Vanadium-phosphorus oxide catalyst for preparing maleic anhydride through cyclohexane oxidation, and preparation method thereof

A vanadium phosphorus oxide and catalyst technology, which is applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., to achieve uniform distribution of active centers, good reactivity, and good maleic anhydride selectivity.

Active Publication Date: 2015-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In the prior art, the impinging flow reaction is used to improve the interphase mass transfer efficiency and enhance the mass transfer coefficient during the preparation of the catalyst precursor (vanadium phosphorus oxide). Alcohol and changing the reaction temperature, rotation speed, etc.) to obtain vanadium phosphorus oxide with small grain size and suitable grain size distribution, and use the precursor to prepare high activity vanadium phosphorus oxide catalyst for the process of cyclohexane oxidation to maleic anhydride research has not been reported so far

Method used

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  • Vanadium-phosphorus oxide catalyst for preparing maleic anhydride through cyclohexane oxidation, and preparation method thereof
  • Vanadium-phosphorus oxide catalyst for preparing maleic anhydride through cyclohexane oxidation, and preparation method thereof
  • Vanadium-phosphorus oxide catalyst for preparing maleic anhydride through cyclohexane oxidation, and preparation method thereof

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preparation example Construction

[0050] (2) Preparation of vanadium phosphorus oxygen catalyst

[0051] Step (1) The obtained vanadium phosphorus oxide is first formed to obtain a vanadium phosphorus oxygen catalyst intermediate, and then activated; or the obtained vanadium phosphorus oxide is first activated to obtain a vanadium phosphorus oxygen catalyst intermediate, and then formed to obtain vanadium phosphorus oxygen catalyst.

[0052] The shape of the obtained vanadium-phosphorus-oxygen catalyst can be shapes such as pressed sheet, sphere, extruded bar, and the phase of matter of the catalyst is mainly super vanadyl phosphate ((VO 2 ) 2 P 2 o 7 )Mutually.

[0053] The above-mentioned molding process generally includes: adding vanadium phosphorus oxide powder (or activated vanadium phosphorus catalyst intermediate) to graphite powder with a mass fraction of 3% to 5%, after mixing thoroughly, using a rotary tablet press, Properly adjust the impact strength, extrude into a certain shape, such as colum...

Embodiment 1

[0060] exist figure 1 In the impingement flow reactor shown, add 500 mL of isoamyl alcohol, start the impingement flow reactor, and make the rotation speed of the stirring blade reach 1500 r / min, and the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 130±2°C, beat 29.53g of vanadium pentoxide and 149mL of isoamyl alcohol in a FSH-2 high-speed homogenizer to form a suspension, and make 44.7g of phosphoric acid with a concentration of 85% and the above The suspension was added into the reactor from two inlets of the impinging flow reactor at a certain flow acceleration rate, and the reaction time was maintained for 6 hours to complete the reaction. 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...

Embodiment 2

[0064] exist figure 1 In the impingement flow reactor shown, add 500 mL of isoamyl alcohol, 0.3 g of ferric nitrate hexahydrate, and 0.5 g of zirconium nitrate. The deflector creates impingement flow. Raise the reaction temperature and keep it at 135±2°C, beat 29.53g of vanadium pentoxide and 149mL of isoamyl alcohol in a FSH-2 high-speed homogenizer to form a suspension, and make 34.98g of phosphoric acid with a concentration of 100% and the above The suspension was added into the reactor from two inlets of the impinging flow reactor at a certain flow acceleration rate, and the reaction time was maintained for 8 hours to complete the reaction. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isoamyl alcohol three times, then the filter cake was placed in an enamel dish and dried naturally at room temperature, dried in an oven at 100°C for 10 hours, and finally dried in a muffle furnace. ...

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Abstract

The present invention discloses a vnadium-phosphorus oxide catalyst for preparing maleic anhydride through cyclohexane oxidation, and a preparation method thereof. According to the vanadium-phosphorus oxide catalyst, a nanometer vanadium-phosphorus oxide is adopted as a precursor, and is sequentially subjected to activation and forming or forming and activation to prepare the vanadium-phosphorus oxide catalyst, wherein the grain size of the nanometer vanadium-phosphorus oxide is less than 100 nm, and the grain size distribution adopting the volume as the benchmark is that the content of the particles with the grain size of 10-70 nm is 7-25%, the content of the particles with the grain size of 70-85 nm is 60-88%, and the content of the particles with the grain size of more than 85 nm is 5-15%; in the catalyst prepared by adopting the nanometer vanadium-phosphorus oxide as the precursor, the octahedron structure of the (VO)2P2O7 crystal phase is regular, the catalyst structure is stable, and the catalysis activity and the catalyst stability are high; and with the application of the catalyst of the present invention to catalyze the maleic anhydride preparation reaction through the cyclohexane oxidation, the cyclohexane conversion rate can achieve 57-70 mol%, and the maleic anhydride selectivity can achieve 65-74 mol%.

Description

technical field [0001] The invention relates to a vanadium-phosphorus-oxygen catalyst and a preparation method thereof. The catalyst is suitable for the catalytic reaction process of cyclohexane oxidation to prepare maleic anhydride and acetic acid. Background technique [0002] Maleic anhydride, also known as maleic anhydride for short, is an important organic chemical raw material and the third largest organic anhydride in the world after phthalic anhydride and acetic anhydride. It is widely used in petrochemical, food processing, and pharmaceutical industries. , Building materials and other industries. Its specific applications include the manufacture of unsaturated polyester resins, alkyd resins, maleic acid (maleic acid), fumaric acid (fumaric acid), and pesticides, coatings, glass fiber reinforced plastics, lubricating oil additives, paper chemistry Product additives, surfactants, etc. The advent of the new method of maleic anhydride fatification and low-pressure hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/10C07D307/60B82Y40/00B82Y30/00
Inventor 王海波宋丽芝勾连科薛冬侯学伟范丹丹
Owner CHINA PETROLEUM & CHEM CORP
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