Preparation method for bis-fluorosulfonyl imide compound

A technology of bisfluorosulfonimides and compounds, which is applied in the field of preparation of bisfluorosulfonimides, can solve the problems of unfavorable wide application, high purification cost, and large passivation film resistance, and achieve the requirements of undemanding operating equipment, Easy separation and purification, the effect of simple steps

Inactive Publication Date: 2018-12-11
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, pyridineboronic acid pinacol esters and phenylboronic acid pinacol esters are difficult to synthesize, the cost of purification is high, and they are not widely used.
The passivation film formed by the nitrile electrolyte additive has a large resistance, which is not conducive to the battery rate and low temperature discharge

Method used

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  • Preparation method for bis-fluorosulfonyl imide compound

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[0021] A preparation method of bisfluorosulfonyl imides, the preparation method comprising the following steps:

[0022] (1) the FSO 2 X, nitrogen source, acid-binding agent and aprotic solvent are mixed to obtain a mixture; wherein, the nitrogen source is a primary amine, and the acid-binding agent is an aprotic organic amine; the acid-binding agent and FSO 2 The molar ratio of X is 1:2~5; the molar ratio of nitrogen source and acid-binding agent is 1:3~8; the X is F or C n f 2n+1 , n=1-5;

[0023] (2) Heat the mixture to reflux and react for 12h to 72h;

[0024] (3) After the reflux reaction is finished, cool down, release the pressure, spin dry the solvent, add water to wash and filter, and obtain the crude product;

[0025] (4) Recrystallize the crude product to obtain finished products of bisfluorosulfonimide compounds.

[0026] The acid-binding agent is at least one of triethylamine, tetramethylethylenediamine and tetramethyl-1,3-propylenediamine.

[0027] The apro...

Embodiment 1

[0037] (1) Add 200g acetonitrile and 150.2g triethylamine in 1L autoclave, add 45.9g aniline, slowly add 100g sulfuryl fluoride (F 2 SO 2 ) mixed to obtain a mixture; aniline, F 2 SO 2 The molar ratio to triethylamine is 1:2:3; heat the autoclave to 80°C, and continue to stir and reflux for 36 hours; then cool to normal temperature, wash and extract to obtain the filtrate; use a rotary evaporator to remove the The solvent was distilled off to obtain a crude product, which was put into an oven to heat and vacuum-dry to obtain the final product, weighing 110 g, with a yield of 87%.

[0038] (2) The final product can be further purified to obtain bisfluorosulfonimide compounds with a purity greater than 99%. The specific steps are as follows: 110 g of the final product is stirred and dissolved with 220 g of methanol, allowed to stand at -24°C for 24 hours, and filtered , the obtained solid precipitate was put into an oven for vacuum drying to obtain purified N-phenylbisfluoros...

Embodiment 2

[0042] (1) Add 300g dichloromethane and 145.2g tetramethylethylenediamine in 1L autoclave, add 40g 2-aminopyridine, slowly add 85g sulfonyl fluoride (F 2 SO 2 ) mixed to obtain a mixture; 2-aminopyridine, F 2 SO2 The molar ratio to tetramethylethylenediamine is 1:2:3; heat the autoclave, raise the temperature to 40°C, and continue to stir and reflux for 36 hours; then cool to normal temperature, wash and extract to obtain the filtrate; use a rotary evaporator to The solvent in the filtrate was distilled off to obtain a crude product, which was put into an oven, heated and dried under vacuum to obtain the final product, weighing 96 g, with a yield of 89%.

[0043] (2) The final product can be further purified to obtain a bisfluorosulfonimide compound with a purity greater than 99%. The specific steps are as follows: stir and dissolve the final product with 192 g of methanol and 96 g of the final product, stand at -24°C for 36 hours, and filter. The obtained solid precipitate ...

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Abstract

The invention discloses a preparation method for a bis-fluorosulfonyl imide compound. The preparation method comprises the following steps that (1) FSO2X, a nitrogen source, an acid-binding agent andan aprotic solvent are mixed so as to obtain a mixture; (2) heating is carried out to enable the mixture to be subjected to reflux reaction, and reaction is continuously carried out for 12-72 hours; (3) after the reflux reaction is ended, cooling is carried out, the pressure is released, the solvent is dried in a spun mode, water is added for washing, and filtering is carried out so as to obtain acrude product; and (4) the crude product is recrystallized so as to obtain a finished product of the bis-fluorosulfonyl imide compound. The preparation method for the bis-fluorosulfonyl imide compound has the advantages that raw materials are easy to obtain, the steps are simple, the risk is avoided, and pollution is avoided; the yield is high, separation and purification are easy; and the requirement for operating equipment is not rigorous, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of preparation of bisfluorosulfonimides, in particular to a preparation method of bisfluorosulfonimide compounds. Background technique [0002] Lithium secondary batteries have the advantages of high storage energy density, long service life, environmental protection, high and low temperature adaptability, etc., and are widely used in electronic products, electric vehicles, aerospace, energy storage and other fields. However, with the widespread application of lithium secondary batteries, higher requirements are put forward for their cycle performance, energy density, high and low temperature adaptability, and rate performance. [0003] Electrolyte additives are an important part of lithium secondary batteries. Excellent electrolyte additives have a positive electrochemical effect in lithium secondary batteries, which can improve the kinetic characteristics of the battery, thereby significantly improving the overall p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086H01M10/0567
CPCC01B21/086H01M10/0567Y02E60/10
Inventor 赵经纬许磊信勇孙安乐
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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