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Production method of 3,3-biethylene sulfate

A technology of vinyl disulfate and vinyl disulfite, which is applied in the field of production of 3,3-vinyl disulfite, can solve the problems of affecting battery performance, affecting the reaction process, troublesome solvent handling, etc. Achieve the effects of preventing capacity reduction, avoiding hydrolysis, and improving purity and yield

Inactive Publication Date: 2017-06-30
TIANJIN XINYUAN GUANGTAI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation of additives, carbon tetrachloride is used as a solvent to provide polarity. During the reaction, hydrogen chloride will be generated and dissolved in carbon tetrachloride, which will affect the reaction process and troublesome solvent handling in the later stage. , is not easy to remove, and carbon tetrachloride is a toxic product, which is harmful to the human body and is not recommended to be used; at the same time, sodium periodate and ruthenium trichloride are used in the reaction, so that the 3,3-disulfuric acid ethylene produced by oxidation Esters are prone to hydrolysis, the yield is very low, and the purity is poor, which affects their performance in batteries

Method used

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  • Production method of 3,3-biethylene sulfate
  • Production method of 3,3-biethylene sulfate
  • Production method of 3,3-biethylene sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1, using thionyl chloride and erythritol as reaction raw materials for addition reaction to obtain the intermediate 3,3-diethylene disulfite; adding thionyl chloride to the first reaction kettle and lowering the temperature To -15°C, add erythritol dropwise, fully react at -15°C to obtain the first reaction liquid, then carry out vacuum distillation on the first reaction liquid, and distill out the intermediate 3,3-bidia Vinyl sulfate is refluxed into the second reaction kettle by condensation and reflux; the molar ratio of thionyl chloride and erythritol is 3:1; the erythritol is added dropwise to the first reaction kettle by dropping at a constant speed , took 1 hour; the reaction time was 1 hour, the time to continue the reaction after adding erythritol dropwise; mechanical stirring was carried out in the first reaction kettle, so that thionyl chloride and erythritol fully contacted and reacted .

[0037] Step 2, intermediate oxidation reaction to obtain 3,3-di...

Embodiment 2

[0041] Step 1, using thionyl chloride and erythritol as reaction raw materials for addition reaction to obtain the intermediate 3,3-diethylene disulfite; adding thionyl chloride to the first reaction kettle and lowering the temperature To -10°C, add erythritol dropwise, and react fully at -10°C to obtain the first reaction solution, and then carry out vacuum distillation on the first reaction solution to distill out the intermediate 3,3-bidia Vinyl sulfate is refluxed into the second reaction kettle through condensation and reflux; the molar ratio of thionyl chloride and erythritol is 2:1; the erythritol is added dropwise to the first reaction kettle by dropping at a constant speed , during 2 hours; the reaction time was 3 hours, and the reaction time included the time of dripping erythritol, and the time to continue the reaction after dripping erythritol; ultrasonic dispersion was carried out in the first reactor, so that Thionyl chloride and erythritol fully contact and reac...

Embodiment 3

[0046] Step 1, using thionyl chloride and erythritol as reaction raw materials for addition reaction to obtain the intermediate 3,3-diethylene disulfite; adding thionyl chloride to the first reaction kettle and lowering the temperature To -5°C, add erythritol dropwise, fully react at -5°C to obtain the first reaction liquid, then carry out vacuum distillation on the first reaction liquid, and distill out the intermediate 3,3-bidia Vinyl sulfate is refluxed into the second reaction kettle by condensation and reflux; the molar ratio of thionyl chloride and erythritol is 1:1; erythritol is added dropwise to the first reaction kettle by dropping at a constant speed , with a time of 1.5 hours; the reaction time was 3 hours, and the reaction time was the time for continuing the reaction after dripping erythritol; ultrasonic dispersion was carried out in the first reaction kettle, so that thionyl chloride and erythritol were fully Touch and react.

[0047] Step 2, intermediate oxida...

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Abstract

The invention discloses a production method of 3,3-biethylene sulfate. The production method comprises the following steps of by using thionyl chloride and erythritol as reaction raw materials, performing addition reaction, so as to obtain an intermediate, namely 3,3-biethylene sulfite; performing oxidizing reaction with sodium bicarbonate, sodium hypochlorite and a catalyst; finally, distilling molecules, so as to obtain the 3,3-biethylene sulfate. The 3,3-biethylene sulfate prepared by the technical scheme has the advantages that the purity can reach 99.5% or above, the water content is less than or equal to 100PPM, and the acid value is less than or equal to 100PPM; after the 3,3-biethylene sulfate is used as an electrolyte additive of a cell, an SEI film is formed on a negative electrode, the negative electrode is effectively protected, the degrading of capacity at high temperature is prevented, and the property of the cell at high temperature is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of chemical power sources, and in particular relates to a method for producing 3,3-vinyl disulfate. Background technique [0002] With the development of my country's electronic information industry, the demand for chemical power is increasing, and its performance requirements are getting higher and higher. Lithium-ion batteries have the advantages of small size, good safety performance, light weight, high specific energy, high voltage, long life, no pollution, etc., which are incomparable to other chemical power sources. The main power supply for portable electronic devices such as camcorders and digital cameras. In recent years, the basic research and application development of lithium-ion batteries have become one of the hot spots. A lithium battery includes a positive electrode, a negative electrode, an electrolyte, and a separator. However, during the charging and discharging process, the battery will...

Claims

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Application Information

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IPC IPC(8): C07D327/10H01M10/0569
CPCC07D327/10H01M10/0569Y02E60/10
Inventor 刘鹏
Owner TIANJIN XINYUAN GUANGTAI NEW MATERIAL TECH CO LTD
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