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Preparation method and application of 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 troublesome post-processing, low oxidation efficiency, and low product purity, and achieve simple post-processing, easy operation, and high yield Effect

Active Publication Date: 2018-11-16
LIAONING KELONG FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem is that the post-processing of the product is cumbersome and the product purity is low, which affects the performance and service life of the lithium battery
When synthesizing vinyl sulfite, organic matter is used as a solvent, which has the disadvantages of low oxidation efficiency and difficult product purification

Method used

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  • Preparation method and application of ethylene sulfate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Get 108.2g (1mol) vinyl sulfite, 200ml distilled water and 0.2g powdered catalyst (by mass ratio, CuO:NiO:Al 2 o 3 =1:0.85:1.3), stir slowly and evenly, control the temperature at 5°C, pass ozone 0.05L / min (ozone concentration is 20mL / L), and react for 45 minutes. After the reaction was finished, the mixture was left standing to separate layers, and the organic layer was taken. The organic layer was washed twice with distilled water and dried to obtain vinyl sulfate with a yield of 94.53%. The product was analyzed by liquid chromatography, and the results showed that the content of vinyl sulfate was 94.36%, and the content of vinyl sulfite was 5.52%.

Embodiment 2

[0020] Get 216.3g (2mol) vinyl sulfite, 200 milliliters of distilled water and 0.4g granular catalyst (by mass ratio, Cu:NiO:MnO 2 =1:1.2:0.8), stir slowly and evenly, control the temperature at 5°C, pass ozone 0.05L / min (ozone concentration is 20mL / L), and react for 45min. After the reaction was completed, the layers were left to stand, and the organic layer was taken. The organic layer was washed twice with distilled water and dried to obtain vinyl sulfate with a yield of 95.84%. The product was analyzed by liquid chromatography, and the results showed that the content of vinyl sulfate was 95.63%, and the content of vinyl sulfite was 4.28%.

Embodiment 3

[0022] Get 2.161kg (2mol) vinyl sulfite, 2L distilled water and 4g powdered catalyst (by mass ratio, Fe:MnO:Al 2 o 3 =1:1.1:0.9), stir slowly and evenly, control the temperature at 5°C, pass through ozone 0.05L / min (ozone concentration is 20mL / L), react for 60min, after the reaction is over, let it stand for stratification, and take the organic layer , the organic layer was washed twice with distilled water and dried to obtain vinyl sulfate with a yield of 95.17%. The product was analyzed by liquid chromatography, and the results showed that the vinyl sulfate content was 95.13%, and the vinyl sulfite content was 4.68%.

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Abstract

The invention relates to a preparation method and an application of ethylene sulfate. Ethylene sulfate is prepared through a catalytic oxidation reaction with glycol sulfite as a raw material, water as a reaction medium, metal and / or metal oxide as a catalyst and ozone as an oxidizing agent. The method has the characteristics that the yield is high, operation is convenient, aftertreatment is simple, no pollution is caused to the environment and the like.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of vinyl sulfate. Background technique [0002] With the development of my country's electronic information industry, the performance requirements for chemical power sources are getting higher and higher. Lithium-ion batteries have become the main power source of portable electronic devices due to their small size, good safety performance, light weight, and no pollution. Lithium-ion batteries will release heat during charging and discharging, resulting in reduced battery performance. In the prior art, the battery performance at high temperature is improved by adding vinyl sulfate additive to the electrolyte. The existing method for preparing vinyl sulfate is: oxidizing vinyl sulfite into vinyl sulfate in inorganic oxidation systems such as potassium permanganate, periodate and hypochlorite. The existing problem is that the post-processing of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 武显峰姜勇周济仓王炳帅姜艳
Owner LIAONING KELONG FINE CHEM
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