution reaction. First, 1300g (10mol) of ethylene glycol is added to the reaction kettle, and then chlorine is added dropwise to the first reaction kettle at room temperature. Sulfoxide 3300g (13mol), the dropwise addition time is 1.5h, and the dropwise addition temperature is controlled at 30°C. After the dropwise addition, keep the temperature at 37°C for 1 hour, then increase the temperature to 50°C, and keep the temperature for 2 hours. Thereby obtain the reaction solution containing vinyl sulfite, wash the reaction solution with deionized water, then let the reaction solution stand, layer and separate vinyl sulfite 2614g (purity is 98.17%), then separate the Vinyl sulfite is added to th...

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Abstract

The invention relates to a method for preparing ethylene sulfate. According to the technical scheme, the method comprises the following steps: firstly, taking sulfoxide chloride and ethylene glycol asreactive raw materials to carry out a substitution reaction; secondly, adding a catalyst and a buffer agent into the reaction product, and oxidizing with sodium hypochlorite; and thirdly, centrifuging the reactant in the previous step, re-crystallizing, filtering, refining, and drying, thereby obtaining the finished product. The method disclosed by the invention has the beneficial effects that the method has the characteristics of being readily available in reactive raw materials, low in preparation cost, high in molar yield, high in purity of the prepared product and low in moisture content,the reaction can be rapidly and efficiently carried out by the catalyst adopted in the invention, the oxidation time is reduced, and hydrolysis of the ethylene sulfate is reduced. In addition, the mixed aqueous solution of ammonium di-hydrogen phosphate and borax is adopted as a buffer agent needed by oxidation, the oxidative pH value can be effectively controlled to be 6-7, and stable oxidationis promoted. Moreover, by taking magnesium sulfate as a water removal agent, the moisture of the product is controlled to be 50ppm or less.

Description

technical field [0001] The invention relates to the preparation of a lithium ion battery electrolyte additive, in particular to a preparation method of vinyl sulfate. Background technique [0002] In recent years, the field of lithium-ion batteries has developed rapidly, the range of use of lithium-ion batteries is expanding, and the technology is also improving. Adding some additives to the electrolyte of lithium-ion batteries can improve various performances of the battery. [0003] Among them, vinyl sulfate is an SEI film-forming additive that can form an SEI film at the initial stage of charging to prevent lithium ions from reacting with carbon negative electrodes or other substances during charge and discharge. In addition, the SEI film functions as an ion channel and allows only lithium ions to pass through. The ion channel can prevent the destruction of the structure of the carbon negative electrode due to the co-intercalation of the organic solvent with high molecul...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 郭建军
Owner 东营石大胜华新能源有限公司
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