Dimethyl Carbonate → Lithium phosphorodifluoridate

Participants

Reaction Conditions

Reaction Steps

Difluorophosphoric acid (reagent, produced by Fluorochem Ltd.) (15.4 g) was weighed into a 250 ml-volume PFA vessel, and 3.4 g of lithium hexafluorophosphate (reagent, produced by Stella Chemifa Corporation) was added. Furthermore, 7.1 g of magnesium chloride (reagent, produced by Wako Pure Chemical Industries, Ltd.) and 15.0 g of dimethyl carbonate (reagent, produced by Kishida Chemical Co., Ltd.) were added, and the mixture was stirred for 1 hour under nitrogen flow and after heating at 130° C. for 17 hours, cooled to room temperature to obtain a mixed crystal of magnesium difluorophosphate and lithium difluorophosphate. Anion analysis was performed in the same manner as in Example 2-6, as a result, the obtained difluorophosphate ion was 91% in terms of the relative area.

Provenance & Evidence