Method for producing ultra-pure bis(chlorosulfonyl)imide
US-2024391774-A1 · Nov 28, 2024 · US
US9985317B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9985317-B2 |
| Application number | US-201715409708-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jan 19, 2017 |
| Priority date | May 28, 2010 |
| Publication date | May 29, 2018 |
| Grant date | May 29, 2018 |
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The present invention provides an alkali metal salt of fluorosulfonyl imide having favorable heat resistance and a reduced content of specific impurities and a water content, and provides a method for producing an alkali metal salt of fluorosulfonyl imide, which is capable of easily removing a solvent from a reaction solution. An alkali metal salt of fluorosulfonyl imide of the present invention is represented by the following general formula (I) and has a mass loss rate of 2% or less when the alkali metal salt of fuluorosulufonyl imide is kept at 100° C. for 8 hours under an air current. A method for producing an alkali metal salt of fluorosulfonyl imide of the present invention comprises a step of concentrating a solution of the alkali metal salt of fulorosulfonyl imide by bubbling a gas into a reaction solution containing the alkali metal salt of fulorosulfonyl imide, and/or concentrating a solution of the alkali metal salt of fulorosulfonyl imide by thin layer distillation.
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The invention claimed is: 1. An electrolytic solution comprising an alkali metal salt of fluorosulfonyl imide of formula (I) and a medium, wherein a content of SO 4 2− in the electrolytic solution is 0 to 1,500 ppm by mass, wherein in the formula (I), M a is an alkali metal, and R a and R b are independently a fluorine atom, or an alkyl group having 1 to 6 carbon atoms in which one or more hydrogen atoms are substituted with a fluorine atom, and at least one of R a or R b is a fluorine atom. 2. The electrolytic solution according to claim 1 , wherein the content of SO 4 2− in the electrolytic solution is 0 to 500 ppm by mass. 3. The electrolytic solution according to claim 1 , wherein the content of SO 4 2− in the electrolytic solution is 0 to 250 ppm by mass. 4. The electrolytic solution according to claim 1 , wherein the content of SO 4 2− in the electrolytic solution is 1 to 1,500 ppm by mass. 5. The electrolytic solution according to claim 1 , wherein the content of SO 4 2− in the electrolytic solution is 14 to 1,500 ppm by mass. 6. The electrolytic solution according to claim 1 , wherein a content of water is 250 ppm by mass or less. 7. The electrolytic solution according to claim 6 , wherein the content of water is 150 ppm by mass or less. 8. The electrolytic solution according to claim 6 , wherein the content of water is 50 ppm by mass or less. 9. The electrolytic solution according to claim 6 , further comprising 2,000 ppm by mass or less of a residual solvent. 10. The electrolytic solution according to claim 9 , wherein the content of the residual solvent is 1,500 ppm by mass or less. 11. The electrolytic solution according to claim 9 , wherein a content of F − is 500 ppm by mass or less. 12. The electrolytic solution according to claim 11 , wherein the content of F − is 400 ppm by mass or less. 13. The electrolytic solution according to claim 12 , wherein the content of F − is 150 ppm by mass or less. 14. The electrolytic solution according to claim 1 , wherein the alkali metal salt of fluorosulfonyl imide is an alkali metal salt of bis(fluorosulfonyl)imide. 15. The electrolytic solution according to claim 1 , wherein the alkali metal salt of fluorosulfonyl imide is selected from a sodium salt, a potassium salt or a lithium salt. 16. The electrolytic solution according to claim 1 , further comprising one or more other electrolytes, wherein a cation species constituting the one or more other electrolytes is selected from the group consisting of alkali metal ions, alkaline earth metal ions and onium cations, and an anion species constituting the one or more other electrolytes is selected from the group consisting of PF 6 − , BF 4 − , ClO 4 − , AlCl 4 − , C[(CN) 3] − , N[(CN) 2] − , B[(CN) 4] − , N[(SO 2 CF 3 ) 2] − , CF 3 (SO 3 ) − , C[(CF 3 SO 2 ) 3] − , AsF 6 − , SbF 6 − , and dicyanotriazolate ion. 17. The electrolytic solution according to claim 16 , wherein an amount of the one or more other electrolytes is 0.1% by mass or more and 99% by mass or less with respect to 100% by mass of the total amount of the alkali metal salt of fluorosulfonyl imide and the one or more other electrolytes. 18. The electrolytic solution according to claim 16 , wherein a total amount of the alkali metal salt of fluorosulfonyl imide and the one or more other electrolytes in the electrolytic solution is 0.1% by mass or more and the saturation concentration or less. 19. The electrolytic solution according to claim 16 , wherein an amount of the medium is 50 parts by mass or more and 99.9 parts by mass or less with respect to 100 parts by mass of the total amount of the alkali metal salt of fluorosulfonyl imide, the one or more other electrolytes and the medium.
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