Patent classifications
C01B21/086
METHOD FOR PREPARING IMIDE SALTS CONTAINING A FLUOROSULFONYL GROUP
The present invention concerns a method for preparing a compound of the following formula (III): R.sub.2(SO.sub.2)NM(SO.sub.2)F (III) in which R.sub.2 represents one of the following radicals: F, CF.sub.3, CHF.sub.2, CH.sub.2F, C.sub.2HF.sub.4, C.sub.2H.sub.2F.sub.3, C.sub.2H.sub.3F.sub.2, C.sub.2F, C.sub.3F.sub.7, C.sub.3H.sub.4F.sub.3, C.sub.3HF.sub.6, C.sub.4F.sub.9, C.sub.4H.sub.2F.sub.7, C.sub.4H.sub.4F, CF.sub.11, C.sub.6F.sub.13, C.sub.7F.sub.1, C.sub.8F.sub.17 or C.sub.9F.sub.19. M represents a monovalent or divalent cation; the method comprising: a step b) of fluorinating a compound of the following formula (I): R.sub.1(SO.sub.2)NH(SO.sub.2)Cl (I) in which R represents one of the following radicals: Cl, F, CF.sub.3, CHF.sub.2, CH.sub.2F, C.sub.2HF.sub.4, C.sub.2H.sub.2F.sub.3, C.sub.2H.sub.3F.sub.2, C.sub.2F, C.sub.3F.sub.7, C.sub.3H.sub.4F.sub.3, C.sub.3HF.sub.6, C.sub.4F.sub.9, C.sub.4H.sub.2F.sub.7, C.sub.4H.sub.4F, CF.sub.11, C.sub.6F.sub.13, C.sub.7F.sub.15, C.sub.8F.sub.17 or C.sub.9F.sub.19, R preferably representing Cl; with at least one fluorinating agent; 2a step c) of distilling the composition obtained in step b).
METHOD FOR PREPARING IMIDE SALTS CONTAINING A FLUOROSULFONYL GROUP
The present invention concerns a method for preparing a compound of the following formula (III): R.sub.2(SO.sub.2)NM(SO.sub.2)F (III) in which R.sub.2 represents one of the following radicals: F, CF.sub.3, CHF.sub.2, CH.sub.2F, C.sub.2HF.sub.4, C.sub.2H.sub.2F.sub.3, C.sub.2H.sub.3F.sub.2, C.sub.2F, C.sub.3F.sub.7, C.sub.3H.sub.4F.sub.3, C.sub.3HF.sub.6, C.sub.4F.sub.9, C.sub.4H.sub.2F.sub.7, C.sub.4H.sub.4F, CF.sub.11, C.sub.6F.sub.13, C.sub.7F.sub.1, C.sub.8F.sub.17 or C.sub.9F.sub.19. M represents a monovalent or divalent cation; the method comprising: a step b) of fluorinating a compound of the following formula (I): R.sub.1(SO.sub.2)NH(SO.sub.2)Cl (I) in which R represents one of the following radicals: Cl, F, CF.sub.3, CHF.sub.2, CH.sub.2F, C.sub.2HF.sub.4, C.sub.2H.sub.2F.sub.3, C.sub.2H.sub.3F.sub.2, C.sub.2F, C.sub.3F.sub.7, C.sub.3H.sub.4F.sub.3, C.sub.3HF.sub.6, C.sub.4F.sub.9, C.sub.4H.sub.2F.sub.7, C.sub.4H.sub.4F, CF.sub.11, C.sub.6F.sub.13, C.sub.7F.sub.15, C.sub.8F.sub.17 or C.sub.9F.sub.19, R preferably representing Cl; with at least one fluorinating agent; 2a step c) of distilling the composition obtained in step b).
METHOD FOR PREPARING AN IMIDE SALT CONTAINING A FLUOROSULPHONYL GROUP
A method for preparing a compound having the following formula (IV): R.sub.2(SO.sub.2)NLi(SO.sub.2)F (IV), the method including a step a) of reacting a sulphamide having the following formula (A): R.sub.0(SO.sub.2)NH.sub.2 (A) with at least one sulphur-containing acid and at least one chlorinating agent, the step a) being carried out: at a temperature between 90 C. and 130 C., and at a pressure which is strictly greater than 7 bar (absolute).
METHOD FOR PREPARING AN IMIDE SALT CONTAINING A FLUOROSULPHONYL GROUP
A method for preparing a compound having the following formula (IV): R.sub.2(SO.sub.2)NLi(SO.sub.2)F (IV), the method including a step a) of reacting a sulphamide having the following formula (A): R.sub.0(SO.sub.2)NH.sub.2 (A) with at least one sulphur-containing acid and at least one chlorinating agent, the step a) being carried out: at a temperature between 90 C. and 130 C., and at a pressure which is strictly greater than 7 bar (absolute).
Method for Preparing Lithium Bis(Fluorosulfonyl)imide Salt
The present invention relates to a method for preparing a lithium bis(fluorosulfonyl)imide salt, including a step of dissolving bis(chlorosulfonyl)imide in an organic solvent in a non-glass vessel to prepare a first reaction solution; a step of injecting lithium fluoride (LiF) to the first reaction solution in the non-glass vessel and refluxing while heating to prepare a second reaction solution; a step of separating a product including a lithium bis(fluorosulfonyl)imide salt and the organic solvent from the second reaction solution; and a step of obtaining the lithium bis(fluorosulfonyl)imide salt in a solid phase from the product, wherein the organic solvent is at least one or more selected from the group consisting of ethyl acetate, butyl acetate, chloroform, dichloromethane, dichloroethane, benzene, xylene and acetonitrile.
Free-solvent-free lithium sulfonamide salt compositions that are liquid at room temperature, and uses thereof in lithium ion battery
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.
Method for producing bis(fluorosulfonyl)imide alkali metal salt and method for producing non aqueous electrolytic solution
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.
Method for producing bis(fluorosulfonyl)imide alkali metal salt and method for producing non aqueous electrolytic solution
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.
PURIFICATION OF BIS(FLUOROSULFONYL) IMIDE
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 Sulfonamide Salt Compositions That Are Liquid at Room Temperature, and Uses Thereof In Lithium Ion Battery
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.