Method for producing difluorophosphate
View Patent ↗Provided is a method for producing a difluorophosphate, which can simply and easily produce a high-purity difluorophosphate in an industrially advantageous manner. The method includes steps of: reacting an aqueous hydrofluoric acid solution with an oxyhalide of phosphorous (except phosphoric trifluoride) to produce a crude difluorophosphoric acid; reacting the crude difluorophosphoric acid with a halide of an alkali metal, an alkaline earth metal, aluminum or an onium to produce a difluorophosphate in the crude difluorophosphoric acid; and heating and drying the crude difluorophosphoric acid containing the difluorophosphate to distill away the crude difluorophosphoric acid, or precipitating the difluorophosphate in the crude difluorophosphoric acid by crystallization, subsequently separating the difluorophosphate by solid-liquid separation, and further distilling away the crude difluorophosphoric acid contained in the difluorophosphate after solid-liquid separation.
1. A method for producing a difluorophosphate, comprising:
a step of reacting an aqueous hydrofluoric acid solution with an oxyhalide of phosphorous (except phosphoric trifluoride) to produce a crude difluorophosphoric acid,
a step of reacting the crude difluorophosphoric acid with a halide of an alkali metal, an alkaline earth metal, aluminum or an onium to produce a difluorophosphate in the crude difluorophosphoric acid, and
a step of heating and drying the crude difluorophosphoric acid containing the difluorophosphate to distill away the crude difluorophosphoric acid, or a step of precipitating the difluorophosphate in the crude difluorophosphoric acid by crystallization, subsequently separating the difluorophosphate by solid-liquid separation, and further distilling away the crude difluorophosphoric acid contained in the difluorophosphate after the solid-liquid separation.
2. The method for producing a difluorophosphate according to claim 1 , wherein the step of reacting the aqueous hydrofluoric acid solution with the oxyhalide of phosphorous to produce a crude difluorophosphoric acid is performed by adding the aqueous hydrofluoric acid solution to the oxyhalide of phosphorous while the oxyhalide of phosphorous is cooled.
3. The method for producing a difluorophosphate according to claim 1 , wherein the halide of an alkali metal, an alkaline earth metal, aluminum or an onium is in the form of particles, and the maximum particle diameter thereof is less than 10 mm.
4. The method for producing a difluorophosphate according to claim 1 , wherein the step for producing the difluorophosphate in the crude difluorophosphoric acid is performed by keeping the liquid temperature of the crude difluorophosphoric acid in the range of −40° C. to 100° C. at the time of adding the halide of an alkali metal, an alkaline earth metal, aluminum or an onium to the crude difluorophosphoric acid.
5. The method for producing a difluorophosphate according to claim 1 , wherein the following step is repeated: a step of adding, to the crude difluorophosphoric acid after the solid-liquid separation, a halide of an alkali metal, an alkaline earth metal, aluminum or an onium, and subsequently heating and drying the resultant system to distill away a surplus of the crude difluorophosphoric acid; or a step of separating a deposit deposited by crystallizing the crude difluorophosphoric acid containing the difluorophosphate by solid-liquid separation, and further distilling away the crude difluorophosphoric acid contained in the deposit.
6. The method for producing a difluorophosphate according to claim 2 , wherein the halide of an alkali metal, an alkaline earth metal, aluminum or an onium is in the form of particles, and the maximum particle diameter thereof is less than 10 mm.
7. The method for producing a difluorophosphate according to claim 6 , wherein the step for producing the difluorophosphate in the crude difluorophosphoric acid is performed by keeping the liquid temperature of the crude difluorophosphoric acid in the range of −40° C. to 100° C. at the time of adding the halide of an alkali metal, an alkaline earth metal, aluminum or an onium to the crude difluorophosphoric acid.
8. The method for producing a difluorophosphate according to claim 7 , wherein the following step is repeated: a step of adding, to the crude difluorophosphoric acid after the solid-liquid separation, a halide of an alkali metal, an alkaline earth metal, aluminum or an onium, and subsequently heating and drying the resultant system to distill away a surplus of the crude difluorophosphoric acid; or a step of separating a deposit deposited by crystallizing the crude difluorophosphoric acid containing the difluorophosphate by solid-liquid separation, and further distilling away the crude difluorophosphoric acid contained in the deposit.