Synthesis of tetrabutylammonium bis(fluorosulfonyl)imide and related salts
AssigneeTrinapco, Inc.
InventorMartin Reid Johnson
Life of this patent
Estimating the term…
Abstract
The present invention is directed to methods comprising adding ammonia, either as an ammonium salt or as a gas at pressures below 0.01 MPa, to a sulfuryl fluoride solution to form the anion of bis(fluorosulfonyl)amine under conditions well suited for large-scale production. The bis(fluorosulfonyl)amine so produced can be isolated by methods described in the prior art, or isolated as an organic ion pair, such as an alkylammonium solid salt, or as an ionic liquid.
Claims20
A process for the production of a salt of bis(fluorosulfonyl) imide anion (Mx+m[(FSO2)2N−]n, wherein M+ is an inorganic or organic cation and x, n and m are integers from 1-4, comprising:
- adding ammonia (NH3) to a solution of sulfuryl fluoride (SO2F2) in a solvent in a sealed reactor, in the presence of an aprotic base, while maintaining a pressure inside the sealed reactor below 0.01 MPa (75 Torr), to produce a solution or concentrate comprising the product ion [(FSO2)2N]− (“FSI”);
- mixing the solution comprising the product ion [(FSO2)2N]− (“FSI”) to a solution or concentrate comprising of a salt of Mx+ and
- isolating the resulting salt comprising bis(fluorosulfonyl) imide anion ([(FSO2)2N]−).
A process for the production of a salt of bis(fluorosulfonyl) imide anion (Mxx+m[(FSO2)2N−]n, wherein M+ is an inorganic or organic cation and x, n and m are integers from 1-4, comprising,
- adding ammonia (NH3) to a solution comprising an initial amount of sulfuryl fluoride (SO2F2) in a solvent in a sealed reactor, in the presence of an aprotic base, while maintaining a pressure inside the sealed reactor below 0.01 MPa (75 Torr);
- continuously adding an additional amount of sulfuryl fluoride (SO2F2) after the step of adding ammonia is complete, at a pressure greater than 0.008 MPa, until a pre-determined stoichiometry has been reached to form a dissolved [(FSO2)2N]− anion and a dissolved fluoride anion;
- optionally distilling off the solvent;
- and
- isolating a salt comprising the [(FSO2)2N−] anion.
A process for the production of a salt of bis(fluorosulfonyl) imide anion (Mx+m[(FSO2)2N−]n, wherein M+ is an inorganic or organic cation and x, n and m are integers from 1-4, comprising:
- adding sulfuryl fluoride (SO2F2) to a suspension, pellet, or other form of solid ammonium fluoride in a solvent in a sealed reactor, in the presence of an aprotic base, wherein the pressure within said sealed reactor is below 0.01 MN (75 torr) after ammonium fluoride is added;
- and
- isolating said salt.
Dependencies are inferred from the claim text.