Fluorosulfonate-based compound preparation method

A fluorosulfonic acid ester and compound technology, which is applied in the field of preparation of fluorosulfonic acid ester compounds, can solve the problems of unfavorable mass production and green environmental protection concept, affecting application effect, and high water content of additives, and achieves improvement of charge-discharge performance and cycle. The effect of the number of times, the three wastes is less, and the equipment investment is small

Inactive Publication Date: 2019-06-21
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 three wastes, high energy consumption, long working hours, and large equipment investment, which is not conducive to industrialized mass production and the concept of green environmental protection; the prepared additives have high moisture content and high acid value, which seriously affects the application. Effect

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  • Fluorosulfonate-based compound preparation method
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  • Fluorosulfonate-based compound preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of fluorosulfonyloxybenzene:

[0024] Chemical formula:

[0025] Take 1mmol of phenol, 1.1mmol of triethylamine, and 14mL of dioxane into the reaction vessel, stir at room temperature for 1h, pass 1mmol of sulfuryl fluoride gas into it, control the reaction pressure of the system to 7atm, and the reaction temperature to 50°C, and react for 24h. Then add hydrochloric acid aqueous solution to acidify for 20min, spin the solvent under reduced pressure, separate and purify by silica gel column chromatography, and select petroleum ether (60°C) and ethyl acetate with a volume ratio of 0.1:1 as the eluent to obtain 158.5 mg of fluorosulfonyl oxide Benzene.

[0026] The density of the detected fluorosulfonyloxybenzene is 1.42g / cm 3 , the boiling point is 221.3°C 760mmHg, the purity is 99.5%, the water content is 30ppm, the acid value is 36ppm, and the yield is 89.97%.

Embodiment 2

[0028] Preparation of fluorosulfonyloxyethane:

[0029] Chemical formula:

[0030] Take 1mmol of ethanol, 1.5mmol of triethylamine, and 8mL of dioxane into the reaction vessel, stir at room temperature for 2 hours, pass 1.1mmol of sulfuryl fluoride gas into it, control the reaction pressure of the system to 8 atm, and the reaction temperature to 45°C, and react for 20 hours , and then add hydrochloric acid aqueous solution to acidify for 30 minutes, spin the solvent under reduced pressure, separate and purify by silica gel column chromatography, and select petroleum ether (70°C) and ethyl acetate with a volume ratio of 0.2:1 as the eluent to obtain 119.15 mg of fluorosulfonyl Oxyethane.

[0031] The density of the detected fluorosulfonyloxyethane is 1.35g / cm 3 , the boiling point is 117.2°C 760mmHg, the purity is 99.7%, the water content is 27ppm, the acid value is 32ppm, and the yield is 93%.

Embodiment 3

[0033] Preparation of allyl fluorosulfonate:

[0034] Chemical formula:

[0035] Take 1mmol of allyl alcohol, 1.2mmol of triethylamine, and 10mL of dioxane into the reaction vessel, stir at room temperature for 1.5h, and pass 1.05mmol of sulfuryl fluoride gas into it, control the reaction pressure of the system to 9atm, and the reaction temperature to 40°C , reacted for 15h, then added hydrochloric acid aqueous solution to acidify for 25min, spin-dried the solvent under reduced pressure, separated and purified by silica gel column chromatography, and selected petroleum ether (80°C) and ethyl acetate with a volume ratio of 0.1:1 as the eluent to obtain 128.3mg Allyl Fluorosulfonate.

[0036] The density of the obtained allyl fluorosulfonate is 1.29g / cm 3 , the boiling point is 210°C 760mmHg, the purity is 99.5%, the water content is 23ppm, the acid value is 25ppm, and the yield is 91.64%.

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Abstract

The invention relates to a fluorosulfonate-based compound preparation method, and belongs to the technical field of battery electrolytic solution additives. The preparation method comprises: using phenol, ethanol, allyl alcohol or 4-pentyne-1-ol as a raw material, adding the raw material, triethylamine and dioxane to a reaction container, stirring for 1-2 h at a room temperature, introducing sulfuryl fluoride gas, carrying out a reaction for 12-24 h at a reaction temperature of 35-50 DEG C by controlling the reaction pressure of the system at 7-10 atm, adding a hydrochloric acid aqueous solution, acidifying for 20-30 min, carrying out pressure reducing rotary evaporation on the solvent, and carrying out separation purification to obtain fluorosulfonyloxybenzene, fluorosulfonyloxyethane, allyl fluorosulfonate or 4-pentyne-fluorosulfonate. According to the present invention, the preparation method is simple, and the prepared fluorosulfonate-based compound has characteristics of high purity, high yield, safety and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, relates to fluorosulfonate compounds applied to battery electrolyte, and specifically relates to a preparation method of fluorosulfonate compounds. The preparation method of the invention is simple, and the prepared fluorosulfonate compound has high purity and high yield, and is green, safe and environment-friendly. 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 batteries in which lithium ions are inserted and extracted for cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/24C07C305/26H01M10/0567H01M10/0525
CPCY02E60/10
Inventor 闫彩桥刘鹏侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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