A kind of vanadium phosphorus oxide and preparation method thereof

A technology of vanadium phosphorus oxide and vanadium pentoxide, which is applied in the direction of phosphorus compounds, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of increasing catalyst manufacturing costs, insufficient particle size concentration, and uneven grain size distribution. Achieve the effects of stable catalyst structure, concentrated particle size distribution, and shortened reaction time

Active Publication Date: 2017-02-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large amount of polyethylene glycol dispersant is added in the preparation process of this method, and the obtained product has the problems of uneven grain size distribution and insufficient concentration of particle size, and the addition of a large amount of polyethylene glycol also has the disadvantage of additionally increasing the catalyst manufacturing cost
Although the reaction performance of the vanadium phosphorus oxygen catalyst is better, the activity and selectivity of the catalyst still need to be further improved.

Method used

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  • A kind of vanadium phosphorus oxide and preparation method thereof
  • A kind of vanadium phosphorus oxide and preparation method thereof
  • A kind of vanadium phosphorus oxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] exist figure 1 In the impingement flow reactor shown, add isobutanol, benzyl alcohol mixture 500mL, isobutanol / benzyl alcohol volume ratio 10:1, silane coupling agent A-147 0.29g, start the impingement flow reactor, make stirring The rotation speed of the paddle reaches 1500r / min, and the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 110±2°C, mix 29.53g of vanadium pentoxide and 149mL of isobutanol and benzyl alcohol in a FSH-2 high-speed homogenizer to form a suspension, so that the concentration of 85% Phosphoric acid 44.7g and the above-mentioned suspension were added into the reactor from two inlets of the impingement 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 iso...

Embodiment 2

[0054] exist figure 1 In the impingement flow reactor shown, add 500mL of isobutanol and benzyl alcohol mixture, the volume ratio of isobutanol / benzyl alcohol is 15:1, 0.29g of silane coupling agent A-151, and 0.3g of ferric nitrate hexahydrate , zirconium nitrate 0.5g, start the impingement flow reactor, so that the rotation speed of the stirring blade reaches 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, mix 29.53g of vanadium pentoxide and 149mL of isobutanol and benzyl alcohol in a FSH-2 high-speed homogenizer to form a suspension, so that the concentration of 100% Phosphoric acid 34.98g and the above-mentioned suspension were added into the reactor from two inlets of the impingement 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 wa...

Embodiment 3

[0058] exist figure 1 In the impingement flow reactor shown, add isobutanol, benzyl alcohol mixed solution 500mL, isobutanol / benzyl alcohol volume ratio 20:1, silane coupling agent A-147 0.44g, start impingement flow reactor, make stirring The rotation speed of the paddle reaches 3500r / min, and the reaction liquid passes through the guide tube to form an impingement flow. Raise the reaction temperature and keep it at 97±2°C, mix 29.53g of vanadium pentoxide and 149mL of isobutanol and benzyl alcohol in a FSH-2 high-speed homogenizer to form a suspension, so that the concentration of 95% Phosphoric acid 33.47g and the above-mentioned suspension were added into the reactor from two inlets of the impingement 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 isobutanol t...

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Abstract

The present invention discloses a vanadium-phosphorus oxide and a preparation method thereof, wherein the grain size of the 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 less than 15 nm is 9-15%, the content of the particles with the grain size of 15-30 nm is 62-80%, and the content of the particles with the grain size of 30-100 nm is 11-23%. According to the present invention, the nanometer vanadium-phosphorus oxide is prepared by using an immersion circulating type impinging stream reactor, and a silane coupling agent is added to obtain the vanadium-phosphorus oxide with characteristics of small grain, concentrated grain size distribution and large specific surface area; and the octahedron structure of the vanadium-phosphorus oxide crystal phase is regular, the active crystal face (020 crystal face) exposure is large, the activity of the catalyst prepared from the precursor is high, and with the application of the vanadium-phosphorus oxide of the present invention to catalyze the maleic anhydride preparation reaction through the n-butane oxidation, the n-butane molar conversion rate can achieve 90-95%, and the maleic anhydride selectivity can achieve 75-88 mol%.

Description

technical field [0001] The invention relates to a vanadium-phosphorus oxide and a preparation method thereof. The vanadium-phosphorus oxide is suitable as a catalyst precursor for preparing maleic anhydride by n-butane oxidation. 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), as well as pesticides, coatings, glass fiber reinforced plastics, lubricating oil additives, paper chemistry Product additives, surfactants, etc. The advent of the new method of maleic anhydride esterification and low-pressure hydrogenation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/198C07D307/60C01B25/37C01B25/42
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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