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Process for preparing bis(fluorosulfonyl) imide

A technology of fluorosulfonyl and imide, applied in the field of bisimide preparation, which can solve the problem of increasing carbon footprint

Pending Publication Date: 2021-12-10
ARKEMA FRANCE SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Furthermore, the operating conditions applied in this method require significant energy input, which increases the carbon footprint of this method

Method used

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  • Process for preparing bis(fluorosulfonyl) imide
  • Process for preparing bis(fluorosulfonyl) imide
  • Process for preparing bis(fluorosulfonyl) imide

Examples

Experimental program
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Effect test

Embodiment approach

[0032] According to a particular embodiment, said liquid phase A2 comprises bis(halosulfonyl)imide but is free of organic solvents. Thus, step ii) of fluorination of the bis(halosulfonyl)imide to bis(fluorosulfonyl)imide is carried out in the absence of an organic solvent.

[0033] According to an alternative particular embodiment, said liquid phase A2 comprises a bis(halosulfonyl)imide and an organic solvent. The organic solvent SO1 may be selected from esters, nitriles, ethers, aromatic solvents, carbonates, cyclic or heterocyclic solvents and mixtures thereof. Preferably, the organic solvent SO1 is selected from methyl acetate, butyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyronitrile, valeronitrile, benzonitrile, diisopropyl ether, 2-methyl acetate Oxy-2-methylbutane, cyclopentyl methyl ether, benzene, toluene, chlorobenzene, dichlorobenzene, xylene, ethylbenzene, 1,4-dioxane, dimethyl carbonate, ethylene Ethyl carbonate, sulfolane and mixtures there...

Embodiment 1

[0095]Into a stirred 1 liter reactor were introduced 394 g of liquid bis(chlorosulfonyl)imide (HCSI) and 19.7 g of liquid 1,4-dioxane. The weight ratio between 1,4-dioxane and HCSI was 5%. The mixture was agitated using a turbine with 6 pitched blades and allowed to reach 40 °C before introducing hydrofluoric acid. The reaction is carried out by adjusting the temperature of the reaction medium at 40° C. and by continuous injection of gaseous HF. Gaseous HF is injected slowly directly into the liquid reaction medium through a dip tube. The total amount of HF injected was 110 g, which corresponds to a molar ratio of HF to HCSI of 3. The rate of introduction of gaseous HF was adjusted at 37 g / h. The reaction time was 3 hours. The reaction is accompanied by the formation of HCl, which is continuously removed from the reactor. The gas leaving the reactor is sent to a water trap. When all the HF has been introduced, a nitrogen stream with a flow rate of 50 l / h is introduced in...

Embodiment 2

[0100] Into a stirred 1 liter reactor were introduced 397 g of liquid bis(chlorosulfonyl)imide (HCSI) and 12 g of liquid 1,4-dioxane. The weight ratio between 1,4-dioxane and HCSI was 3%. The mixture was agitated using a turbine with 6 pitched blades and allowed to reach 45°C before introducing hydrofluoric acid. The reaction is carried out by adjusting the temperature of the reaction medium at 45° C. and by continuous injection of gaseous HF. Gaseous HF is injected slowly directly into the liquid reaction medium through a dip tube. The total amount of HF introduced was 100 g, which corresponds to a molar ratio of HF to HCSI of 2.7. The introduction rate of gaseous HF was adjusted at 38 g / h. The reaction time was 2 hours and 40 minutes. The reaction is accompanied by the formation of HCl, which is continuously removed from the reactor. The gas leaving the reactor is sent to a water trap. When all the HF has been introduced, a nitrogen stream with a flow rate of 50 l / h is...

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Abstract

The invention relates to a process for preparing bis(fluorosulfonyl) imide, comprising the steps of: i) providing a stream A1 containing HF and a reactor containing a liquid phase A2 that contains bis(chlorosulfonyl) imide; ii) in said reactor, bringing said liquid phase A2 into contact with said stream A1 to produce bis(fluorosulfonyl) imide, said process being characterized in that said stream A1 is injected into said liquid phase A2.

Description

technical field [0001] The present invention relates to a process for the preparation of bis(fluorosulfonyl)imides. In particular, the present invention relates to a process for the preparation of bis(fluorosulfonyl)imides from bis(halosulfonyl)imides. Background technique [0002] Due to the very low basicity of sulfonylimide-type anions, they are increasingly being used in the field of energy storage in the form of inorganic salts in batteries or as organic salts in supercapacitors or in ionic liquids used in the field. Since the battery market is rapidly developing and reducing battery manufacturing costs is becoming an important issue, large-scale, low-cost synthetic methods of this type of anion are required. [0003] In the specific field of Li-ion batteries, the most widely used salt is LiPF 6 , but this salt has many disadvantages such as limited thermal stability, susceptibility to hydrolysis and thus reduced battery safety. Recently, FSO with 2 – group, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086C01B21/093C07F1/02H01M10/0525H01M10/0568H01M10/052
CPCC01B21/086C01B21/0935H01M10/0568H01M10/052Y02E60/10
Inventor D.德里-伯特
Owner ARKEMA FRANCE SA
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