Method for synthesizing ethylene sulfate

A technology of vinyl sulfate and vinyl sulfite, which is applied in the field of synthesis of vinyl sulfate, can solve the problems of poor battery performance and achieve the effects of improving purity and yield, good catalytic effect, and high acid value

Inactive Publication Date: 2018-10-16
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention provides the synthetic method of vinyl sulfate in order to solve the defect of poor battery performance in high temperature conditions in the prior art, which is simple to operate, and the synthetic vinyl sulfate has high yield and high purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1), in a 200ml autoclave with electromagnetic valve stirring, add 5.0g composite catalyst (the composite catalyst is composed of iron trichloride, ruthenium trichloride and ruthenium dioxide with a molar ratio of 2:1:1), After replacing the air with nitrogen, add 100g of ethylene oxide, then heat up the reaction solution, but when the reaction temperature rises to 120°C, feed sulfur dioxide gas to 8MPa, and keep the temperature and pressure for 1.5h. Pass cooling water through the kettle, cool to 40-50°C, discharge the product in the kettle to obtain a crude product of vinyl sulfite, and conduct vacuum distillation on the obtained crude product to obtain 241.03 g of refined vinyl sulfite, which is analyzed by chromatography , the purity is 99.2%, and the yield is 98.2% (relative to ethylene oxide).

[0024] (2), add aqueous sodium bicarbonate solution to the vinyl sulfite obtained in step (1), adjust the pH value to 8-9, cool down to -5-3°C, and dropwise add high The ...

Embodiment 2

[0027] (1), in a 200ml autoclave with electromagnetic valve stirring, add 8.0g composite catalyst (the composite catalyst is composed of iron trichloride, ruthenium trichloride and ruthenium dioxide with a molar ratio of 3:2:1), After replacing the air with nitrogen, add 100g of ethylene oxide, then heat up the reaction solution, but when the reaction temperature rises to 140°C, feed sulfur dioxide gas to 6MPa, and keep the temperature and pressure for 2h. Cooling water was passed inside, cooled to 40-50°C, and the product in the kettle was discharged to obtain a crude product of vinyl sulfite, which was subjected to vacuum distillation to obtain 242.5 g of refined vinyl sulfite, which was analyzed by chromatography. The purity was 99.4%, and the yield was 98.8% (relative to ethylene oxide).

[0028] (2), add aqueous sodium bicarbonate solution to the vinyl sulfite obtained in step (1), adjust the pH value to 8-9, cool down to -3-5°C, and dropwise add high The mixed solution ...

Embodiment 3

[0031] (1), in a 200ml autoclave with electromagnetic valve stirring, add 10.0g composite catalyst (the composite catalyst is composed of iron trichloride, ruthenium trichloride and ruthenium dioxide with a molar ratio of 4:1:2), After replacing the air with nitrogen, add 100g of ethylene oxide, then heat up the reaction solution, but when the reaction temperature rises to 160°C, feed sulfur dioxide gas to 10MPa, and keep the temperature and pressure for 2.5h. Pass cooling water through the kettle, cool to 40-50°C, discharge the product in the kettle to obtain a crude product of vinyl sulfite, and conduct vacuum distillation on the obtained crude product to obtain 241.77 g of refined vinyl sulfite, which is analyzed by chromatography , the purity is 99.5%, and the yield is 98.5% (relative to ethylene oxide).

[0032] (2), add sodium bicarbonate aqueous solution to the vinyl sulfite obtained in step (1), adjust the pH value to 8-9, cool down to -4 ~ 1 ° C, dropwise add high Th...

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Abstract

The invention relates to a method for synthesizing ethylene sulfate, and belongs to the technical field of chemical power supplies. The method comprises the following steps: A, carrying out a contactreaction on sulfur dioxide with ethylene oxide in the presence of a composite catalyst, controlling the reaction temperature to be 120-160 DEG C, introducing sulfur dioxide gas to keep the pressure ofthe reaction system at 5-12 MPa, and controlling the reaction time at 1-2.5 hours to obtain ethylene sulfite for standby use; B, adding an aqueous solution of sodium hydrogen carbonate into the ethylene sulfite obtained in the step A, carrying out cooling to a temperature ranging from -5 DEG C to 5 DEG C, dropwise adding a mixed solution of sodium periodate and ruthenium trichloride under a condition with a temperature ranging from -5 DEG C to 5 DEG C, keeping the temperature for 1-1.5 hours after the adding is completed so as to obtain a reaction solution with co-existed water phase and organic phase, carrying out standing for layering, and separating out the water phase to obtain the organic phase, namely a crude product of the ethylene sulfate; and C, carrying out molecular distillation on the crude product of the ethylene sulfate obtained in the step B under the condition with a temperature of 70-80 DEG C to obtain the ethylene sulfate. The ethylene sulfate prepared by the methodhas high purity and high yield, and when the ethylene sulfate is added into a battery, the performance of the battery is better.

Description

technical field [0001] The invention belongs to the technical field of chemical power sources, and in particular relates to a synthesis method of vinyl sulfate. 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 releas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 闫彩桥刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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