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Preparation method for perfluoro-substituted disulfonic anhydride

A technology of disulfonic anhydride and ethylene disulfonic anhydride, which is applied in the field of preparation of perfluoro-substituted disulfonic anhydride and perfluoro-substituted disulfonic anhydride. Problems, achieve the effect of improving charge and discharge performance and cycle times, small equipment investment, and less three wastes

Inactive Publication Date: 2018-05-01
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the existing battery electrolyte additives are prepared, there are many wastes, high energy consumption, long working hours, and large investment in equipment, which is not conducive to industrialized mass production and the concept of green environmental protection.

Method used

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  • Preparation method for perfluoro-substituted disulfonic anhydride
  • Preparation method for perfluoro-substituted disulfonic anhydride
  • Preparation method for perfluoro-substituted disulfonic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 0.1mol (19g) of ethanedisulfonic acid, add molecular sieves, add 76g of phosphorus trichloride and react at room temperature for 5 hours, then raise the temperature to 180°C, continue to react for 3 hours under a vacuum of 1-3mmHg, and then extract with dichloromethane, Crystallization was carried out to obtain 17.05g of ethanedisulfonic anhydride with a yield of 99.13%;

[0026] Fluorine gas was passed into the ethanedisulfonic anhydride obtained above, and the molar ratio of ethanedisulfonic anhydride to fluorine gas was controlled to be 1:6 to prepare 23.5 g of perfluoro-substituted ethanedisulfonic anhydride with a yield of 97.19%. The total yield was calculated to be 96.34%.

[0027] The purity of the obtained perfluoro-substituted ethanedisulfonic anhydride is 99.8%, the boiling point is 259.3°C, 760mmHg, and the density is 2.18g / cm 3 , The impurity content of ethanedisulfonic acid and difluoro-substituted disulfonic anhydride is less than 1ppm.

Embodiment 2

[0029] Take 0.1mol (19g) of ethanedisulfonic acid, add molecular sieves, add 57g of phosphorus trichloride and react at room temperature for 8 hours, then raise the temperature to 200°C, continue to react for 5 hours under a vacuum of 1-3mmHg, and then extract with dichloromethane, Crystallization, to obtain 16.75g of ethanedisulfonic anhydride, the yield is 97.38%;

[0030] Fluorine gas was passed into the ethanedisulfonic anhydride obtained above, and the molar ratio of ethanedisulfonic anhydride to fluorine gas was controlled to be 1:4, and 22.9 g of perfluoro-substituted ethanedisulfonic anhydride were prepared with a yield of 96.4%. The calculated total yield was 93.87%.

[0031] The purity of the obtained perfluoro-substituted ethanedisulfonic anhydride is 99.85%, the boiling point is 259.6°C, 760mmHg, and the density is 2.17g / cm 3 , The impurity content of ethanedisulfonic acid and difluoro-substituted disulfonic anhydride is less than 1ppm.

Embodiment 3

[0033] Take 0.1mol (19g) of ethanedisulfonic acid, add molecular sieves, add 95g of phosphorus trichloride and react at room temperature for 6 hours, then raise the temperature to 190°C, continue to react for 2 hours under a vacuum of 1-3mmHg, and then extract with dichloromethane, Crystallization, to obtain 16.89g ethanedisulfonic anhydride, the yield is 98.2%;

[0034] Fluorine gas was passed into the ethanedisulfonic anhydride obtained above, and the molar ratio of ethanedisulfonic anhydride to fluorine gas was controlled to be 1:7, and 23.14 g of perfluoro-substituted ethanedisulfonic anhydride was prepared with a yield of 96.58%. The calculated total yield was 94.84%.

[0035] The purity of the obtained perfluoro-substituted ethanedisulfonic anhydride is 99.87%, the boiling point is 259.2°C, 760mmHg, and the density is 2.19g / cm 3 , The impurity content of ethanedisulfonic acid and difluoro-substituted disulfonic anhydride is less than 1ppm.

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Abstract

The invention provides a preparation method for perfluoro-substituted disulfonic anhydride, belonging to the technical field of battery electrolyte additives. The preparation method comprises the following steps: A, with ethanedisulfonic acid or propanedisulfonic acid as a raw material, adding a molecular sieve into the ethanedisulfonic acid or the propanedisulfonic acid, allowing an obtained mixture to react with phosphorus trichloride at a normal temperature for 5 h, then carrying out heating to 180 to 200 DEG C, continuing a reaction at a vacuum degree of 1 to 3 mmHg for 2 to 5 h, then carrying out extraction through dichloromethane, and carrying out crystallization so as to obtain ethanedisulfonic anhydride or propanedisulfonic anhydride; and B, introducing fluorine gas into the ethanedisulfonic anhydride or the propanedisulfonic anhydride obtained in the step A, and controlling a mol ratio of the ethanedisulfonic anhydride / the propanedisulfonic anhydride to the fluorine gas to be1: (4-10) so as to prepare the perfluoro-substituted disulfonic anhydride. The preparation method provided by the invention is simple; and the perfluoro-substituted disulfonic anhydride prepared by using the preparation method provided by the invention has high yield and high purity, and has good effects when applied to battery electrolytes.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, relates to perfluoro-substituted disulfonic anhydrides used in battery electrolytes, and specifically relates to a preparation method of perfluoro-substituted disulfonic anhydrides. The preparation method of the invention is simple, and the prepared perfluoro-substituted disulfonic acid anhydride has high yield and high purity, and the effect is good when applied to battery electrolyte. Background technique [0002] In recent years, portable electronic devices such as video cameras, digital cameras, cellular phones, and notebook computers have been widely used, and reducing their size and weight and achieving their long lifespan have become urgent demands. Accompanying this demand, batteries, particularly secondary batteries that are small and lightweight and capable of obtaining high energy density have been developed as power sources. [0003] Among them, lithium ion seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/00H01M10/0567
CPCC07D327/00H01M10/0567H01M2300/0025Y02E60/10
Inventor 王军刘鹏闫鹏飞
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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