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Preparation method of difluoro-sulfonyl imine salt

The technology of a bisfluorosulfonimide salt and a purification method is applied in the field of preparation of the bisfluorosulfonimide salt, which can solve the problems of unobtainable reaction raw materials, low purity, difficulty in separation and purification, etc., and meets the requirements of operation and equipment The conditions are not harsh, the reaction steps are simple, and the effect of separation and purification is easy

Active Publication Date: 2015-04-01
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] In summary, in the prior art, the reports related to the preparation of bisfluorosulfonimide salts mainly have the following defects: the reaction raw materials are not easy to obtain, dangerous, pollute the environment, such as strong corrosion, strong oxidation, poisonous, etc. ; The yield of the reaction product is low, the purity is not high, the separation and purification are difficult, and it is difficult to meet the high purity requirements of the electrolyte material; the reaction steps are many, the operating conditions are harsh, and the equipment requirements are high, so it is not suitable for industrial production

Method used

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  • Preparation method of difluoro-sulfonyl imine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Add 383g of acetonitrile and 130g of lithium carbonate to a 2L autoclave, cool the autoclave to -34°C after mixing, add 10g of anhydrous liquid NH 3 , slowly add 100g sulfuryl fluoride (F 2 SO 2 ) mixed to obtain a mixture; NH 3 , F 2 SO 2 The mol ratio with lithium carbonate is 1:2:3;

[0058] Heat the autoclave to 120°C, and continue to stir and reflux for 72 hours;

[0059] Cool to normal temperature then, filter to obtain filtrate;

[0060] The solvent in the filtrate was evaporated and removed with a rotary evaporator to obtain a crude product. The crude product was put into an oven to be heated and vacuum-dried to obtain the final product. The final product was tested by Raman spectroscopy. The test conditions were: light source Nd:YAG ( λ=1064nm), the measured Raman spectrum is as follows figure 1 As shown, it is proved that the final product obtained is lithium bisfluorosulfonyl imide (LiN(SO 2 f) 2 ), heavy 98g, productive rate 89%.

[0061] The final...

Embodiment 2

[0064] Add 1000g of acetone and 420g of sodium bicarbonate to a 5L autoclave, cool the autoclave to -100°C after mixing, add 10g of anhydrous gaseous NH 3 , while stirring, slowly add 580g chlorosulfuryl fluoride (FSO 2 Cl) mixed to obtain a mixture; NH 3 、FSO 2 The molar ratio of Cl to sodium bicarbonate is 1:10:10;

[0065] Heat the autoclave to -50°C, and continue to stir and reflux for 48 hours;

[0066] Place to normal temperature then, filter to obtain filtrate;

[0067] The solvent in the filtrate was evaporated and removed with a rotary evaporator to obtain a crude product. The crude product was put into an oven to be heated and vacuum-dried to obtain the final product. The final product was tested by Raman spectroscopy. The test conditions were: light source Nd:YAG ( λ=1064nm), the measured Raman spectrum is as follows figure 1 As shown, it is proved that the final product obtained is sodium bisfluorosulfonyl imide (NaN(SO 2 f) 2 ), weighs 250.5g, and the yield...

Embodiment 3

[0069] Add 500g methylene chloride and 4245g potassium phosphate in 10L autoclave, after mixing, add 53.5g ammonium chloride, slowly add 152g bromosulfuryl fluoride (FSO 2 Br) mixed to obtain a mixture; ammonium chloride, FSO 2 The molar ratio of Br to potassium phosphate is 1:2:10;

[0070] Heat the autoclave to 50°C, and continue to stir and reflux for 5 hours;

[0071] Then cool and filter to normal temperature, filter to obtain the filtrate;

[0072] The solvent in the filtrate was evaporated and removed with a rotary evaporator to obtain a crude product. The crude product was put into an oven to be heated and vacuum-dried to obtain the final product. The final product was tested by Raman spectroscopy. The test conditions were: light source Nd:YAG ( λ=1064nm), the measured Raman spectrum is as follows figure 1 As shown, it is proved that the final product obtained is potassium bisfluorosulfonyl imide (KN(SO 2 f) 2 ), weighs 174.5g, and the yield is 86%.

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Abstract

The invention relates to a preparation method of a difluoro-sulfonyl imine salt, and belongs to the field of fine chemical engineering. The difluoro-sulfonyl imine salt is MN(SO2F)2, wherein M is Li, Na, K, Rb or Cs. The preparation method comprises the following steps: mixing FSO2X, a nitrogen source, an acid-binding agent and an aprotic solvent to obtain a mixture, wherein X is F, Cl, Br or I, the nitrogen source is anammonium salt or anhydrous NH3, the acid-binding agent is a lithium, sodium, potassium, rubidium or cesium salt, the mole ratio of NH3 or ammonium ion to FSO2X is 1:(2-10), and the mole ratio of NH3 or the ammonium ion to the acid-binding agent is 1:(3-10); heating to perform reflux reaction on the mixture for 5-8 hours; cooling to obtain a filtrate; and removing the solvent to obtain a crude product, and performing vacuum drying to obtain the difluoro-sulfonyl imine salt. The preparation method has easily available raw material, is safe and pollution-free, is high in yield, is easy to realize separation and purification, is simple in step, is not severe in requirement of operation equipment, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of bisfluorosulfonimide salt, specifically, relate to a kind of molecular formula MN(SO 2 f) 2 The preparation method of bisfluorosulfonimide salt, wherein, the M is lithium (Li), sodium (Na), potassium (K), rubidium (Rb) or cesium (Cs); belongs to the fine chemical industry field. Background technique [0002] Bisfluorosulfonyl imide salts, especially lithium bisfluorosulfonimide salts, due to their large anion structure, fluoride ions have strong electric absorption, which makes their binding force with cations very weak, making them in molten state or organic Lithium ions are highly dissociated in the presence of a solvent and can be used as a lithium electrolyte in lithium secondary batteries; at the same time, due to its excellent electrical conductivity, it can be used in supercapacitors and aluminum electrolytic capacitors; it can also be used as a Lewis acid catalyst. It has import...

Claims

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Application Information

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IPC IPC(8): C01B21/096
Inventor 彭立培刘智慧杨献奎宋富财郭绪涛冀延治董云海
Owner PERIC SPECIAL GASES CO LTD
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