Method for preparing a vanadium phosphate
The present invention relates to a process for preparing an ammonium vanadium phosphate of formula (NH 4 )(VO 2 )(HPO 4 ). It also relates to a process for preparing a vanadium orthophosphate VPO 4 .
1. A process for preparing a phosphate of formula (NH 4 )(VO 2 )(HPO 4 ), the process consisting of stirring a mixture of V 2 O 5 and of NH 4 H 2 PO 4 in the solid state and adding water in an initial proportion of between 0.1% and 200.0%, this proportion being calculated relative to the whole of the two reactants V 2 O 5 and NH 4 H 2 PO 4 , wherein V 2 O 5 and NH 4 H 2 PO 4 are powders that comprise particles having a diameter d 50 of at most 100 μm, d 50 being a median diameter obtained from a volume size distribution determined by a laser particle size analyzer.
2. A process for preparing a phosphate of formula (NH 4 )(VO 2 )(HPO 4 ), the process consisting of stirring a mixture of V 2 O 5 and of NH 4 H 2 PO 4 , both in the solid state, and also of water, an initial proportion of which is between 0.1% and 200.0%, this proportion being calculated by weight relative to the whole of the two reactants V 2 O 5 and NH 4 H 2 PO 4 and not taking into account water optionally present initially in the two reactants, wherein V 2 O 5 and NH 4 H 2 PO 4 are powders that comprise particles having a diameter d 50 of at most 100 μm, d 50 being a median diameter obtained from a volume size distribution determined by a laser particle size analyzer.
3. The process as claimed in claim 1 , wherein the mixture of V 2 O 5 and of NH 4 H 2 PO 4 is present in an initial V/P ratio of between 0.9 and 1.1.
4. The process as claimed in claim 1 , wherein the mixture of V 2 O 5 and of NH 4 H 2 PO 4 is in a form of a powder, a paste or a fluid dispersion.
5. The process as claimed in claim 1 , wherein the mixture is subjected to reactive milling.
6. The process as claimed in claim 1 , wherein the process is conducted at a temperature of at most 100° C.
7. The process as claimed in claim 1 , wherein the phosphate of formula (NH 4 )(VO 2 )(HPO 4 ) contains less than 5% by weight of residual V 2 O 5 .
8. The process as claimed in claim 1 , wherein the phosphate of formula (NH 4 )(VO 2 )(HPO 4 ) contains less than 5% by weight of residual NH 4 H 2 PO 4 .
9. The process as claimed in claim 1 , wherein a product derived from the reaction is screened and/or dried to eliminate the water.
10. The process as claimed in claim 1 , wherein the initial proportion of water is:
between 0.5% and 200.0%.
11. A process for preparing VPO 4 from a phosphate of formula (NH 4 )(VO 2 )(HPO 4 ), obtained by the process of claim 1 , the process consisting of heating, to a temperature of at least 800° C., a reaction mixture comprising the phosphate in a confined environment so that NH 3 is released by the reaction mixture, and said NH 3 remains in contact with the reaction mixture.
12. The process as claimed in claim 11 , wherein carbon black is mixed with the phosphate of formula (NH 4 )(VO 2 )(HPO 4 ).
13. A process for preparing NVPF of formula Na 3 V 2 (PO 4 ) 2 F 3 , the process comprising:
preparing VPO 4 by heating a reaction mixture comprising a phosphate of formula (NH 4 )(VO 2 )(HPO 4 ), obtained by the process of claim 1 , to a temperature of at least 800° C. in a confined environment so that NH 3 is released by the reaction mixture, and said NH 3 or a portion thereof remains in contact with the reaction mixture, optionally in the presence of carbon black;
exposing, under an inert atmosphere, the_VPO 4 to sodium fluoride in a stoichiometric ratio of 1:1.5, VPO 4 :NaF, and optionally at least one hydrocarbon- and oxygen-containing compound, a source of elemental carbon, to temperature conditions suitable for obtaining NVPF.
14. The process as claimed in claim 1 wherein V 2 O 5 and NH 4 H 2 PO 4 are in the form of powders, the particles of which have a diameter d 50 of at most 50 μm, d 50 being the median diameter obtained from a volume size distribution determined by a laser particle size analyzer.
15. The process as claimed in claim 3 , wherein the mixture of V 2 O 5 and of NH 4 H 2 PO 4 is present in an initial V/P ratio of between 0.95 and 1.05.
16. The process as claimed in claim 7 , wherein the phosphate of formula (NH 4 )(VO 2 )(HPO 4 ) contains less than 1% by weight of residual V 2 O 5 .
17. The process as claimed in claim 8 , wherein the phosphate of formula (NH 4 )(VO 2 )(HPO 4 ) contains less than 1% by weight of residual NH 4 H 2 PO 4 .
18. The process as claimed in claim 10 , wherein the initial proportion of water is:
between 0.5% and 10.0%; or
between 80.0% and 150.0%.