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A kind of purification and decolorization method of sulfuric acid ester

A sulfate and decolorization technology, applied in organic chemistry and other directions, can solve the problems of purification and decolorization, deep color, low purity, etc., and achieve the effect of reducing color number

Active Publication Date: 2022-05-24
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, liquid sulfuric acid esters cannot be purified and decolorized by conventional vacuum distillation, so the color of the substance is usually darker and the purity is lower, and directly adding it to the electrolyte will affect the quality of the electrolyte

Method used

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  • A kind of purification and decolorization method of sulfuric acid ester
  • A kind of purification and decolorization method of sulfuric acid ester
  • A kind of purification and decolorization method of sulfuric acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The purification and decolorization method of sulfuric acid ester described in the present embodiment is as follows:

[0029] Select 500 g of 4-ethyl vinyl sulfate with a purity of 98.9% and a moisture content of 400 ppm, add 1.610 g of hexamethyldisilazane to the 4-ethyl vinyl sulfate for dehydration pretreatment, and react at room temperature for 9 hours. The water content in the 4-ethyl vinyl sulfate after dehydration pretreatment was 20 ppm.

[0030] Add 0.25g BHT to the 4-ethyl vinyl sulfate pretreated by dehydration, and put it into the molecular distillation feed pump storage tank after mixing. , the oil bath was set at 90°C, cooled at 0°C, and after the above parameters were stabilized, the stirring was started, and the stirring speed was 200 rpm, and the light group was collected by feeding the material. The results confirmed that it was the target product 4-ethyl vinyl sulfate, the purity was 99.5%, and the appearance was colorless and transparent.

Embodiment 2

[0032] The purification and decolorization method of sulfuric acid ester described in the present embodiment is as follows:

[0033] Select 500 g of 4-methyl vinyl sulfate with a purity of 98.6% and a moisture content of 200 ppm, add 0.805 g of hexamethyldisilazane to the 4-methyl vinyl sulfate for dehydration pretreatment, and react at room temperature for 3 hours. The water content in the 4-methyl vinyl sulfate after dehydration pretreatment was 30 ppm.

[0034] Add 0.375g BHA to the 4-methyl vinyl sulfate pretreated by dehydration, and put it into the molecular distillation feed pump storage tank after mixing. , the oil bath was set to 80°C, cooled to 0°C, and after the above parameters were stabilized, the stirring was started, and the stirring speed was 150 rpm, and the light group was collected by feeding the material. As a result, it was confirmed that it was the target product, 4-methyl vinyl sulfate, with a purity of 99.5% and a colorless and transparent appearance. ...

Embodiment 3

[0036] The purification and decolorization method of sulfuric acid ester described in the present embodiment is as follows:

[0037] Select 500g of 4-propyl vinyl sulfate with a purity of 98.9% and a moisture content of 400ppm, add 1.789g of hexamethyldisilazane to the 4-propyl vinyl sulfate for dehydration pretreatment, and measure it after 3 hours of reaction at room temperature The water content in the 4-propyl vinyl sulfate after dehydration pretreatment was 30 ppm.

[0038] Add 0.495g BHA to the 4-propyl vinyl sulfate pretreated by dehydration, and put it into the molecular distillation feed pump storage tank after mixing. , the oil bath is set at 80°C, and cooled to -10°C. After the above parameters are stabilized, the stirring is turned on, and the stirring speed is 150 rpm. The light group is collected by feeding the material, and the light group is characterized by GC-MS (gas chromatography-mass spectrometer) and nuclear magnetic resonance. , the results confirmed th...

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Abstract

The invention discloses a method for purifying and decolorizing sulfuric acid esters. The specific steps are as follows: adding a dehydrating agent to liquid sulfuric acid esters for dehydration pretreatment, adding a stabilizer after the dehydration pretreatment, and performing purification and decolorization by molecular distillation. The above method can purify and decolorize the liquid sulfuric acid ester, reduce the color number of the finished sulfuric acid ester, and make the finished sulfuric acid ester more suitable as an additive for the electrolyte.

Description

technical field [0001] The invention relates to a purification and decolorization method of sulfate. Background technique [0002] In recent years, with the continuous enhancement of people's awareness of environmental protection and the issue of green and sustainable energy development, the research on high-energy chemical power sources has continued to develop in depth around the world. Among them, lithium-ion batteries have become one of the types of power sources with practical advantages. It is a kind of battery that uses lithium metal or lithium alloy as negative electrode material and uses non-hydrolyzable electrolyte solution. [0003] The electrolyte system, which is an important component of lithium-ion batteries, has also undergone continuous development. Whether it is electrolyte lithium salts, new organic solvents or electrolyte additives, research on these components has also been carried out. [0004] Since additives can have a great impact on battery perform...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 常楠卢云龙陶力刘磊陈晓华刘栋成
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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