Vanadium-phosphorus-oxygen catalyst, and preparation method thereof

A technology of vanadium phosphorus oxide and catalyst, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of increasing catalyst manufacturing cost, uneven grain size distribution, and insufficient concentration of particle size distribution, etc. Achieve the effects of promoting micro-mixing, concentrating grain size distribution, and uniform distribution of active centers

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The preparation process of this method adds a large amount of polyethylene glycol dispersant, and the obtained product has the problems of uneven grain size distribution and insufficient concentration of particle size distribution, and there is a deficiency that the raw material polyethylene glycol increases 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.
[0013] In the prior art, the principle of reaction engineering is used to improve the interphase mass transfer efficiency and enhance the mass transfer coefficient during the preparation of the catalyst precursor, so as to obtain nano-sized vanadium phosphorus oxides with small grain size and high specific surface area. The research on the preparation of highly active vanadium-phosphorus-oxygen catalysts for precursors has not been reported so far

Method used

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  • Vanadium-phosphorus-oxygen catalyst, and preparation method thereof
  • Vanadium-phosphorus-oxygen catalyst, and preparation method thereof

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preparation example Construction

[0045] (2) Preparation of vanadium phosphorus oxygen catalyst

[0046] 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.

[0047] 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 vanadyl pyrophosphate ((VO 2 ) 2 P 2 o 7 )Mutually.

[0048] 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 columna...

Embodiment 1

[0055] 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, keep the reflux time for 4 hours, then add 44.7g of phosphoric acid with a concentration of 85%, 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 furnace. Calcined at 250°C for 5 hours to obtain dark brown van...

Embodiment 2

[0059] 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, then add 34.98g of phosphoric acid with a concentration of 100%, 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 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 ...

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Abstract

The invention discloses a vanadium-phosphorus-oxygen catalyst, and a preparation method thereof. According to the preparation method, a nano vanadium phosphorus oxide is taken as a precursor, is subjected to activating and then moulding, or is subjected to moulding and then activating so as to obtain the vanadium-phosphorus-oxygen catalyst; grain size of the nano vanadium phosphorus oxide is less than 100nm, and by volume, particles with a grain size of 30 to 50nm accounts for 7 to 14%, particles with a grain size of 50 to 70nm accounts for 54 to 79%, and particles with a grain size more than 70nm accounts for 7 to 39%. According to the vanadium-phosphorus-oxygen catalyst prepared by taking the nano vanadium phosphorus oxide as a precursor, octahedral structure of (VO)2P2O7 is neater, catalyst structure is stable, and catalytic activity and catalyst stability are higher. When the vanadium-phosphorus-oxygen catalyst is used for catalytic preparation of maleic anhydride via oxidation of n-butane, n-butane conversion rate reaches 87 to 95mol%, and maleic anhydride selectivity reaches 72 to 84mol%.

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 n-butane oxidation to maleic anhydride. 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 fatification and low-pressure hydrogenation to produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J27/199C07D307/60
Inventor 王海波勾连科宋丽芝薛冬侯学伟范丹丹
Owner CHINA PETROLEUM & CHEM CORP
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