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Supported-type vanadium-phosphorus oxide, and preparation method and applications thereof

A vanadium phosphorus oxide, supported technology, applied in chemical instruments and methods, chemical/physical processes, organic chemistry, etc., to achieve high porosity, many surface active centers, uniform and stable pore structure

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In the prior art, using the principle of reaction engineering, in the process of catalyst preparation, interphase transfer and microscopic mixing are strengthened to prepare nano-scale small grain size, high activity supported VPO catalyst with high specific surface area, which has not been reported so far.

Method used

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  • Supported-type vanadium-phosphorus oxide, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] exist figure 1 In the impingement flow reactor shown, add isobutanol and benzyl alcohol mixed solution 649mL, isobutanol / benzyl alcohol volume ratio 10:1, vanadium pentoxide 29.53g, start the impingement flow reactor, make the stirring blade rotate When it reaches 1500r / min, the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 110±2°C, carry out the reflux reaction, and keep the reflux time for 4 hours. Add 72g of nano silicon dioxide, reflux for 4 hours; then add 44.7g of phosphoric acid with a concentration of 85wt%, continue to reflux for 4 hours, and the reaction ends. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed three times with a small amount of isobutanol, and then the filter cake was placed in an enamel tray and dried naturally at room temperature, dried in an oven at 105°C for 8 hours, and finally placed in a muffle furn...

Embodiment 2

[0055] exist figure 1 In the impingement flow reactor shown, add 649mL of isobutanol and benzyl alcohol mixture, the volume ratio of isobutanol / benzyl alcohol is 15:1, 29.53g of vanadium pentoxide, 0.3g of ferric nitrate hexahydrate, and 0.5 g of zirconium nitrate, start the impingement flow reactor, make the rotation speed of the stirring blade reach 2500r / min, and the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 100±2°C, carry out the reflux reaction, keep the reflux time for 4 hours, add 68g of nano-silicon dioxide, and reflux for 4 hours; then add 34.98g of phosphoric acid with a concentration of 100%, and the phosphorus / vanadium molar ratio is 1.1 , continue to reflux for 4 hours, and the reaction ends. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was washed three times with a small amount of isobutanol, and then the filter cake was place...

Embodiment 3

[0060] exist figure 1 In the impingement flow reactor shown, add isobutanol and benzyl alcohol mixed solution 649mL, isobutanol / benzyl alcohol volume ratio 20:1, vanadium pentoxide 29.53g, start the impingement flow reactor, make the stirring blade rotate When it reaches 3500r / min, the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 97±2°C, carry out the reflux reaction, keep the reflux time for 2 hours, add 94g of nano-silicon dioxide, and reflux for 4 hours; then add 33.47g of phosphoric acid with a concentration of 95%, and the phosphorus / vanadium molar ratio is 1.0 , continue to reflux for 4 hours, and the reaction ends. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isobutanol three times, then the filter cake was placed in an enamel tray and dried naturally at room temperature, dried in an oven at 100°C for 8...

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Abstract

The invention discloses a supported-type vanadium-phosphorus oxide, and a preparation method thereof. Grain size of the supported-type vanadium-phosphorus oxide is less than 150nm, and by volume, particles with a grain size of 50 to 90nm accounts for 6 to 12%, particles with a grain size of 90 to 120nm accounts for 45 to 79%, and particles with a grain size more than 120nm accounts for 10 to 42%. The supported-type vanadium-phosphorus oxide is prepared by using an immersion circulating type impinging stream reactor. Reaction efficiency of the preparation method is high; reaction time is shortened; mass transfer effect is excellent; and the obtained supported-type vanadium-phosphorus oxide is small in grain size, concentrate in grain size distribution, and large in specific surface area. A catalyst prepared by taking the supported-type vanadium-phosphorus oxide as a precursor is used for catalytic preparation of maleic anhydride via oxidation of n-butane, n-butane molar conversion rate is high, and maleic anhydride selectivity is excellent.

Description

technical field [0001] The invention relates to a supported vanadium-phosphorus oxide and a preparation method thereof. The supported vanadium-phosphorus oxide is suitable for use as a catalyst precursor in the reaction of n-butane oxidation to maleic anhydride. Background technique [0002] Maleic anhydride, referred to as maleic anhydride, also known as maleic anhydride, is an important organic chemical raw material and fine chemical product. It is currently the third largest anhydride in the world after phthalic anhydride and acetic anhydride. Its specific applications mainly include Production of unsaturated polyester resins, alkyd resins, pesticides, pharmaceuticals, coatings, inks, lubricating oil additives, paper chemicals, textile finishing agents, food additives and surfactants, etc. In addition, maleic anhydride can also be used as a raw material to produce a series of fine chemical products with wide applications, such as 1,4-butanediol, tetrahydrofuran, maleic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/00C07D307/60
Inventor 薛冬乔凯王海波宋丽芝勾连科
Owner CHINA PETROLEUM & CHEM CORP
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