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Nanometer vanadyl phosphate as well as preparation method and application thereof

A vanadyl phosphate and nano-technology, applied in the field of nano-materials, can solve the problems of carbon deposition on the catalyst surface, reduced catalyst activity, excessive oxidation of raw materials, etc., and achieve the effects of small size, improved reactivity, and uniform particle size distribution

Inactive Publication Date: 2012-07-25
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Vanadyl phosphate is widely used in heterogeneous catalysis, and the conversion rate of raw materials in the catalytic reaction is high, but the temperature required for the catalytic reaction is often high, resulting in excessive oxidation of some raw materials. After a period of reaction, carbon deposits will occur on the surface of the catalyst , leading to a significant decrease in catalyst activity

Method used

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  • Nanometer vanadyl phosphate as well as preparation method and application thereof
  • Nanometer vanadyl phosphate as well as preparation method and application thereof
  • Nanometer vanadyl phosphate as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh out the V of 1.0 2 o 5 and 0.54 g of H 3 PO 4 Put it in a 25ml hydrothermal reactor with a Teflon lining, add 18ml of methanol and mix well; after sealing, put the hydrothermal reactor into a resistance furnace and heat it to 180°C, using its own pressure to keep the temperature constant Hydrothermal treatment for 24 hours; after the reaction, the reaction kettle was naturally cooled to room temperature; the blue-green product in the reaction kettle was separated by suction filtration and washed repeatedly with distilled water and ethanol respectively, and then placed in vacuum drying at 60°C for 4 hours to obtain the vanadyl phosphate precursor The precursor is calcined at 600°C in a nitrogen atmosphere in a resistance furnace for 2 hours, and cooled to room temperature to obtain nano-β-phase vanadyl phosphate in a granular hollow structure, with a particle size of 10-20nm and a wall thickness of 1-3nm.

Embodiment 2

[0025] According to the molar ratio of vanadium to phosphorus of 1:1, the total mass of 2.2g of V 2 o 4 and P 2 o 5 Put it in a 100ml hydrothermal reaction kettle, add 50ml of glycerol and 30ml of distilled water and mix well. After sealing, put the reaction kettle into a resistance furnace and heat it to 280°C. After constant temperature reaction for 2 hours, cool naturally to room temperature. Filter the product in the reaction kettle and wash it repeatedly with distilled water and ethanol respectively, then dry it in vacuum at 60°C for 5h to obtain the vanadyl phosphate precursor, calcinate the precursor in a resistance furnace at 700°C for 3h, cool to room temperature, and obtain granular Nano β-phase vanadyl phosphate with a hollow structure, the particle size is 20-30nm, and the wall thickness is 2-5nm.

Embodiment 3

[0027] According to the molar ratio of vanadium to phosphorus of 1:1, the V 2 o 3 and (NH 4 ) 3 PO 4 Place in a 100ml autoclave, then add 20ml of acetaldehyde, 20ml of ethanol and 40ml of distilled water and mix well. After sealing, put the reaction kettle into a resistance furnace and heat it to 120°C. After constant temperature reaction for 200h, naturally cool to room temperature. Filter the product in the reaction kettle and wash it repeatedly with distilled water and ethanol respectively, then dry it in vacuum at 60°C for 5 hours to obtain the vanadyl phosphate precursor, which is calcined in a resistance furnace at 400°C for 8 hours, and cooled to room temperature to obtain a granular Nano β-phase vanadyl phosphate with a hollow structure, the particle size is 10-30nm, and the wall thickness is 1-4nm.

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Abstract

The invention discloses nanometer vanadyl phosphate as well as a preparation method and application thereof. The beta-phase nanometer vanadyl phosphate is of a granular hollow structure; the particle diameter of nanometer vanadyl phosphate is 10-30nm; and the wall thickness of nanometer vanadyl phosphate is 1-5nm. The preparation method disclosed by the invention comprises the steps of: placing a vanadium source and a phosphorus source in a metal atom molar ratio of 1:1 in a pressure vessel, adding a solvent and uniformly mixing, heating to 120-280 DEG C after sealing to carry out solvent thermal reaction for 2-240 hours, filtering, washing and vacuum drying the product to obtain a vanadyl phosphate precursor; and calcining the precursor for 0.5-12 hours at a temperature of 400-900 DEG C, and cooling to room temperature to obtain nanometer vanadyl phosphate. The prepared nanometer vanadyl phosphate is small in size, uniform in particle diameter distribution, good in dispersity and large in specific surface area, simple in the preparation method and available in raw material. The nanometer vanadyl phosphate has very high catalytic activity and good reaction selectivity when being used for catalyzing ammoxidation of methyl aromatics to prepare aromatic nitrile, and reaction temperature is reduced compared with the vanadyl phosphate prepared by adopting a conventional method.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a nanovanadyl phosphate, its preparation method and application. Background technique [0002] Vanadyl Phosphate (VOPO 4 ) is based on C 4 Hydrocarbons are the most important catalysts for the production of maleic anhydride from raw materials. It was later found that it also has good catalytic activity for the ammoxidation of aromatic hydrocarbons. Martin et al. conducted in-depth research on unsupported vanadyl phosphate catalysts. They used α, β-VOPO 4 et al. carried out ammoxidation reactions for precursors and found that they had similar catalytic activity (Ch.Srilaxmi, N.Lingaiah, A.Hussain, P.S.Sai Prasad, K.V.Narayana, A.Martin, B.Lucke.Catalysis Communications, 2004, 5:199-203.). Vanadyl phosphate is widely used in heterogeneous catalysis, and the conversion rate of raw materials in the catalytic reaction is high, but the temperature required for the catalyti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/10C07C253/28C07C255/50C07C255/54C07D213/85
Inventor 谢光勇张爱清李金林
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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