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Preparation method of 1-fluorine-disulfonic anhydride

A technology of ethanedisulfonic anhydride and ethanedisulfonic acid, which is applied in the field of preparation of 1-fluoro-ethanedisulfonic anhydride and 1-fluoro-ethanedisulfonic anhydride, can solve unfavorable mass production, green environmental protection concept, and equipment investment Large, high energy consumption and other issues, to achieve the effect of improving charge and discharge performance and cycle times, small equipment investment, and high yield

Inactive Publication Date: 2018-04-27
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 of 1-fluorine-disulfonic anhydride
  • Preparation method of 1-fluorine-disulfonic anhydride
  • Preparation method of 1-fluorine-disulfonic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 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, to obtain 17g ethanedisulfonic anhydride, the yield is 98.8%;

[0022] Pass fluorine gas into the ethanedisulfonic anhydride obtained above, control the molar ratio of ethanedisulfonic anhydride and fluorine gas to 1:0.8, and prepare 18.25g of 1-fluoro-ethanedisulfonic anhydride (CAS1234622-61-7). The rate is 97.2%. The total yield was calculated to be 96.03%.

[0023] The purity of the obtained 1-fluoro-ethanedisulfonic anhydride is 99.8%, the boiling point is 338.6°C, 760mmHg, 1.99g / cm 3 , the impurity content of ethanedisulfonic acid and 1,2-difluoroethanedisulfonic anhydride is detected to be less than 1ppm, and the 1H NMR spectrum is as follows figure 1 shown.

Embodiment 2

[0025] 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 16.77g ethanedisulfonic anhydride, the yield is 97.5%;

[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 1:0.5, and 17.84 g of 1-fluoro-ethanedisulfonic anhydride was prepared with a yield of 96.3%. The calculated total yield was 93.89%.

[0027] The purity of the obtained 1-fluoro-ethanedisulfonic anhydride is 99.6%, the boiling point is 337.8°C, 760mmHg, 2.01g / cm 3 , The impurity content of ethanedisulfonic acid and 1,2-difluoroethanedisulfonic anhydride was detected to be less than 1ppm.

Embodiment 3

[0029] 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 16.9g ethanedisulfonic anhydride, the yield is 98.25%;

[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 1:0.7 to prepare 18.07 g of 1-fluoro-ethanedisulfonic anhydride with a yield of 96.79%. The total yield was calculated to be 95.1%.

[0031] The purity of the obtained 1-fluoro-ethanedisulfonic anhydride is 99.7%, the boiling point is 338.4°C, 760mmHg, 1.98g / cm 3 , The impurity content of ethanedisulfonic acid and 1,2-difluoroethanedisulfonic anhydride was detected to be less than 1ppm.

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Abstract

A preparation method of 1-fluorine-disulfonic anhydride belongs to the technical field of a battery electrolyte additive and comprises the following steps of A, taking disulfonic anhydride as a raw material, adding a molecule sieve, performing reaction with phosphorus trichloride for 5 hours under a normal temperature, rising the temperature to 180-200 DEG C, continuing to reaction for 2-5 hours under vacuum degree of 1-3mmHg, and performing extraction and crystallization on dichloromethane to obtain the disulfonic anhydride; and B, introducing fluorine gas into the disulfonic anhydride obtained in the step A, controlling a mole ratio of the disulfonic anhydride and the fluorine gas to be 1:(0.5-0.9), and preparing to obtain the 1-fluorine-disulfonic anhydride. The preparation method is simple, and the prepared 1-fluorine-disulfonic anhydride is high in yield and purity and has good an effect when applied to a battery electrolyte.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, relates to 1-fluoro-ethanedisulfonic anhydride used in battery electrolyte, and specifically relates to a preparation method of 1-fluoro-ethanedisulfonic anhydride. The preparation method of the invention is simple, the yield of the prepared 1-fluoro-ethanedisulfonic acid anhydride is high, the purity is high, and the effect is good when applied to the 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 secondary batterie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0567
CPCH01M10/0567Y02E60/10
Inventor 闫彩桥刘鹏侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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