Preparation method and application of lithium vanadium fluorophosphate
A technology for compounding lithium vanadium fluorophosphate and vanadium source is applied in the preparation/purification of carbon, chemical instruments and methods, phosphorus compounds, etc., and can solve problems such as side reactions and reduction of product purity.
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Embodiment 1
[0029] VPO 4 Preparation of LiVPO as precursor by @C 4 F@C
[0030] Mix 0.05mol ammonium metavanadate, 0.05mol ammonium dihydrogen phosphate, and an appropriate amount of citric acid in a beaker filled with 200ml of water, and stir mechanically at 80°C for 10 hours to obtain mixed solution A; the mass of citric acid is ammonium metavanadate 40% of mass;
[0031] Put the prepared mixed solution A in an oven at 100 degrees to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 750 ° C for 6 hours at a constant temperature, take it out and grind it to obtain black carbon-composite vanadium phosphate Powder (VPO 4 @C);
[0032] The resulting VPO 4 @C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and the mixed solution B is placed in a 180-degree reaction kettle for 48 hours of solvothermal reaction, suction filtered, and dried. LiVPO can be obtained by grinding...
Embodiment 2
[0034] V 2 o 3 Preparation of LiVPO as precursor by @C 4 F@C
[0035] Put 0.05mol ammonium metavanadate and an appropriate amount of citric acid into a beaker containing 200ml of water and mix them, and mechanically stir at 80°C for 10 hours to obtain a mixed solution A; the mass of citric acid is 50% of the mass of ammonium metavanadate;
[0036] Put the prepared mixed solution A in a 100-degree oven to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 750 ° C for 6 hours, take it out and pulverize it to obtain black V 2 o 3 @C powder;
[0037] The resulting V 2 o 3 Mix @C with 0.05mol ammonium fluoride, 0.05mol ammonium dihydrogen phosphate, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and place the mixed solution B in a reactor at 180 degrees for 48 hours of solvothermal reaction , suction filtration, drying, and grinding to obtain LiVPO 4 F@C powder;
Embodiment 3
[0039] VPO 4 @C is the precursor to prepare LiVPO 4 F@C
[0040] Mix 0.05mol ammonium metavanadate, 0.05mol ammonium dihydrogen phosphate, and an appropriate amount of citric acid in a beaker filled with 200ml of water, and stir mechanically at 80°C for 10 hours to obtain mixed solution A; the mass of citric acid is ammonium metavanadate 40% of mass;
[0041] Put the prepared mixed solution A in an oven at 100 degrees to dry for 12 hours, take it out and pulverize it, put it in a tube furnace with an argon atmosphere at 600 ° C for 10 hours at a constant temperature, take it out and pulverize it to obtain black carbon-composite vanadium phosphate Powder (VPO 4 @C);
[0042] The resulting VPO 4@C is mixed with 0.05mol ammonium fluoride, 0.05mol lithium hydroxide, and 80ml water to obtain a mixed solution B, and the mixed solution B is placed in a 180-degree reaction kettle for 48 hours of solvothermal reaction, suction filtered, and dried. LiVPO can be obtained by grindin...
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