Method for preparing bis(fluorosulfonyl)imide acid and salts thereof

Patent metadata

Field	Value
Publication number	US-10122048-B2
Application number	US-201415101149-A
Country	US
Kind code	B2
Filing date	Dec 3, 2014
Priority date	Dec 5, 2013
Publication date	Nov 6, 2018
Grant date	Nov 6, 2018

Abstract

The invention relates to a method for preparing bis(fluorosulfonyl)imide acid, comprising: the reaction of sulphamic acid or one of the salts thereof with a halogenosulfuric acid and at least one fluorinating agent selected from SOF2, F—SO2—F and SF4, and the subsequent recovery of bis(fluorosulfonyl)imide acid. The invention also relates to a method for producing salts of bis(fluorosulfonyl)imide from the bis(fluorosulfonyl)imide acid thus produced.

First claim

The invention claimed is:

1. A process for preparing bis(fluorosulfonyl)imide acid of formula F—SO 2 —NH—SO 2 —F, the process comprising the reaction of sulfamic acid or a salt thereof with at least one halosulfuric acid and at least one fluorinating agent selected from the group consisting of SOF 2 , F—SO 2 —F and SF 4 , then the recovery of the bis(fluorosulfonyl)imide acid.

2. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein the halosulfuric acid has the formula X—SO 2 —OH wherein X is a halogen selected from the group consisting of fluorine, chlorine, bromine and iodine.

3. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein said reaction is carried out in the presence of an organic solvent.

4. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein the halosulfuric acid represents from 1 mol % to 5 molar equivalents expressed relative to the sulfamic acid or salts thereof and the fluorinating agent is F—SO 2 —F.

5. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 4 , wherein the halosulfuric acid represents from 5 mol % to 1 molar equivalent expressed relative to the sulfamic acid or salts thereof.

6. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein the halosulfuric acid represents from 1 to 5 molar equivalent(s) expressed relative to the sulfamic acid or salts thereof and the fluorinating agent is SOF 2 or SF 4 .

7. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein said fluorinating agent represents from 1 to 10 molar equivalent(s) expressed relative to the sulfamic acid or salts thereof.

8. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein said reaction is performed at a temperature between 0 and 180° C.

9. The process for preparing bis(fluorosulfonyl)imide acid as claimed in claim 1 , wherein said bis(fluorosulfonyl)imide acid is recovered by distillation, by sublimation or by extraction.

10. A process for preparing at least one bis(fluorosulfonyl)imide salt, the process comprising preparing the bis(fluorosulfonyl)imide acid according to the process as defined in claim 1 , followed by bringing said acid into contact with at least one salification agent.

11. The process for preparing at least one bis(fluorosulfonyl)imide salt as claimed in claim 10 , wherein the salification agent is a metal hydroxide, a metal halide, a metal hydride, a metal trifluoroacetate or a metal trifluoromethanesulfonate.

12. The process for preparing at least one bis(fluorosulfonyl)imide salt as claimed in claim 10 , wherein said salt has the general formula F—SO 2 —N-M-SO 2 —F, where M represents an alkali metal, an alkaline-earth metal, a transition metal or a metal selected from lanthanides.

13. The process for preparing at least one bis(fluorosulfonyl)imide salt as claimed in claim 10 , wherein said salt is lithium bis(fluorosulfonyl)imide.

14. The process for preparing at least one bis(fluorosulfonyl)imide salt as claimed in claim 10 , also comprising a step of purifying said salt.

15. The process for preparing at least one bis(fluorosulfonyl)imide salt as claimed in claim 14 , wherein the purification step consists of a recrystallization.

Assignees

• Rhodia Operations

Inventors

• Buisine Olivier

Classifications

• C01B21/093

  containing also one or more sulfur atoms · CPC title

• C01B21/086

  containing one or more sulfur atoms · CPC title

• H01M10/0568 Primary

  characterised by the solutes · CPC title

• H01M2300/0025

  Organic electrolyte · CPC title

• C01B21/0935 Primary

  Imidodisulfonic acid; Nitrilotrisulfonic acid; Salts thereof · CPC title