Preparation methods for bis(fluorosulfonyl)imide and lithium bis(fluorosulfonyl)imide

A technology of lithium bisfluorosulfonimide and bisfluorosulfonimide, which is applied in the field of preparation of fluorine-containing compounds, can solve the problems of difficult control of reaction conditions, low yield, and many by-products, etc., so as to improve utilization rate and reduce Production cost and reduction of by-products

Inactive Publication Date: 2019-11-12
湖南福邦新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Aiming at the problems of many by-products, low yield and difficult control of reaction conditions in the existing preparation method of

Method used

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Examples

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preparation example Construction

[0043] The invention provides a kind of preparation method of bisfluorosulfonimide, comprising the following steps:

[0044] Mix hydrogen fluoride and liquid compound S to prepare S.nHF complex, wherein compound S is selected from liquid ammonia, N,N'-dimethylformamide, N,N'-dimethylacetamide, hexamethyl Phosphoramide, 1-methyl-2-pyrrolidone, tetramethylurea, N,N'-dimethylpropaneurea, 1,3-dimethyl-2-imidazolinone, 1,3-di-n-butyl One or more of base-2-imidazolinone, melamine, poly(vinylpyridine) and ester compounds; n is selected from 1 to 20, preferably 1 to 10;

[0045] Mix the S.nHF complex with bischlorosulfonimide to react to form a mixed solution containing bisfluorosulfonimide;

[0046] The mixture was distilled to collect difluorosulfonimide fractions.

[0047] The inventors have found that bisfluorosulfonimides are prone to decomposition reactions with some organic solvents (such as ethers) at high temperatures, thereby producing by-products and affecting the yield o...

Embodiment 1

[0088] This example is used to illustrate the preparation method of bisfluorosulfonimide disclosed in the present invention, including the following steps:

[0089] Preparation of HFSI from 1-methyl-2-pyrrolidone hydrofluoric acid complex

[0090] 1) Under nitrogen protection and stirring, add 85.1g of 1-methyl-2-pyrrolidone (1mol) to a dry 1L three-necked flask, stir and cool down to -20°C, then slowly add 185g of anhydrous hydrofluoric acid ( 9.23mol), make the complex solution of 1-methyl-2 pyrrolidone.HF, be denoted as NMP.nHF, be warming up to room temperature and isolate air preservation then;

[0091] 2) Add 270.1g of NMP.nHF (containing 1mol 1-methyl-2-pyrrolidone, 9.23mol HF) to a dry three-necked flask under nitrogen protection, start stirring, raise the temperature to 45°C, and then pass through the constant pressure dropping funnel Add 112g of HClSI (0.5mol) dropwise, control the drop rate, keep the temperature in the system at 45°C±5°C, raise the temperature to 1...

Embodiment 2

[0093] This example is used to illustrate the preparation method of bisfluorosulfonimide disclosed in the present invention, including the following steps:

[0094] Preparation of HFSI from N,N'-Dimethylformamide Hydrofluoric Acid Complex

[0095] 1) Under nitrogen protection and stirring, add 73.9g of N,N'dimethylformamide (1mol) to a dry 1L three-necked flask, stir and cool down to -60°C, then slowly add 100g of anhydrous hydrofluoric acid (5mol) to make a complex solution of N,N'-dimethylformamide.HF, which is denoted as DMF.nHF, and then warmed up to room temperature and stored in isolation from air;

[0096] 2) Add 347.8g of DMF.nHF (containing 2mol N,N'-dimethylformamide, 10mol HF) to a dry three-neck flask under nitrogen protection, start stirring, raise the temperature to 45°C, and then drop the liquid through constant pressure Add 224g of HClSI (1mol) dropwise into the funnel, control the rate of addition, and keep the temperature in the system at 45°C±5°C. After the...

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Abstract

In order to overcome the problems of a plurality of by-products, low yield and difficulty in controlling of reaction conditions for a conventional preparation method of bis(fluorosulfonyl)imide, the invention provides a preparation method for the bis(fluorosulfonyl)imide. The preparation method comprises the following operation steps: preparing an S.nHF complex, wherein a compound S is one or moreselected from the group consisting of liquid ammonia, N,N'-dimethylformamide, N,N'-dimethylacetamide, hexamethylphosphoramide, 1-methyl-2-pyrrolidone, tetramethylurea, N,N'-dimethylpropylurea, 1,3-dimethyl-2-imidazolinone, 1,3-di-n-butyl-2-imidazolinone, melamine, poly(vinylpyridine) and an ester compound; and mixing the S.nHF complex with bis(chlorosulfonyl)imide, and collecting a fraction of the bis(fluorosulfonyl)imide. Meanwhile, the invention also discloses a preparation method for lithium bis(fluorosulfonyl)imide. The preparation method for the bis(fluorosulfonyl)imide provided by the invention can effectively reduce generation of by-products, and improves the yield of the bis(fluorosulfonyl)imide.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing compounds, and in particular relates to a preparation method of bisfluorosulfonimide and lithium bisfluorosulfonimide. Background technique [0002] LiFSI is a key high-performance electrolyte material in new energy devices such as lithium-ion batteries and supercapacitors, and has high industrial application value. [0003] The existing LiFSI synthesis method is to prepare LiFSI by directly reacting HClSI with lithium fluoride LiF, as described in the patent US2004097757, this preparation method will produce a large amount of corrosive gas hydrogen fluoride, and at the same time, it is difficult to completely separate the excess LiF from LiFSI , thereby affecting the quality of the product. [0004] Most of the existing synthetic methods of LiFSI are to synthesize bischlorosulfonimide HClSI first, and then combine it with fluorinated metal salt MF x reaction to prepar...

Claims

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Application Information

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IPC IPC(8): C01B21/093C01B21/086
CPCC01B21/086C01B21/093C01P2006/80C01P2006/82
Inventor 刘振国曾爱国曾赐林谭连芳喻京鼎朱海春任明月曾翼
Owner 湖南福邦新材料有限公司
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