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Method for preparing ethylene sulfate by using microchannel reactor

A microchannel reactor, vinyl sulfate technology, applied in the direction of organic chemistry, etc., can solve the problems of poor temperature control effect, low production capacity per unit time, and long mixing and dissolving time in the single-pot reaction, so as to shorten the production cycle and have no amplification effect. , beneficial to industrial applications

Active Publication Date: 2018-05-01
ZHANGJIAGANG HICOMER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation method of vinyl sulfate, such as the technical scheme disclosed in the application number 2016100158438, has the disadvantages of: intermittent operation, low production capacity per unit time, and large energy consumption; The mixing and removal time is long, the separation is slow, and by-products are easily produced, and the molar yield is not high

Method used

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  • Method for preparing ethylene sulfate by using microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]Raw material preparation: sodium hypochlorite solution: the mass concentration is 13%, and the mass is 689g. Dichloromethane solution of vinyl sulfite: Dissolve 108g of vinyl sulfite in 1200g of dichloromethane at room temperature, and keep stirring to configure, with a mass concentration of 9%. Sodium bicarbonate solution: Dissolve 84g of sodium bicarbonate in 1120g of deionized water at room temperature and stir continuously, with a mass concentration of 7%. Ruthenium trichloride solution: prepared by dissolving 0.78g of ruthenium trichloride in 48g of deionized water at room temperature, stirring continuously, with a mass concentration of 1.6%. The molar ratio of vinyl sulfite to sodium hypochlorite is 1:1.2, and the molar ratio of ruthenium trichloride to vinyl sulfite is 0.03%.

[0025] The preparation process is as follows: set the temperature of the temperature control tank 1 at -10 to 10°C, prepare the prepared dichloromethane solution of vinyl sulfite with a ma...

Embodiment 2

[0027] Raw material preparation: sodium hypochlorite solution: the mass concentration is 13%, and the mass is 687g. Dichloromethane solution of vinyl sulfite: Dissolve 108g of vinyl sulfite in 1200g of dichloromethane at room temperature, and keep stirring to configure, with a mass concentration of 9%. Sodium bicarbonate solution: Dissolve 84g of sodium bicarbonate in 1120g of deionized water at room temperature and stir continuously, with a mass concentration of 7%. Ruthenium trichloride solution: prepared by dissolving 0.78g of ruthenium trichloride in 48g of deionized water at room temperature, stirring continuously, with a mass concentration of 1.6%. The molar ratio of vinyl sulfite to sodium hypochlorite is 1:1.2, and the molar ratio of ruthenium trichloride to vinyl sulfite is 0.03%.

[0028] The preparation process is as follows: set the temperature of the temperature control tank 1 at -10 to 10°C, prepare the prepared dichloromethane solution of vinyl sulfite with a m...

Embodiment 3

[0030] Raw material preparation: sodium hypochlorite solution: the mass concentration is 13%, and the mass is 687g. Dichloromethane solution of vinyl sulfite: Dissolve 108g of vinyl sulfite in 1200g of dichloromethane at room temperature, and keep stirring to configure, with a mass concentration of 9%. Sodium bicarbonate solution: Dissolve 84g of sodium bicarbonate in 1120g of deionized water at room temperature and stir continuously, with a mass concentration of 7%. Ruthenium trichloride solution: prepared by dissolving 0.78g of ruthenium trichloride in 48g of deionized water at room temperature, stirring continuously, with a mass concentration of 1.6%. The molar ratio of vinyl sulfite to sodium hypochlorite is 1:1.2, and the molar ratio of ruthenium trichloride to vinyl sulfite is 0.03%.

[0031] The preparation process is as follows: set the temperature of the temperature control tank 1 at -20 to 20°C, prepare the prepared dichloromethane solution of vinyl sulfite with a m...

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Abstract

The invention discloses a method for preparing ethylene sulfate by using a microchannel reactor, wherein the method has a high yield and high product purity and is convenient for industrial application. Production equipment includes the microchannel reactor, the microchannel reactor is internally provided with a premixer and a microchannel module, the premixer communicates with three micro-pumps,an oxidant micropump communicates with a conveying pipe between the premixer and the microchannel module, and a material discharge pipe is arranged at the material discharge end of the microchannel module. The temperature of the microchannel reactor is controlled at -30 to 30 DEG C, a dichloromethane solution of glycol sulfite, a sodium bicarbonate solution and a ruthenium trichloride solution areseparately pumped by the three micropumps to the premixer to form a mixed solution, a sodium hypochlorite solution is pumped by the oxidant micropump, the sodium hypochlorite solution and the mixed solution are pumped synchronously to a microchannel in the microchannel module for an oxidation reaction, a reaction solution generated after complete reaction in the microchannel module is delivered outwards from the material discharge pipe, and the reaction solution is sequentially subjected to layering, drying and concentration, so that the target product ethylene sulfate is obtained.

Description

technical field [0001] The invention relates to the technical field of additives for lithium battery electrolytes, in particular to a preparation method of vinyl sulfate. Background technique [0002] Microchannel reactor technology emerged in the 1990s. It can not only enhance mass transfer and heat transfer, but also meet continuous large-scale production, so it has attracted widespread attention. The microchannel reactor achieves instantaneous uniform mixing of materials and efficient heat transfer through the collision of reaction fluids. The microchannel reactor is equipped with a microchannel module, and the microchannel module is provided with a microchannel. [0003] Vinyl sulfate is a new type of organic film-forming additive for sulfate ester lithium battery electrolyte with excellent effect. Due to the stronger electronegativity of the central sulfur atom, the reducibility at the graphite negative electrode interface is stronger than that of the corresponding car...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 赵建庞宝华谢栋翟涛张宇许国荣
Owner ZHANGJIAGANG HICOMER CHEM CO LTD
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