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Preparation method and purification process of fluorine-containing lithium sulfimide

A lithium sulfonyl imide and process technology, which is applied in the field of preparation of fluorine-containing lithium sulfonyl imide, can solve problems such as low product yield, potential safety hazards, and cumbersome preparation methods

Active Publication Date: 2020-08-28
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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  • Preparation method and purification process of fluorine-containing lithium sulfimide
  • Preparation method and purification process of fluorine-containing lithium sulfimide
  • Preparation method and purification process of fluorine-containing lithium sulfimide

Examples

Experimental program
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Effect test

Embodiment 1

[0066] The preparation method and purification process of lithium bistrifluoromethanesulfonyl imide comprise the following steps:

[0067] (1) Preparation process one:

[0068] Under stirring condition, add 100g nitrogen-containing substance trifluoromethanesulfonyl chloride, isopropanol, reaction solvent toluene in 1L dry reactor, the molar ratio of sulfur-containing substance trifluoromethanesulfinyl chloride, isopropanol respectively The ratio 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 was completed, the temperature was lowered to normal temperature, the insoluble matter was filtered off, the filtrate was evaporated under reduced pressure to remove the solvent, concentrated, and the crude compound II was prepared;

[0069] (2) Preparation process two:

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

Embodiment 2

[0078] The preparation method and purification process of lithium bisfluorosulfonyl imide comprise the following steps:

[0079] (1) Preparation process one:

[0080] Under stirring condition, add 100g nitrogen-containing substance trifluoromethanesulfonyl chloride, isopropanol, reaction solvent toluene in 1L dry reactor, the molar ratio of sulfur-containing substance trifluoromethanesulfinyl chloride, isopropanol respectively The ratio 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 was completed, it was lowered to normal temperature. The insolubles were removed by filtration, the filtrate was evaporated under reduced pressure to remove the solvent, concentrated, and the crude compound II was prepared;

[0081] (3) Preparation process two:

[0082] Under stirring conditions, add 100 g of compound II and toluene as a reaction solvent to a 1 L dry reactor, add the oxidizing substanc...

Embodiment 3

[0090] Preparation and Purification Process of Lithium Bisperfluoroethylsulfonylimide

[0091] (1) Preparation process one:

[0092] Under stirring conditions, add 100g of nitrogen-containing substance perfluoroethylsulfinyl chloride, isopropanol, and reaction solvent toluene to a 1L dry reactor, and the molar ratios of sulfur-containing substance perfluoroethylsulfinyl chloride and butyl acetate are respectively The ratio 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 was completed, the temperature was lowered to normal temperature, the insoluble matter was filtered off, the filtrate was evaporated under reduced pressure to remove the solvent, concentrated, and the crude compound II was prepared;

[0093] (2) Preparation process two:

[0094] Under stirring conditions, add 100 g of compound II and butyl acetate as a reaction solvent into a 1 L dry reactor, and add the fluorine-contain...

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Abstract

The invention discloses a preparation method and a purification process of fluorine-containing lithium sulfimide, and belongs to the technical field of lithium ion battery electrolytes. The preparation process is divided into three steps: (1) a first preparation step: reacting a nitrogen-containing reagent with at least one of a sulfur-containing reagent and a Y-containing reagent to obtain a compound II; and (2) a second preparation step: reacting the compound II with at least one of an oxidation reagent, a lithium-containing reagent and a fluorine-containing reagent to obtain a compound I, namely fluorine-containing lithium sulfimide. Finally, the prepared fluorine-containing lithium sulfimide crude product is subjected to the purification process to obtain a high-purity fluorine-containing lithium sulfimide refined product, and the prepared fluorine-containing lithium sulfimide can be used as an electrolyte lithium salt and an electrolyte additive of a lithium ion battery.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery electrolytes, and in particular relates to a preparation method and a purification process of fluorine-containing lithium sulfonylimide. Background technique [0002] In recent years, compared with other types of secondary batteries, lithium-ion batteries have advantages such as large specific energy, high voltage, environmental protection and no memory effect, so lithium-ion batteries have become more and more widely used in applications such as energy storage, electronic , military industry and power and other fields. In the composition and structure of lithium-ion batteries, the non-aqueous electrolyte is a key component that affects the performance of lithium-ion batteries. The electrolyte is the link connecting the positive and negative electrode materials of lithium-ion batteries, and plays a role in the transmission of lithium ions in lithium-ion batteries. effect. [0003] At...

Claims

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Application Information

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Patent Type & Authority Applications(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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