Preparation method of bis(fluorosulfonyl)imine alkali metal salt

A technology of imine bases and metal salts, applied in the direction of nitrogen and non-metallic compounds, nitrosyl chloride, etc., can solve problems such as increased difficulty, poor effect of ionic liquids, harsh reaction conditions, etc., to improve quality and performance, and production costs Inexpensive and mild reaction conditions

Active Publication Date: 2018-07-13
LEE & MAN CHEM CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Use this method to synthesize MFSI process is loaded down with trivial details, the fluorinating agent SbF that adopts 3 、BiF 3 etc. are more expensive and highly toxic, and ZnF is used 2 A large amount of amine-containing wastewater will be produced in the later stage, and the use of HF is more dangerous, and the high toxicity and high corrosiveness make the reaction more difficult.
Using this method to obtain MFSI raw materials is highly toxic and dangerous, consumes a lot, and also produces a lot of waste
[0007] Chinese patent (CN 105523530 A) has reported that KF is used as fluorinating agent to react with bis(chlorosulfonyl)imide in the presence of organic solvent, but KF has poor solubility in organic solvent in this reaction, so the reaction rate The efficiency of fluorination and fluorination is not good. If a good fluorination effect is to be achieved, the reaction conditions will be very harsh
First of all, the cost of crown ether is relatively high, and it consumes a lot for industrial production
Secondly, the crown ether is extremely difficult to remove because the oxygen on the crown ether has a strong ability to coordinate with Li ions
Again, the complexes formed by crown ethers and other metal ions are easy to introduce metal ions into LiFSI and not easy to remove, which will affect the application effect of LiFSI in batteries
[0009] Chinese patent (CN 105731398 A) has reported that in a polar aprotic solvent, an alkali metal fluoride is used as a fluorinating agent, and an ionic liquid is used as a phase transfer catalyst to catalyze the reaction, but the ionic liquid is expensive, although the patent says It can be recycled, which is theoretically feasible, but the actual operation is difficult, and the effect of the recovered ionic liquid is not as good as before

Method used

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  • Preparation method of bis(fluorosulfonyl)imine alkali metal salt

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The synthesis of potassium bis(fluorosulfonyl)imide (KFSI) is as follows:

[0029]

[0030] Under nitrogen protection, KClSI (125.5 g, 0.5 mol), CH 3 COOH (60mL), after stirring at room temperature for 0.5h, KF (58g, 1mol) was added, and after reacting at room temperature for 20h, the protic solvent was evaporated with a rotary evaporator for recycling. Then add 120 mL of organic solvent ethyl acetate to filter the insoluble matter, collect the filtrate to concentrate and recover the solvent, then add 100 mL of ethanol to the concentrated solution, heat and reflux for 2 hours, filter a small amount of insoluble matter while it is hot, concentrate the filtrate, and then add dropwise the poor organic solvent dichloro 80 mL of methane precipitated colorless crystals, then filtered and dried in vacuo to obtain 88 g of colorless crystals with a yield of 80% and a content of ≥99%.

Embodiment 2

[0032] The synthesis of bis(fluorosulfonyl)imide sodium (NaFSI) is as follows:

[0033]

[0034] Under nitrogen protection, NaClSI (116.5 g, 0.5 mol) and HCOOH (20 mL) were successively added to a 500 mL three-neck flask equipped with a stirrer, and NaF (42 g, 1 mol) was added after stirring at room temperature for 0.5 h under stirring, and then After reacting at room temperature for 18 h, the protic solvent was evaporated with a rotary evaporator for recycling. Then add 120mL of organic solvent dimethyl carbonate to filter the insoluble matter, collect the filtrate to concentrate and recover the solvent, then add 100mL of methanol to the concentrated solution, heat and reflux for 2h, filter a small amount of insoluble matter while it is hot, concentrate the filtrate, and then add the poor organic solvent ring Hexane 80mL, colorless crystals were precipitated, filtered, and vacuum-dried to obtain 76g of colorless crystals, yield 76%, content ≥ 99%.

Embodiment 3

[0036] The synthesis of lithium bis(fluorosulfonyl)imide (LiFSI) is as follows:

[0037]

[0038] Under nitrogen protection, LiClSI (109.5 g, 0.5 mol), CH 3COOH (60mL), under stirring, stirred at room temperature for 0.5h, then added LiF (26g, 1mol), then reacted at room temperature for 24h, and evaporated the protic solvent with a rotary evaporator for recycling. Then add 120 mL of organic solvent acetonitrile to filter the insoluble matter, collect the filtrate to concentrate and recover the solvent, then add 100 mL of ethanol to the concentrated liquid, heat to reflux for 2 hours, filter a small amount of insoluble matter while it is hot, concentrate the filtrate, and then add dropwise 80 mL of poor organic solvent dichloromethane , colorless crystals were precipitated, filtered, and vacuum-dried to obtain 70 g of colorless crystals with a yield of 75% and a content of ≥99%.

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Abstract

The invention discloses a preparation method of bis(fluorosulfonyl)imine alkali metal salt. The preparation method takes bis(chlorosulfonyl)imine alkali metal salt (M1ClSI) as a raw material and alkali metal fluoride (M2F) as a fluorinating agent and comprises the following steps: taking the raw material and the fluorinating agent to be subjected to fluorinating reaction in a weak acidic proton solvent; after reaction, extracting an obtained bis(fluorosulfonyl)imine alkali metal salt crude product; filtering, concentrating, crystallizing and drying to obtain a target product bis(fluorosulfonyl)imine alkali metal salt, wherein M1 in the M1ClSI represents an alkaline metal element and M2 in the M2F represents an alkaline metal element; the pKa of the weak acidic proton solvent is 3 to 10. The preparation method provided by the invention has the characteristics of moderate reaction conditions, high product yield, high purity, low raw material cost, simple technology and easiness for realizing industrialized preparation.

Description

technical field [0001] The invention relates to a preparation method of bis(fluorosulfonyl)imide alkali metal salt, belonging to the technical field of chemical synthesis. Background technique [0002] The research on lithium-ion batteries has developed rapidly in recent decades when energy resources are increasingly scarce. Lithium hexafluorophosphate (LiPF 6 ) and lithium bis(fluorosulfonyl)imide (LiTFSI), but the thermal stability and chemical stability of the first two are poor, so lithium bis(fluorosulfonyl)imide (LiFSI) came into being, its thermal High stability, no decomposition below 200°C, and good chemical stability. Therefore, LiFSI has become the latest and hottest direction of lithium battery electrolyte research. [0003] The bis(fluorosulfonyl)imide alkali metal salt studied in the present invention is an important raw material for preparing lithium bis(fluorosulfonyl)imide. [0004] The chemical structural formula of bis(fluorosulfonyl)imide alkali metal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086
Inventor 苏秋铭张梦辛伟贤谢文健陈新滋
Owner LEE & MAN CHEM CO LTD
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