Process for preparing bis(fluorosulfonyl) imide

Patent metadata

Field	Value
Publication number	US-12404175-B2
Application number	US-202017604829-A
Country	US
Kind code	B2
Filing date	Apr 21, 2020
Priority date	Apr 25, 2019
Publication date	Sep 2, 2025
Grant date	Sep 2, 2025

Abstract

The invention relates to a process for preparing bis(fluorosulfonyl)imide, comprising the steps of: i) providing a stream A 1 containing HF and a reactor containing a liquid phase A 2 that contains bis(chlorosulfonyl)imide; ii) in said reactor, bringing said liquid phase A 2 into contact with said stream A 1 to produce bis(fluorosulfonyl)imide, said process being characterized in that said stream A 1 is injected into said liquid phase A 2.

First claim

The invention claimed is:

1. A process for preparing bis(fluorosulfonyl)imide comprising the steps of:
i. providing a stream A 1 comprising HF and providing a reactor containing a liquid phase A 2 comprising bis(halosulfonyl)imide, excluding bis(fluorosulfonyl)imide;
ii. in said reactor, bringing said liquid phase A 2 into contact with said stream A 1 to produce bis(fluorosulfonyl)imide; wherein said stream A 1 is injected into said liquid phase A 2 , wherein when unreacted HF is removed from the reactor, it is not returned to the reactor, wherein said reactor also comprises a dip tube through which said stream A 1 is injected into said liquid phase A 2 .

2. The process as claimed in claim 1 , wherein said reactor comprises a mechanical stirring means for mechanical stirring of said liquid phase A 2 , wherein said mechanical stirring means does not use a magnetic device inside said reactor.

3. The process as claimed in claim 1 , wherein step ii) is carried out under pressure and temperature conditions so as to keep the bis(halosulfonyl)imide and the bis(fluorosulfonyl)imide produced in liquid form.

4. The process as claimed in claim 1 , wherein, during step ii), the temperature of said liquid phase A 2 is kept substantially constant.

5. The process as claimed in claim 1 , wherein, during step ii), the temperature of said liquid phase A 2 varies by at most 5° C. in absolute value.

6. The process as claimed in claim 1 , wherein said reactor comprises a mechanical stirring means for said liquid phase A 2 and said stream A 1 is injected into said liquid phase A 2 close to said mechanical stirring means.

7. The process as claimed in claim 1 , wherein the rate of introduction, into said liquid phase A 2 , of the hydrofluoric acid contained in said stream A 1 is at least 1 mol of HF/mole of bis(halosulfonyl)imide/hour.

8. The process as claimed in claim 1 , wherein step ii) is carried out with an HF/[bis(halosulfonyl)imide]molar ratio of at least 2.0 and at most 3.0.

9. The process as claimed in claim 1 , wherein step ii) is performed at a temperature above 0° C.

10. The process as claimed in claim 1 , wherein the bis(halosulfonyl)imide compound is bis(chlorosulfonyl)imide.

11. A process for preparing a lithium bis(fluorosulfonyl)imide salt, comprising the steps:
a) carrying out the process for preparing the bis(fluorosulfonyl)imide as claimed in claim 1 ;
b) bringing the bis(fluorosulfonyl)imide into contact with a composition comprising at least one lithium salt in order to form said lithium bis(fluorosulfonyl)imide salt.

12. The process as claimed in claim 1 , wherein step ii) is carried out at a temperature above 15° C. and below 50° C.

13. The process as claimed in claim 1 , wherein step ii) is carried out in the absence of a catalyst.

Assignees

• Arkema France

Inventors

• Deur-Bert Dominique

Classifications

• H01M10/0568

  characterised by the solutes · CPC title

• H01M10/052

  Li-accumulators · CPC title

• C01B21/0935 Primary

  Imidodisulfonic acid; Nitrilotrisulfonic acid; Salts thereof · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title

• C01B21/086 Primary

  containing one or more sulfur atoms · CPC title