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A kind of preparation method and application of vanadium phosphorus oxygen catalyst

A technology of vanadium phosphorus oxide and catalyst, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low conversion rate, easy over-oxidation, difficult conversion control, etc. Large specific surface area and the effect of increasing active sites

Active Publication Date: 2020-10-13
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the early catalysts were prepared by the aqueous phase method. At present, the preparation of VPO catalysts for industrial applications at home and abroad is by the organic phase method, but the catalysts prepared by this method still have problems such as small specific surface area, poor selectivity and easy over-oxidation.
Moreover, the catalyst obtained by the existing method has a limited number of active sites, the structure is easy to collapse, and the conversion rate is low; due to the complexity of the catalyst structure, the transformation between its phase states is often difficult to control, resulting in unstable catalyst performance

Method used

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  • A kind of preparation method and application of vanadium phosphorus oxygen catalyst
  • A kind of preparation method and application of vanadium phosphorus oxygen catalyst
  • A kind of preparation method and application of vanadium phosphorus oxygen catalyst

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preparation example Construction

[0018] The embodiment of the present invention provides a method for preparing a vanadium phosphorus oxygen catalyst, which includes the following steps:

[0019] S01: Put the vanadium source in a container, add a mixture of isobutanol and benzyl alcohol with a volume ratio of 2-6:1, heat up to 100-180°C for 2-8 hours, then cool to 30-80°C, add glucose , then add a phosphorus source into the container, heat up to 100-200°C and continue the reaction for 10-24 hours, the product is filtered, washed, and dried to obtain a vanadium-phosphorus-oxygen precursor, wherein the phosphorus in the phosphorus source and the vanadium source The molar ratio of vanadium is 0.8-1.5:1, the concentration of the vanadium pentoxide in the mixture of isobutanol and benzyl alcohol is 0.02g / mL-0.12g / mL, and the mass ratio of the vanadium source to glucose is 3 ~15:1;

[0020] S02: Calcining the vanadium phosphorus oxide precursor at a temperature of 350˜550° C. for 10˜24 hours, and cooling to obtain...

Embodiment 1

[0029] Weigh 20g V 2 o 5 Place in a 500mL three-neck flask, add a mixture of 160mL isobutanol and 40mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 4 hours, then cool down to 60°C, then add 2.0g of glucose, and then slowly drop 15.2mL 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue precipitate, and dry it in air at 120°C for 24 hours to obtain a catalyst precursor powder. The obtained catalyst precursor powder is compressed under a pressure of 15MPa, crushed, and 20-40 mesh catalyst particles are sieved. Afterwards, the catalyst particles were activated in situ from room temperature to 380°C at a rate of 5°C / min under a nitrogen atmosphere for 12 hours to obtain a vanadium-phosphorus-oxygen catalyst.

[0030] Weigh 4.5g of vanadium-phosphorus-oxygen catalyst and place it in a fixed-bed reactor with an inner diameter of 14mm for catalyst performance evaluation. 4 h 10 / O 2...

Embodiment 2

[0032] Weigh 20g V 2 o 5 Place in a 500mL three-neck flask, add a mixture of 160mL isobutanol and 40mL benzyl alcohol, stir and mix evenly, reflux at 135°C for 4 hours, then cool down to 60°C, then add 2.8g of glucose, and then slowly drop 15.2mL 85% H 3 PO 4 , and continued to reflux for 16 hours at a temperature of 135° C. Filter and wash with absolute ethanol to obtain a blue precipitate, and dry it in air at 120°C for 24 hours to obtain a catalyst precursor powder. The obtained catalyst precursor powder is compressed under a pressure of 15MPa, crushed, and 20-40 mesh catalyst particles are sieved. Afterwards, the catalyst particles were activated in situ from room temperature to 380°C at a rate of 5°C / min under a nitrogen atmosphere for 12 hours to obtain a vanadium-phosphorus-oxygen catalyst.

[0033] Weigh 4.5g of vanadium-phosphorus-oxygen catalyst and place it in a fixed-bed reactor with an inner diameter of 14mm for catalyst performance evaluation. 4 h 10 / O 2...

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Abstract

The invention relates to a vanadium phosphorus oxide catalyst, a preparation method and applications thereof. The preparation method comprises: placing a vanadium source in a container, adding a mixing liquid comprising isobutanol and benzyl alcohol according to a volume ratio of 2-6:1, heating to a temperature of 100-180 DEG C, carrying out a reaction for 2-8 h, cooling to a temperature of 30-80DEG C, adding glucose, adding a phosphorus source to the container, heating to a temperature of 100-200 DEG C, continuously carrying out a reaction for 10-24 h, filtering the product, washing the product, and drying to obtain a vanadium phosphorus oxide precursor, wherein a molar ratio of the phosphorus in the phosphorus source to the vanadium in the vanadium source is 0.8-1.5:1, the concentrationof vanadium pentoxide in the mixture of isobutanol and benzyl alcohol is 0.02-0.12 g / mL, and a mass ratio of the vanadium source to the glucose is 3-15:1; and calcining the vanadium phosphorus oxideprecursor for 10-24 h at a temperature of 350-550 DEG C, and cooling to obtain the vanadium phosphorus oxide catalyst. According to the present invention, the vanadium phosphorus oxide catalyst prepared by the method has large specific surface area; the preparation method is simple, and is suitable for large-scale preparation; and with the application of the vanadium phosphorus oxide catalyst in the maleic anhydride preparation reaction by catalyzing the selective oxidation of n-butane, the problems of low reaction yield, poor selectivity and the like of the maleic anhydride preparation reaction through the selective oxidation of n-butane in the prior art are improved.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and in particular relates to a preparation method and application of a vanadium-phosphorus-oxygen catalyst. Background technique [0002] Vanadium-phosphorus-oxygen catalyst is a composite oxide catalyst with defective structure, which is composed of three elements V, P, and O. Therefore, it has good electron and oxygen transport functions, and has a wide range of applications in the field of catalysis and electrochemistry. At the same time, the catalyst is currently the only catalyst for the selective oxidation of low-carbon alkanes that has been industrialized. Its crystal structure is relatively complex, and its active phase is also different for different reactions, mainly (VO) 2 P 2 o 7 、VOPO 4 etc. Different preparation conditions often lead to different crystal structures, and their catalytic performance and microscopic morphology are also quite different. Factors affecting its struc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/198C07D307/60
CPCB01J27/198C07D307/60
Inventor 刘瑞霞南琳琳代飞张瑞锐贺滨李自航李雅婧张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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