Reaction #658753

ord-6d10dc91474a4f76a6d086d2e6d987c3

Reaction equation

O=P(O)(F)F
Difluorophosphoric acid
[Cl-].[K+]
potassium chloride
COC(=O)OC
dimethyl carbonate
F[P-](F)(F)(F)(F)F.[Li+]
lithium hexafluorophosphate
→
O=P([O-])(F)F.[K+]
potassium difluorophosphate
O=P([O-])(F)F.[Li+]
lithium difluorophosphate

Reactants

O=P(O)(F)F
Difluorophosphoric acid
[Cl-].[K+]
potassium chloride
COC(=O)OC
dimethyl carbonate
F[P-](F)(F)(F)(F)F.[Li+]
lithium hexafluorophosphate

Reagents

None

Conditions

Temperature
130°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturecooled to room temperature

Procedure

Difluorophosphoric acid (reagent, produced by Fluorochem Ltd.) (18.6 g) was weighed into a 250 ml-volume PFA vessel, and 4.1 g of lithium hexafluorophosphate (reagent, produced by Stella Chemifa Corporation) was added. Furthermore, 13.5 g of potassium chloride (reagent, produced by Wako Pure Chemical Industries, Ltd.) and 20.0 g of dimethyl carbonate 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 potassium 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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09028786B2uspto-grants-2015_05