Free-solvent-free lithium sulfonimide salt compositions that are liquid at room temperature, and methods of making free-solvent-free liquid lithium sulfonimide salt compositions. In an embodiment, the methods include mixing one or more lithium sulfonimide salts with one or more ether-based solvents and then removing the free solvent(s) under suitable vacuum, temperature, and time conditions so as to obtain a free-solvent-free liquid lithium sulfonimide salt composition that is liquid at room temperature. In an embodiment, the only solvent molecules that remain in the liquid lithium sulfonimide salt composition are adducted with lithium sulfonimide salt molecules. An example automated processing system for making free-solvent-free liquid lithium sulfonimide salts is also disclosed.

Provided is a method the enables easy production of bis(fluorosulfonyl)imide suitable for a non-aqueous electrolytic solution for a lithium ion secondary battery, etc. The method for producing a bis(fluorosulfonyl)imide alkali metal salt according to the present invention comprises reacting bis(fluorosulfonyl)imide with an alkali metal compound in a reaction solution containing an organic solvent, wherein the organic solvent includes at least one organic solvent (A) selected from the group consisting of carbonate solvents, cyclic ether solvents, linear ether solvents having two or more oxygen atoms in the molecule, cyclic ester solvents, sulfolane solvents, N,N-dimethyl formamide, dimethyl sulfoxide, and N-methyl oxazolidinone.

Provided is a method the enables easy production of bis(fluorosulfonyl)imide suitable for a non-aqueous electrolytic solution for a lithium ion secondary battery, etc. The method for producing a bis(fluorosulfonyl)imide alkali metal salt according to the present invention comprises reacting bis(fluorosulfonyl)imide with an alkali metal compound in a reaction solution containing an organic solvent, wherein the organic solvent includes at least one organic solvent (A) selected from the group consisting of carbonate solvents, cyclic ether solvents, linear ether solvents having two or more oxygen atoms in the molecule, cyclic ester solvents, sulfolane solvents, N,N-dimethyl formamide, dimethyl sulfoxide, and N-methyl oxazolidinone.

A method of producing purified bis(fluorosulfonyl) imide includes providing a liquid mixture including bis(fluorosulfonyl) imide and fluorosulfonic acid and then contacting the liquid mixture with gaseous ammonia. The gaseous ammonia reacts with the fluorosulfonic acid to produce ammonium fluorosulfate. The method further includes separating the liquid mixture from the ammonium fluorosulfate.

A method of producing purified bis(fluorosulfonyl) imide includes providing a liquid mixture including bis(fluorosulfonyl) imide and fluorosulfonic acid and then contacting the liquid mixture with gaseous ammonia. The gaseous ammonia reacts with the fluorosulfonic acid to produce ammonium fluorosulfate. The method further includes separating the liquid mixture from the ammonium fluorosulfate.

Free-solvent-free lithium sulfonimide salt compositions that are liquid at room temperature, and methods of making free-solvent-free liquid lithium sulfonimide salt compositions. In an embodiment, the methods include mixing one or more lithium sulfonimide salts with one or more ether-based solvents and then removing the free solvent(s) under suitable vacuum, temperature, and time conditions so as to obtain a free-solvent-free liquid lithium sulfonimide salt composition that is liquid at room temperature. In an embodiment, the only solvent molecules that remain in the liquid lithium sulfonimide salt composition are adducted with lithium sulfonimide salt molecules. An example automated processing system for making free-solvent-free liquid lithium sulfonimide salts is also disclosed.

A method for efficiently removing impurities such as sodium ions, fluoride ions, chloride ions and fluorosulfate ions without reducing the yield of a target product, including a fluorine-containing sulfonylamide compound selected from the group consisting of fluorine-containing sulfonylamide, a metal salt thereof, an ammonium salt thereof and a quaternary ammonium salt thereof is washed with an aqueous solution of salt of sulfuric acid.

A method for efficiently removing impurities such as sodium ions, fluoride ions, chloride ions and fluorosulfate ions without reducing the yield of a target product, including a fluorine-containing sulfonylamide compound selected from the group consisting of fluorine-containing sulfonylamide, a metal salt thereof, an ammonium salt thereof and a quaternary ammonium salt thereof is washed with an aqueous solution of salt of sulfuric acid.

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

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