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A preparation method and purification process of lithium fluorine-containing sulfonylimide

A lithium sulfonyl imide and process technology, which is applied in the field of preparation of fluorine-containing lithium sulfonyl imide, can solve the problems of cumbersome preparation methods, low product yield, and high product impurities, and achieve low raw material cost, high purity, and low cost. low effect

Active Publication Date: 2021-10-26
苏州固锂新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection yield of the prepared product is about 80%. The lithium metal, lithium hydride or lithium ammonia hydride used in the preparation method are all extremely active metal compounds, and there is a possibility of uncontrolled explosion during the reaction process, and the generated Hydrogen is a flammable and explosive gas, which brings huge safety hazards to production
[0007] In order to prepare lithium fluorine-containing sulfonyl imides with higher purity and yield, researchers have conducted a lot of research. The current preparation process of lithium fluorine-containing sulfonyl imides still has cumbersome preparation methods, low product yields, and The shortcomings such as high impurity, therefore, need to provide a kind of production method badly, the preparation method of the fluorine-containing sulfonylimide lithium that product purity is high

Method used

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  • A preparation method and purification process of lithium fluorine-containing sulfonylimide
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  • A preparation method and purification process of lithium fluorine-containing sulfonylimide

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Effect test

Embodiment 1

[0066] The preparation method and purification process of lithium bistrifluoromethanesulfonimide, comprising the following steps:

[0067] (1) Preparation process one:

[0068] Under stirring conditions, 100 g of nitrogen-containing substance trifluoromethylsulfonyl chloride, isopropanol, and reaction solvent toluene were added to a 1L dry reactor, and the molar ratios of sulfur-containing substance trifluoromethylsulfinyl chloride and isopropanol were respectively is 2.5:1, the reaction temperature is 70°C, the reaction pressure is 0.1MPa (gauge pressure), and the reaction time is 4h. After the reaction is completed, it is lowered to normal temperature, the insolubles are filtered off, the filtrate is evaporated under reduced pressure to remove the solvent, and concentrated to prepare a crude product of compound II;

[0069] (2) preparation process two:

[0070] Under stirring conditions, 100 g of compound II and reaction solvent toluene were added to a 1L dry reactor, and ...

Embodiment 2

[0078] The preparation method and purification process of lithium bisfluorosulfonimide, comprising the following steps:

[0079] (1) Preparation process one:

[0080] Under stirring conditions, 100 g of nitrogen-containing substance trifluoromethylsulfonyl chloride, isopropanol, and reaction solvent toluene were added to a 1L dry reactor, and the molar ratios of sulfur-containing substance trifluoromethylsulfinyl chloride and isopropanol were respectively is 2.5:1, the reaction temperature is 70°C, the reaction pressure is 0.1MPa (gauge pressure), and the reaction time is 4h. After the completion of the reaction, the temperature was lowered to normal temperature. The insolubles were removed by filtration, the filtrate was evaporated under reduced pressure to remove the solvent, and concentrated to obtain the crude product of compound II;

[0081] (3) preparation process two:

[0082] Under stirring conditions, 100 g of compound II and reaction solvent toluene were added to ...

Embodiment 3

[0090] Preparation and purification process of lithium bis(perfluoroethylsulfonyl)imide

[0091] (1) Preparation process one:

[0092] Under stirring conditions, 100 g of nitrogen-containing substances perfluoroethylsulfonyl chloride, isopropanol, and reaction solvent toluene were added to a 1L dry reactor, and the molar ratios of sulfur-containing substances perfluoroethylsulfinyl chloride and butyl acetate were respectively is 3:1, the reaction temperature is 80°C, the reaction pressure is 0MPa (gauge pressure), and the reaction time is 6h. After the reaction is completed, it is lowered to normal temperature, the insolubles are filtered off, the filtrate is evaporated under reduced pressure to remove the solvent, and concentrated to prepare a crude product of compound II;

[0093] (2) preparation process two:

[0094] Under stirring conditions, 100 g of compound II and butyl acetate as the reaction solvent were added to a 1L dry reactor, and the fluorine-containing reagent...

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Abstract

The invention discloses a preparation method and a purification process of lithium fluorine-containing sulfonylimide, belonging to the technical field of lithium ion battery electrolyte. Among them, the preparation process is divided into three steps: (1) Preparation step 1: reacting nitrogen-containing reagent with at least one of sulfur-containing reagent and Y-containing reagent to obtain compound II; (2) Preparation step 2: making compound II React with at least one of oxidizing reagents, lithium-containing reagents, and fluorine-containing reagents to obtain compound I, which is lithium fluorine-containing sulfonylimide. Finally, the prepared crude fluorine-containing sulfonyl imide lithium is purified through a purification process to obtain high-purity fluorine-containing lithium sulfonyl imide. The prepared fluorine-containing lithium sulfonyl imide can be used for electrolyte lithium salt, electrolysis liquid additives.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolyte, and in particular relates to a preparation method and purification process of fluorine-containing lithium sulfonimide. Background technique [0002] In recent years, due to the advantages of lithium-ion batteries compared with other types of secondary batteries, such as large specific energy, high voltage, environmental protection and no memory effect, lithium-ion batteries have become more and more widely used, such as energy storage, electronic , military and power industries. In the composition structure of lithium-ion batteries, non-aqueous electrolyte is a key component that affects the performance of lithium-ion batteries. effect. [0003] At present, there are many types of lithium ion electrolytes, among which the main ones are formed by dissolving electrolyte salts in organic solvents, but the performance of conventional electrolytes is limited and generally can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/086C01B21/096
CPCC01B21/086C01B21/096C01P2002/86C01P2002/87C01P2002/89C01P2006/80C01P2006/82
Inventor 蒋玉贵
Owner 苏州固锂新能源科技有限公司
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