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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.

Active Publication Date: 2022-03-08
淄博市翔力致高新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above inventions start from the types of additives, preparation process, and physical characteristics of the vanadium-phosphorus-oxygen catalyst to improve the performance of the catalyst, but none of them improve the catalyst from the aspects of the local material composition on the catalyst surface and the influence of local trace elements.

Method used

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  • A kind of sodium-free vanadium phosphorus oxygen catalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

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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Abstract

A sodium-free vanadium-phosphorus-oxygen catalyst is improved from the aspects of local material composition and local trace elements on the surface of the vanadium-phosphorus-oxygen catalyst to obtain a sodium-free vanadium-phosphorus-oxygen catalyst, which makes the surface of vanadium-phosphorus oxide V 4+ The exposure of the species is more thorough, and the lattice oxygen ion O 2‑ The higher the formation rate, the higher the catalyst activity. In addition, the sodium-free environment on the surface of vanadium phosphorus oxide makes V 4+ The local charge density of the species and the acidity of the active center are more stable, and the target phase state intermediate structure formed between the n-butane molecule and the active center is more unitary, so that the selectivity of the catalyst is higher. The n-butane conversion activity of the sodium-free vanadium-phosphorus-oxygen catalyst of the present invention is greatly increased to over 94%, and at the same time, the selectivity of maleic anhydride is increased to over 71%; and the stability of different batches of reactions is better.

Description

technical field [0001] The invention relates to a sodium-free vanadium-phosphorus oxide catalyst and a preparation method thereof. The sodium-free vanadium-phosphorus oxide catalyst is suitable for the heterogeneous selective oxidation of short-chain alkanes, especially for the preparation of n-butane gas phase oxidation Maleic anhydride. Background technique [0002] Maleic anhydride, maleic anhydride for short, also known as maleic anhydride, is the third largest organic anhydride in the world after phthalic anhydride and acetic anhydride. Maleic anhydride is an important chemical intermediate. Due to the presence of conjugated maleic acid groups in the molecular structure, maleic anhydride has high activity and can undergo addition, self-polymerization, amidation, hydrogenation, alkylation, ester Chemical reactions such as oxidation, hydration, and redox. [0003] One of the most important uses of maleic anhydride is to produce unsaturated polyester resin (UPR) in the F...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/198C07D307/60
CPCC07D307/60B01J27/198
Inventor 侯俊琦马玉磊孙彪蒋强高步良程玉春谭永放徐兴忠
Owner 淄博市翔力致高新材料有限责任公司