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Preparation method of bis(fluorosulfonyl)amine

A technology of bisfluorosulfonimide and ammonium fluoride, applied in the directions of nitrosyl chloride, nitrogen and non-metallic compounds, can solve the problems of high price of FSO3H, severe equipment corrosion, low yield, etc., and achieve easy separation, The effect of stable product quality and simple process

Active Publication Date: 2018-05-04
NANJING REDSUN BIOCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method uses the FSO 3 H is expensive, and it is very corrosive to equipment, and the yield of this method is not high, resulting in very high cost

Method used

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  • Preparation method of bis(fluorosulfonyl)amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 9g of NH to a 500mL autoclave 4 F (ACS grade), 100 g triethylamine and 210 g acetonitrile. Seal the reactor well and pump the reactor to a negative pressure of -0.1MPa (gauge pressure). With constant stirring, slowly introduce SO 2 f 2 The pressure of the gas to the reactor is 0.3MPa, and the reaction temperature is controlled at about 25°C. When the reaction pressure drops to 0.2MPa, continue to add sulfuryl fluoride to 0.3MPa, and cycle in turn until the pressure drops slowly or does not drop. Acyl fluoride no longer participated in the reaction, and the reaction was basically completed. The reaction was carried out for 20 hours in total, 60 g of sulfuryl fluoride was consumed, and 370 g of a light yellow transparent solution was obtained without solid residue. Acetonitrile and unreacted triethylamine were removed by rotary evaporation at 80°C and -0.08MPa (gauge pressure) conditions to obtain 145 g of dark yellow solution, then 30 g of concentrated sulfuric ac...

Embodiment 2

[0030] Add 9g of NH to a 500mL autoclave 4 F (ACS grade), 100 g triethylamine and 210 g acetonitrile. Seal the reactor well and pump the reactor to a negative pressure of -0.1MPa (gauge pressure). With constant stirring, slowly introduce SO 2 f 2 The gas keeps the pressure of the reactor at 0 MPa, the reaction temperature is kept at 25-28°C, the reaction is carried out for 24 hours, and 72g of SO is consumed 2 f 2 , 385 g of a light yellow transparent solution was obtained, and no solid remained. At 80 DEG C, under the condition of -0.08MPa (gauge pressure), rotary evaporation removes acetonitrile and unreacted triethylamine to obtain 138 g of dark yellow solution, then add 25 g of concentrated sulfuric acid (98% by mass), and the mixed solution is distilled under reduced pressure. 36.8g of HFSI product (purity 99.2%) was collected at 85°C / 650Pa as a colorless solution, which turned into white crystals after cooling with ice water, with a yield of 83.6%.

Embodiment 3

[0032] Add 9g of NH to a 500mL autoclave 4 F (ACS grade), 100 g triethylamine and 210 g acetonitrile. Seal the reactor well and pump the reactor to a negative pressure of -0.1MPa (gauge pressure). With constant stirring, slowly introduce SO 2 f 2 The pressure of the gas to the reactor is 0.6MPa, and the reaction temperature is controlled at about 25°C. When the reaction pressure drops to 0.2MPa, continue to add sulfuryl fluoride to 0.6MPa, and cycle in turn until the pressure drops slowly or does not drop, and the reaction After 14 hours, 75 g of sulfuryl fluoride was consumed to obtain 379 g of a light yellow transparent solution without solid residue. Acetonitrile and unreacted triethylamine were removed by rotary evaporation at 80°C and -0.08MPa (gauge pressure) conditions to obtain 150 g of dark yellow solution, then 30 g of concentrated sulfuric acid (98% by mass) was added, and the mixed solution was distilled under reduced pressure. 41.3g of HFSI product (purity 99....

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Abstract

The invention discloses a preparation method of bis(fluorosulfonyl)amine. The preparation method comprises the following steps of enabling SO2F2 (sulfuryl fluoride), NH4F (ammonium fluoride) and triethylamine to react to prepare organic alkaline salt of bis(fluorosulfonyl)amine; performing replacing reaction with strong acid, and performing pressure-relief distillation, so as to obtain high-puritybis(fluorosulfonyl)amine. The preparation method has the advantages that the SO2F2, the NH4F and the organic alkaline are used as the raw materials, and the FSO3H (fluorosulfonic acid) with strong corrosion property is not used as the raw material; the technology is simple, the continuous operation property is strong, the product is easy to separate and purify, the high-purity (more than or equalto 99%) bis(fluorosulfonyl)amine can be prepared, and the yield rate reaches 90% or above; the chloride ion is not used in the whole reaction process, and the product quality is stable.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery electrolytes, and in particular relates to a preparation method of bisfluorosulfonimide. Background technique [0002] Bisfluorosulfonimide (CAS: 14984-73-7), the chemical formula is (SO 2 F) 2 NH, HFSI for short, density 1.892g / cm 3 , with a melting point of 17°C and a boiling point of 170°C. HFSI and its salts are widely used in fields such as acid catalysts, ionic liquids, and selective fluorinating agents. 2 F) 2 , referred to as LiFSI) as the main raw material, LiFSI has the characteristics of suitable conductivity, high thermal stability, high electrochemical stability, and low probability of side reactions, and is an electrolyte material with wide application prospects. Catalysts and supercapacitors have important industrial application value. [0003] The preparation methods of HFSI mainly include the following types: [0004] chlorosulfonic acid (FSO 3 H), thionyl chlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 慕灯友陈洪龙陈新春薛谊杨成
Owner NANJING REDSUN BIOCHEM CO LTD
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