A carbon-supported sodium vanadium fluorophosphate and its preparation and application
A technology of carbon-supported sodium vanadium phosphate and sodium vanadium phosphate, which is applied in the field of preparation of carbon-supported tetragonal sodium vanadium phosphate by hydrothermal method, can solve problems such as poor performance, achieve rapid and stable deintercalation, good application prospects, The effect of uniform shape and size
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specific Embodiment approach
[0031] The specific embodiment is prepared by the following steps,
[0032] 1) Add vanadium source and reducing agent to the solvent, the molar ratio of vanadium and reducing agent is 1:(0.9-1.1), the preferred ratio is 1:1; in addition, add a carbon source with a mass fraction of 3-10% to obtain a blend Solution, preferably with a mass fraction of 5-8%; wherein the solid content / solvent mass concentration is 15-35 mg / ml, preferably 20-30 mg / ml;
[0033] 2) React the blended solution in step 1) in a water bath environment of 60-90°C for 1-2h to obtain the precursor of the mixture; the preferred temperature range is 70-80°C; the solvent is removed by rotary evaporation of the precursor, and the rotary evaporation temperature is 50-90°C, the preferred temperature is 70-80°C;
[0034]3) Vacuum drying the dried mixture precursor in step 2) and grinding it into powder, the vacuum drying temperature is 90-130°C, preferably the vacuum drying temperature is 100-120°C, and the drying ...
Embodiment 1
[0038] Embodiment 1: (NH4VO3 precursor hydrothermal method prepares NaVPO 4 F)
[0039] Weigh 0.5850g NH4VO3 and 0.6303g oxalic acid dihydrate and add them to a 500mL beaker, add 100ml ethanol and 100ml deionized water, heat in a water bath at 70°C and stir for 1 hour to obtain a dark blue solution, evaporate the solvent to dryness, and place the resulting mixture at 120°C Dry in a positive air drying oven for 12 hours, pre-carbonize the obtained solid powder at 350°C for 5 hours in an argon atmosphere, and sinter at 750°C for 8 hours. Simultaneously as fluorine source and sodium source) and 0.5752g ammonium dihydrogen phosphate, add 0.1g sodium dodecylsulfonate in addition, add the weighed sample together in the PTFE liner of 100mL hydrothermal kettle, add 35mL of ethanol and 35mL of deionized water were placed in a blast drying oven at 180°C for 18h. The resulting mixed solution was centrifuged to remove the supernatant, washed 3 times with deionized water and ethanol and ...
Embodiment 2
[0040] Embodiment 2: (V 2 o 5 Precursor Hydrothermal Preparation of NaVPO 4 F)
[0041] Weigh 0.4550g V 2 o 5 Add 0.6303g oxalic acid dihydrate into a 500mL beaker, add 100ml ethanol and 100ml deionized water, heat in a water bath at 70°C and stir for 1 hour to obtain a dark blue solution. After evaporating the solvent, place the resulting mixture in a positive air drying oven at 120°C Dry for 12 hours, pre-carbonize the obtained solid powder at 350°C for 5 hours in an argon atmosphere, and sinter at 750°C for 8 hours. Sodium source) and 0.5752g ammonium dihydrogen phosphate, add 0.1g sodium dodecyl sulfonate in addition, add the sample that weighed into 100mL polytetrafluoroethylene liner of hydrothermal kettle together, add 35mL ethanol and 35mL to Ionized water was placed in a blast drying oven at 180°C for 18 hours. The resulting mixed solution was centrifuged to remove the supernatant, washed 3 times with deionized water and ethanol and centrifuged, and the obtained...
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