A kind of sodium-free vanadium phosphorus oxygen catalyst and preparation method thereof
A technology of vanadium phosphorus oxides and catalysts, used in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc.
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Embodiment 1
[0036] Weigh 19g sodium-free type V 2 o 5 Powder (sodium ion content 5-0ppm), put into a three-necked flask, add 200mL isobutanol and 50mL benzyl alcohol, heat to reflux at a specific stirring rate, reflux for 6h, drop slowly after dropping to 80°C 100wt% industrial grade phosphoric acid 27.6g, then heated to reflux, reacted for 6h and cooled naturally. Suction filtration was performed after the temperature of the slurry dropped to room temperature, washed with isobutanol, dried at 120°C for 5 hours, and then calcined at 260°C for 5 hours to obtain the VPO catalyst precursor. Add 3% graphite to the obtained precursor powder and mix evenly, punch into pieces, and then place it in an atmosphere oven for activation. The activation atmosphere is controlled to be 50% / 25% / 25% of air / water vapor / nitrogen, and the heating rate is 3 °C / min, the temperature was raised to 430 °C, and kept at 430 °C for 6 hours to obtain the finished VPO catalyst.
[0037] Take 3mL of VPO catalyst, dil...
Embodiment 2
[0039] Weigh 19g industrial grade V 2 o 5 Powder, put into a three-necked flask, add 200mL isobutanol and 50mL benzyl alcohol, heat to reflux at a specific stirring rate, reflux for 6h, and slowly add 27.6g of 100wt% sodium-free phosphoric acid (sodium ion content 5 ~0ppm), then heated to reflux, reacted for 6h and cooled naturally. Suction filtration was performed after the temperature of the slurry dropped to room temperature, washed with isobutanol, dried at 120°C for 5 hours, and then calcined at 260°C for 5 hours to obtain the VPO catalyst precursor. Add 3% graphite to the obtained precursor powder and mix evenly, punch into pieces, and then place it in an atmosphere oven for activation. The activation atmosphere is controlled to be 50% / 25% / 25% of air / water vapor / nitrogen, and the heating rate is 3 °C / min, the temperature was raised to 430 °C, and kept at 430 °C for 6 hours to obtain the finished VPO catalyst.
[0040] Take 3mL of VPO catalyst, dilute it with quartz sa...
Embodiment 3
[0042] Weigh 19g sodium-free type V 2 o 5 Powder (sodium ion content 5-0ppm), put into a three-necked flask, add 200mL of isobutanol and 50mL of benzyl alcohol, heat to reflux at a specific stirring rate, reflux for 6h, and slowly add 100wt% sodium-free type Phosphoric acid 27.6g (sodium ion content 5-0ppm), then heated up to reflux, reacted for 6h and cooled naturally. Suction filtration was performed after the temperature of the slurry dropped to room temperature, washed with isobutanol, dried at 120°C for 5 hours, and then calcined at 260°C for 5 hours to obtain the VPO catalyst precursor. Add 3% graphite to the obtained precursor powder and mix evenly, punch into pieces, and then place it in an atmosphere oven for activation. The activation atmosphere is controlled to be 50% / 25% / 25% of air / water vapor / nitrogen, and the heating rate is 3 °C / min, the temperature was raised to 430 °C, and kept at 430 °C for 6 hours to obtain the finished VPO catalyst.
[0043] Take 3mL of ...
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