Fluorosulfonyl imide salt and method for producing fluorosulfonyl imide salt

Patent metadata

Field	Value
Publication number	US-9947967-B2
Application number	US-201013264244-A
Country	US
Kind code	B2
Filing date	Nov 26, 2010
Priority date	Nov 27, 2009
Publication date	Apr 17, 2018
Grant date	Apr 17, 2018

Abstract

The present invention provides a method for producing a fluorisulfonylimide salt, which enables reducing the impurity content and continuous operation for a long time, and a fluorosulfonyl imide salt. The fluorosulfonyl imide salt of the present invention has a K content of 10,000 ppm or less. The method for producing a fluorosulfonyl imide salt of the present invention is that after a fluorination reaction of chlorosulfonyl imde or a salt thereof, the reaction solution is brought into contact with an aqueous alkaline solution so as to remove impurities. The fluorosulfonyl imide salt of the present invention, in which various impirities are reduced to extremely low levels, is useful as an electrolyte used in a lithium secondary battery, a capacitor or the like, an ionic liquid, or an intermediate for a sulfonyl imide salt, and the like. It is expected that use of the fluorosulfonyl imide salt of the present invention as an electrolyte leads to a high-performance electrochemical device.

First claim

The invention claimed is:

1. A method for producing a di (fluorosulfonyl) imide salt or N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl) imide salt comprising a contacting step wherein a reaction solution is brought into contact with an aqueous alkali solution by pouring the reaction solution into the aqueous alkali solution after a fluorination of chlorosulfonyl imide or a salt thereof and prior to a cation exchange reaction so as to remove an impurity,
wherein the aqueous alkali solution is selected from the group consisting of ammonia water, an aqueous solution of aliphatic amines, alkanolamines or ethylene oxide adducts of these amines, and heterocyclic amines, and
an amount of a basic substance in the aqueous alkali solution is 1 mol or more per 1 mol of a fluorinating agent in the fluorination, and
wherein the di (fluorosulfonyl) imide salt or N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl) imide salt contains:
5,000 ppm by mass or less of K,
500 ppm by mass or less of each of Cl, Si, B, Fe, Cr, Mo and Ni,
at least 0.1 ppm by mass of a total of Si, B, Fe, Cr, Mo and Ni,
0.1 ppm to 5,000 ppm by mass of a total of FSO 2 NH 2 and FSO 3 H, and
1,000 ppm by mass or less of a total of metal elements selected from the group consisting of Zn, Cu and Bi.

2. The method according to claim 1 , wherein the reaction solution is brought into contacted with the aqueous alkali solution at a temperature of about 5° C. to 50° C.

3. The method according to claim 1 , wherein the aqueous alkali solution is used in an amount of from 1 part by mass to 100 parts by mass based on 100 parts by mass of the reaction solution.

4. The method according to claim 1 , wherein the aqueous alkali solution is ammonia water.

5. The method according to claim 1 , wherein the di (fluorosulfonyl) imide salt or N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl) imide salt is a di(fluorosulfonyl)imide salt.

6. The method according to claim 1 , wherein the di (fluorosulfonyl) imide salt or N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl) imide salt is a lithium salt or sodium salt of di (fluorosulfonyl) imide or N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl) imide.

Assignees

• Sato Shimpei
• Okumura Yasunori
• Sato Yuichi
• Miyoshi Yasuyuki
• Nippon Catalytic Chem Ind

Inventors

• Sato Shimpei
• Okumura Yasunori
• Sato Yuichi
• Miyoshi Yasuyuki

Classifications

• C01B21/086

  containing one or more sulfur atoms · CPC title

• H01M10/0568 Primary

  characterised by the solutes · CPC title

• C01B21/0935

  Imidodisulfonic acid; Nitrilotrisulfonic acid; Salts thereof · CPC title

• C01B21/093 Primary

  containing also one or more sulfur atoms · CPC title

• C07C303/36

  of amides of sulfonic acids · CPC title