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Nanometer chromium vanadate as well as preparation method and application thereof

A chromium vanadate and nanotechnology, which is applied in the field of nanomaterials, can solve the problems of carbon on the surface of the catalyst, reduced catalyst activity, excessive oxidation, etc., and achieves the effects of small size, improved reaction activity and low cost

Inactive Publication Date: 2012-07-11
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chromium vanadate prepared by these methods generally has a relatively large particle size, which is at the micron level or above. Therefore, in the ammoxidation catalysis, although the conversion rate of the raw material is high, the temperature required for the catalytic reaction is relatively high, generally at 380-430°C left or right, resulting in excessive oxidation of some raw materials, after a period of reaction, carbon deposits will occur on the surface of the catalyst, resulting in a significant reduction in catalyst activity

Method used

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  • Nanometer chromium vanadate as well as preparation method and application thereof
  • Nanometer chromium vanadate as well as preparation method and application thereof
  • Nanometer chromium vanadate as well as preparation method and application thereof

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Effect test

Embodiment 1

[0023] According to the molar ratio of vanadium to chromium of 1:1, the V 2 o 5 and CrO 3 Put it in a 100ml hydrothermal reaction kettle with polytetrafluoroethylene lining, then add 80ml of methanol and fully stir and mix evenly. After sealing, put the reaction kettle into a resistance furnace and heat it to 180°C. Cool to room temperature. After filtering the product in the reaction kettle and washing it repeatedly with distilled water and ethanol respectively, it was vacuum-dried at 60°C for 5 hours to obtain an amorphous chromium vanadate precursor, which was calcined in a resistance furnace at 600°C for 2 hours to obtain a rod-shaped nano Chromium vanadate.

Embodiment 2

[0025] According to the molar ratio of vanadium to chromium of 1:1, the V 2 o 4 and CrO 3 Put it in a 100ml hydrothermal reaction kettle, add 60ml of methanol and 20ml of distilled water and mix well. After sealing, put the reaction kettle into a resistance furnace and heat it to 160°C. After 48 hours of constant temperature reaction, it is naturally cooled 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 an amorphous chromium vanadate precursor, which is calcined in a resistance furnace at 700°C for 3 hours to obtain granular Nano chromium vanadate.

Embodiment 3

[0027] According to the molar ratio of vanadium to chromium of 1:1, the V 2 o 3 and Cr 2 o 3 Place in a 100ml hydrothermal reaction kettle, then add 50ml of glycerol and 30ml of distilled water and stir well to mix evenly. After sealing, put the reaction kettle into a resistance furnace and heat it to 200°C. After constant temperature reaction for 40h, 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 an amorphous chromium vanadate precursor, which is calcined in a resistance furnace at 650°C for 5 hours to obtain granular Nano chromium vanadate.

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Abstract

The invention discloses nanometer chromium vanadate as well as a preparation method and an application of the nanometer chromium vanadate. The nanometer chromium vanadate is in a particular or sticky structure, the particle size of the particular structure is 30 to 200n, the diameter of the sticky structure is 20 to 100nm, and the length of the sticky structure is 100 to 500nm. Vanadium sources and chromium sources are placed into a pressure container according to a metal atom mol ratio being 1:1, solvents are added, the materials are uniformly mixed, the temperature is raised to 120 to 300 DEG C after the sealing, the solvents take heat reaction for 2 to 200 hours, products are subjected to cooling, filtering, washing and vacuum drying, and precursors are obtained; and the precursors arecalcined for 0.1 to 10 hours at the temperature being 300 to 800 DEG C and are cooled to the room temperature, and the nanometer chromium vanadate is obtained. The prepared nanometer chromium vanadate has small dimension and uniform particle size distribution, the method is simple, raw materials are easy to obtain, and the cost is low. During the aromatic nitriles preparation through methyl aromatics ammoxidation reaction, the ammoxidation reaction temperature is 300 to 380 DEG C. Compared with the conventional chromium vanadate, the nanometer chromium vanadate has the advantages that the reaction temperature is obviously lowered, the selectivity is good, and in addition, the reaction activity is improved by 10 to 40 percent.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a nanometer chromium vanadate, its preparation method and application. Background technique [0002] Chromium vanadate (CrVO 4 ) is an important inorganic functional material, which is widely used in heterogeneous catalysis, battery materials, adsorption materials, sensors and other fields, such as oxidative dehydrogenation catalysts and ammoxidation catalysts in heterogeneous catalysis. There are several methods to synthesize chromium vanadate, as can synthesize orthorhombic or monoclinic chromium vanadate (M.Touboul, K.Melghit.J.Mater.Chem.1995, 5 (1): 147-150.), Takatoshi Tojo et al. 2 o 3 .nH 2 O and V 2 o 5 Tetragonal chromium vanadate was synthesized by mechanical grinding as raw material (Takatoshi Tojo, Qiwu Zhang, Fumio Saito. J. Solid State Chem. 2006, 179: 433-437). However, the chromium vanadate prepared by these methods generally has a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G37/00B01J23/26C07B43/08C07C253/28C07C255/54C07D213/85C07C255/51C07C255/50C07D241/24
Inventor 谢光勇张爱清李金林
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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