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Synthesis method of bis [(trifluoromethyl) sulfonyl] methane

A technology of trifluoromethyl and sodium trifluoromethyl sulfinate is applied in the field of synthesis of bis[sulfonyl]methane and achieves the effects of simple preparation method, stable preparation process and high yield

Pending Publication Date: 2020-06-30
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The existing measures to solve the battery performance and the above-mentioned problems are mainly to add additives to the battery electrolyte. At present, the unified cognition is that the purity of the additive determines its effect. Therefore, preparing high-purity additives and adding them to the battery electrolyte Adding high-purity additives is a common measure to solve battery problems at present, but more and more studies have found that not only the purity of additives has a very important impact on improving battery performance, but when the purity reaches the required level, increasing the purity has even greater impact. Micro, the R&D personnel of Shijiazhuang Shengtai Chemical Co., Ltd. have found through long-term exploration that the acid value and moisture of the added additives also have a very important impact on improving the effect and function of the battery. At present, the high acid value and moisture content are restricting additives. The main reason for the effect

Method used

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  • Synthesis method of bis [(trifluoromethyl) sulfonyl] methane
  • Synthesis method of bis [(trifluoromethyl) sulfonyl] methane
  • Synthesis method of bis [(trifluoromethyl) sulfonyl] methane

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Experimental program
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Effect test

Embodiment 1

[0018] Feed an inert gas into the reactor, add 0.1mol sodium trifluoromethylsulfinate, 0.15mol methylmagnesium bromide and 0.01mol tetrabutylammonium iodide to 500mL propionitrile to obtain a mixed solution, and stir The mixed solution was heated under reflux for 8 hours, and then the reaction solution was cooled to room temperature. After filtering, diethyl ether was added, and one 24-mesh silica gel particle, one 18-mesh silica gel particle and one 14-mesh silica gel particle were added thereto. At 20°C, add 0.22mol tert-butyllithium and 0.11mol trifluoromethanesulfonic anhydride, stir for 20 minutes, pass inert gas, then raise the temperature to 30°C and continue stirring for 20 minutes, after washing, drying, filtering, and concentration, bis [(Trifluoromethyl)sulfonyl]methane, the yield is 93%, and the density of the product detected is 1.83g / cm 3 , boiling point 300°C (760mmHg), purity 99.6%, water content 18ppm, acid value 26ppm.

Embodiment 2

[0020] Feed an inert gas into the reactor, add 0.1mol sodium trifluoromethyl sulfinate, 0.2mol methylmagnesium bromide and 0.02mol tetrabutylammonium iodide to 600mL propionitrile to obtain a mixed solution, under stirring conditions The mixed solution was heated under reflux for 12 hours, and then the reaction solution was cooled to room temperature. After filtering, ether was added, and 1 24-mesh silica gel particle, 18-mesh silica gel particle and 14-mesh silica gel particle were added thereto. At 40°C, add 0.25mol tert-butyllithium and 0.13mol trifluoromethanesulfonic anhydride, stir for 30min, pass inert gas, then raise the temperature to 40°C and continue stirring for 30min, after washing, drying, filtering and concentrating, the bis [(Trifluoromethyl)sulfonyl]methane, the yield is 94%, and the density of the detected product is 1.828g / cm 3 , boiling point 300.3°C (760mmHg), purity 99.7%, water content 15ppm, acid value 24ppm.

Embodiment 3

[0022] Inert gas is passed into the reactor, 0.1mol sodium trifluoromethyl sulfinate, 0.17mol methylmagnesium bromide and 0.017mol tetrabutylammonium iodide are added in 600mL propionitrile to obtain a mixed solution, under stirring conditions The mixed solution was heated under reflux for 10 h, then the reaction solution was cooled to room temperature, after filtration, ether was added, and one 24-mesh silica gel particle, one 18-mesh silica gel particle and one 14-mesh silica gel particle were added thereto, and then - At 25°C, add 0.23mol tert-butyllithium and 0.12mol trifluoromethanesulfonic anhydride, stir for 25min, pass inert gas, then raise the temperature to 35°C and continue stirring for 25min, after washing, drying, filtering, and concentration, bis [(Trifluoromethyl)sulfonyl]methane, the yield is 95%, and the density of the product detected is 1.832g / cm 3 , boiling point 300.6°C (760mmHg), purity 99.7%, moisture content 16ppm, acid value 25ppm.

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Abstract

The invention discloses a synthesis method of bis [(trifluoromethyl) sulfonyl] methane. The invention belongs to the technical field of battery electrolyte. The method comprises the following steps: adding sodium trifluoromethanesulfinate, methyl magnesium bromide and tetrabutylammonium iodide into an organic solvent to obtain a mixed solution; under the stirring condition, subjecting the mixed solution to heating reflux reaction for 8 to 12h; and cooling the reaction solution to room temperature, filtering, adding diethyl ether, adding tert-butyl lithium and trifluoromethanesulfonic anhydrideat -20 to -40 DEG C, stirring for 20-30 minutes, heating to 30-40 DEG C, continuing stirring for 20-30 minutes, washing, drying, filtering, and concentrating to obtain bis [(trifluoromethyl) sulfonyl] methane. The synthesis method is simple, and the obtained bis [(trifluoromethyl) sulfonyl] methane is high in yield, high in purity and low in moisture content.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte, and relates to a battery electrolyte additive bis[(trifluoromethyl)sulfonyl]methane, in particular to a synthesis method of bis[(trifluoromethyl)sulfonyl]methane. The synthesis method is simple, and the obtained bis[(trifluoromethyl)sulfonyl]methane has high yield, high purity and less moisture. Background technique [0002] As a new type of green high-energy battery, lithium-ion batteries are widely used in mobile phones, cameras, notebooks, etc. Portable devices such as computers. However, the charge-discharge cycle performance of the carbonate-based electrolyte of the existing lithium-ion battery is low, and the electrolyte is easily oxidized and decomposed on the surface of the positive electrode of the battery under high voltage, and the oxidative decomposition reaction of the electrolyte itself will also promote the morphology of the positive electrode material. Alteration, st...

Claims

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Application Information

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IPC IPC(8): C07C315/00C07C317/04H01M10/0567
CPCC07C315/00H01M10/0567C07C317/04Y02E60/10
Inventor 侯荣雪苗强强葛建民闫彩桥王军郝俊张民武利斌
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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