Preparation method of vanadyl pyrophosphate
A technology of vanadyl pyrophosphate and vanadium source, applied in the field of vanadyl pyrophosphate, which can solve the problems of long cycle, waste, and shortened preparation cycle, and achieve the effects of easy operation, mild synthesis conditions, and shortened preparation time
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Embodiment 1
[0038] This embodiment discloses a preparation method of vanadyl pyrophosphate, comprising the following steps:
[0039] Step 1. Weigh ammonium metavanadate, phosphoric acid and water, according to V: P: water = 1:1.1:1.0; first put ammonium metavanadate in a beaker, add pure water to stir, stir well, add and weigh Phosphoric acid, stirred in a water bath at 85°C for 2 hours;
[0040] Step 2. After the reaction, filter and dry at 80°C for 4 hours to obtain the precursor NH 4 VO 2 HPO 4 ;
[0041] Step 3. Put the precursor in a crucible, put it into a muffle furnace for oxidative roasting at 440°C for 4 hours, and obtain VOPO 4 ;
[0042] Step 4. Put the VOPO 4 Put it into a tube furnace, feed nitrogen, and roast at 700° C. for 3 hours to obtain the target product. Through XRD detection, the product is vanadyl pyrophosphate with a purity of 99.3%.
[0043] The XRD pattern of the precursor of the present invention is as follows figure 1 As shown, the XRD pattern of the f...
Embodiment 2
[0045] This embodiment discloses a preparation method of vanadyl pyrophosphate, comprising the following steps:
[0046] Step 1. Weigh ammonium metavanadate, ammonium dihydrogen phosphate and water, press V:P:water=1:1.3:1.1; first put ammonium metavanadate in a beaker, add pure water to stir, and stir evenly Add the weighed ammonium dihydrogen phosphate, and stir in a water bath at 90°C for 1.5 hours;
[0047] Step 2. After the reaction, filter and dry at 100°C for 2 hours to obtain the precursor NH 4 VO 2 HPO 4 ;
[0048] Step 3. Put the precursor in a crucible, put it into a muffle furnace for oxidative roasting at 450°C for 2 hours, and obtain VOPO 4 ;
[0049] Step 4. Put the VOPO 4 Put it into a tube furnace, feed inert nitrogen gas, and roast at 750°C for 2 hours to obtain the target product, which is detected by XRD and is vanadyl pyrophosphate with a purity of 99.4%. .
Embodiment 3
[0051] This embodiment discloses a preparation method of vanadyl pyrophosphate, comprising the following steps:
[0052] Step 1. Weigh ammonium polyvanadate, diammonium hydrogen phosphate and water, press V:P:water=1:1.2:1.3; first put ammonium polyvanadate in a beaker, add pure water to stir, and stir evenly Add the weighed diammonium hydrogen phosphate, and stir in a water bath at a constant temperature of 95°C for 1 hour;
[0053] Step 2. After reacting for 2.5 hours, filter and dry at 100°C for 1.5 hours to obtain the precursor NH 4 VO 2 HPO 4 ;
[0054]Step 3. Put the precursor in a crucible, put it into a muffle furnace for oxidative roasting at 430°C for 3 hours, and obtain VOPO 4
[0055] Step 4. Put the VOPO 4 Put it into a tube furnace, feed inert nitrogen, and roast at 800° C. for 2 hours to obtain the target product. Through XRD detection, the product is vanadyl pyrophosphate with a purity of 99.6%.
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