Process for the preparation of lithium or sodium bis(fluorosulphonyl)imide

Patent metadata

Field	Value
Publication number	US-10547084-B2
Application number	US-201615189978-A
Country	US
Kind code	B2
Filing date	Jun 22, 2016
Priority date	May 24, 2011
Publication date	Jan 28, 2020
Grant date	Jan 28, 2020

Abstract

A process for the preparation of a bis(sulphonato)imide salt of formula: (III) (SO 3 − )—N − —(SO 3 − ) 3C + where C + represents a monovalent cation, comprising the reaction of amidosulphuric acid of formula: (I) (OH)—SO 2 —NH 2 with a halosulphonic acid of formula: (II) (OH)—SO 2 —X where X represents a halogen atom, and comprising a reaction with a base which is a salt formed with the cation C + . Also, a process for the preparation of bis(fluorosulphonyl)imide acid of formula: (V) F—(SO 2 )—NH—(SO 2 )—F and to a process for the preparation of lithium bis(fluorosulphonyl)imide salt of formula: (VII) F—(SO 2 )—N − —(SO 2 )—F Li + .

First claim

The invention claimed is:

1. An electrolyte comprising the bis(fluorosulphonyl)imide salt of formula (VII) made by the process for the preparation of bis(fluorosulphonyl)imide salt of formula:
F—(SO 2 )—N − —(SO 2 )—F M +   (VII)

wherein M is Li or Na,
the process comprising the preparation of bis(fluorosulphonyl)imide acid of formula (V)
F—(SO 2 )—NH—(SO 2 )—F  (V)

by fluorination of a bis(chlorosulfonyl)imide acid of formula:
Cl—(SO 2 )—NH—(SO 2 )—Cl; and

purifying the bis(fluorosulfonyl)imide acid of formula (V) by extraction, wherein the extraction comprises extraction with an organic solvent;
wherein the fluorination is carried out with hydrogen fluoride as a fluorinating agent and then the reaction of the bis(fluorosulphonyl)imide acid with a lithium or sodium base,
wherein the lithium or sodium base comprises lithium hydroxide, lithium carbonate, sodium hydroxide or sodium carbonate,
wherein, when M is Li:
wherein LiCI, LiF and FSO 3 Li are each present in the lithium bis(fluorosulphonyl)imide, and
wherein the lithium bis(flourosulphonyl)imide comprises at most 1000 ppm of each of the LiCl, LiF and FSO 3 Li.

2. An electrolyte comprising the bis(fluorosulphonyl)imide salt of formula: F—(SO 2 )—N − —(SO 2 )—F M + made by the process for the preparation of bis(fluoro-sulphonyl)imide salt of formula: F—(SO 2 )—N − —(SO 2 )—F M + , wherein M is Li or Na, the process comprising:
fluorination of a bis(chlorosulfonyl)imide acid of formula: Cl—(SO 2 )—NH—(SO 2 )—Cl to form bis(fluorosulphonyl)imide acid of formula: F—(SO 2 )—NH—(SO 2 )—F;
reaction of the bis(fluorosulphonyl)imide acid with a lithium or sodium base to form the F—(SO 2 )—N − —(SO 2 )—F M + ;
wherein the fluorination is carried out with hydrogen fluoride as a fluorinating agent,
wherein, when M is Li:
wherein LiCI, LiF and FSO 3 Li are each present in the lithium bis(fluorosulphonyl)imide, and
wherein the lithium bis(fluorosulphonyl)imide comprises at most 1000 ppm of each of the LiCI, LiF and FSO 3 Li.

3. A process for the preparation of a bis(fluorosulfonyl)imide acid of formula:
F—(SO 2 )—NH—(SO 2 )—F  (V)

by fluorination of a bis(chlorosulfonyl)imide acid of formula:
Cl—(SO 2 )—NH—(SO 2 )—Cl;

the process comprising fluorinating a starting mixture of Cl—(SO 2 )—NH—(SO 2 )—Cl and KCl,
wherein the fluorination is carried out with hydrogen fluoride as a fluorinating agent.

4. The electrolyte of claim 1 , wherein, when M is Na:
wherein NaCl, NaF and FSO 3 Na are each present in the sodium bis(fluorosulphonyl)imide, and
wherein the sodium bis(fluorosulphonyl)imide comprises at most 1000 ppm of each of the NaCl, NaF and FSO 3 Na.

5. The electrolyte of claim 2 , wherein, when M is Na:
wherein NaCl, NaF and FSO 3 Na are each present in the sodium bis(fluorosulphonyl)imide, and
wherein the sodium bis(fluorosulphonyl)imide comprises at most 1000 ppm of each of the NaCl, NaF and FSO 3 Na.

Assignees

• Arkema France

Inventors

• Schmidt Grégory

Classifications

• C01B21/093

  containing also one or more sulfur atoms · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• H01M10/0568 Primary

  characterised by the solutes · CPC title

• H01M10/054

  Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium · CPC title

• H01M10/052

  Li-accumulators · CPC title