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Preparation method for pyridine ring sulfimide alkali metal salt

A technology of pyridine ring sulfonimide base and pyridine ring sulfonyl chloride is applied in the field of preparation of pyridine ring sulfonimide alkali metal salt, which can solve the problems of difficult separation and purification of products, complicated steps and the like, and achieves high yield and purity , the operation steps are short, the effect of easy separation and purification

Inactive Publication Date: 2017-06-13
HUIZHOU DADO NEW MATERIAL TECH CO LTD
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  • Abstract
  • Description
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Problems solved by technology

[0003] Fluorine-containing alkylsulfonylimides and their alkali metal salts, especially lithium salts, are important fluorine-containing ion compounds, and are used as high-performance non-aqueous electrolyte materials for clean energy devices such as lithium-ion batteries, supercapacitors, and aluminum electrolytic capacitors. , and new high-efficiency catalysts and other fields, all have important industrial application value, but there are still certain defects in the preparation process of pyridine cyclic sulfonimide alkali metal salts, such as cumbersome steps, difficult separation and purification of products, etc., which need to be further developed perfection

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  • Preparation method for pyridine ring sulfimide alkali metal salt
  • Preparation method for pyridine ring sulfimide alkali metal salt
  • Preparation method for pyridine ring sulfimide alkali metal salt

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preparation example Construction

[0028] This embodiment provides a method for preparing alkali metal salt of pyridine cyclic sulfonimide, comprising the following steps:

[0029] (1) Under the protection of argon, mix pyridine ring sulfonyl chloride, sulfonamide, acid-binding agent and appropriate amount of organic solvent in the reaction flask under stirring conditions for reaction, the reaction temperature is -20 ~ 60 ℃, and the reaction time is 8-48h, forming an organic solution containing an imine compound, and removing the solid by-products generated in the organic solution after decompression and filtration;

[0030] (2) Under stirring conditions, the anhydrous alkali metal compound solid that will be 1.0 to 3 times the stoichiometric amount of the imine compound is added to the organic solution in step (1) in batches, and the reaction is continued for 5 to 20 hours. The insoluble matter was filtered off to obtain the crude product of alkali metal salt of pyridine cyclic sulfonylimide;

[0031] (3) sel...

Embodiment 1

[0050] The preparation of (2-pyridinesulfonyl) imide lithium, synthetic reaction route is as follows:

[0051] step one:

[0052]

[0053] Step two:

[0054]

[0055] Add 2-pyridinesulfonamide (79g, 0.5mol), 2-pyridinesulfonyl chloride (88.7g, 0.5mol), triethylamine (50.5g, 0.5mol), and 300mL acetonitrile into a 1000mL three-necked flask, stir magnetically, and react at room temperature After 12 hours, filter under reduced pressure to obtain a light brown solution.

[0056] Magnetic stirring, lithium carbonate (18.5g, 0.25mol) was added at room temperature, and after 10 hours of reaction, the insoluble matter was removed by filtration, and the organic solvent was removed by rotary evaporation to obtain a light yellow solid, which was recrystallized from acetonitrile / methylene chloride to obtain 130g white Solid product, 85% yield.

Embodiment 2

[0058] Preparation of Sodium (2-Pyridinesulfonyl)imide

[0059] step one:

[0060]

[0061] Step two:

[0062]

[0063] Add 2-pyridinesulfonamide (79g, 0.5mol), 2-pyridinesulfonyl chloride (88.7g, 0.5mol), triethylamine (50.5g, 0.5mol), and 300mL acetonitrile into a 1000mL three-necked flask, stir magnetically, and react at room temperature After 12 hours, filter under reduced pressure to obtain a light brown solution.

[0064] Magnetic stirring, sodium carbonate (26.5g, 0.25mol) was added at room temperature, and after 10 hours of reaction, the insoluble matter was removed by filtration, and the organic solvent was removed by rotary evaporation to obtain a light yellow solid, which was recrystallized from acetonitrile / methylene chloride to obtain 141g white Solid product, 88% yield.

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Abstract

The invention provides a preparation method for a pyridine ring sulfimide alkali metal salt. The method comprises the following steps: (1) under argon protection, mixing pyridine ring sulfonyl chloride, sulfamide, acid-binding agent and a defined amount of organic solvent under a stirring condition and reacting in a reaction flask, thereby forming an organic solution containing an imine compound; (2) under a stirring condition, adding the anhydrous alkali metal compound solid of which the chemical amount is 1.0-3 times of that of the imine compound in several times into the organic solution acquired in the step (1), thereby acquiring a crude product of the pyridine ring sulfimide alkali metal salt; and (3) selecting polarity and weak-polarity compound solvent for re-crystallizing, filtering, reducing pressure and drying, thereby acquiring a target product. The preparation method for the pyridine ring sulfimide alkali metal salt provided by the invention has the characteristics of simple operation steps, easiness in separation and purification of the products, ultrahigh product yield and ultrahigh purity and has important industrial application value.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a method for preparing an alkali metal salt of pyridine cyclic sulfonylimide. Background technique [0002] LiPF 6 Poor thermal stability, easy to hydrolyze, use LiPF 6 When the lithium-ion battery works at high temperature (>55°C), the cycle performance and service life are greatly reduced. While other common lithium salts, such as lithium perchlorate (LiClO 4 ), lithium tetrafluoroborate (LiBF 4 ), lithium trifluoromethanesulfonate (Li[CF 3 SO 3 ]), lithium bis(trifluoromethylsulfonyl)imide (LiTFSI), lithium bisoxalate borate (LiBOB), etc., due to different performance defects, these lithium salts have not been widely used in lithium-ion batteries. use. Therefore, the research and development of new conductive lithium salt electrolyte materials with good chemical stability and excellent electrochemical performance to replace LiPF6 is an important research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12C07D213/71
CPCC07D213/71C07D401/12
Inventor 韩鸿波罗乾巩梦洁
Owner HUIZHOU DADO NEW MATERIAL TECH CO LTD