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Hydrothermal method for preparing triclinic-phase FeVO4 micro particles

A technology of micron particles and triclinic phase, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., to achieve the effect of simple experimental steps, convenient operation, and regular appearance of target products

Inactive Publication Date: 2010-12-15
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there are no literature and patent reports on the successful synthesis of triclinic FeVO 4 Mesoporous microrods or triclinic FeVO 4 non-porous microblock

Method used

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  • Hydrothermal method for preparing triclinic-phase FeVO4 micro particles
  • Hydrothermal method for preparing triclinic-phase FeVO4 micro particles
  • Hydrothermal method for preparing triclinic-phase FeVO4 micro particles

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: under stirring condition, 10mmol Fe(NO 3 ) 3 9H 2 O was added to 50mL HNO 3 Solution (concentration is 2mol / L), then add 10mmol NH 4 VO 3 , after being completely dissolved, a transparent brownish-yellow solution is obtained, and the pH value of the mixed solution is adjusted to 4 with 14wt% ammonia water, and the resulting suspension is transferred to an autoclave equipped with a polytetrafluoroethylene liner (volume is 100mL) (Volume filling degree 80%) was treated at a constant temperature of 180 ° C for 6 h, filtered by suction, washed with deionized water and absolute ethanol three times and dried at 100 ° C for 12 h, and then placed in a muffle furnace at 1 ° C / The rate of min is increased from room temperature to 600 °C and maintained at this temperature for 6 h, that is, the triclinic phase FeVO 4 Mesoporous microrods.

Embodiment 2

[0021] Embodiment 2: under stirring condition, 10mmol Fe(NO 3 ) 3 9H 2 O was added to 50mL HNO 3 Solution (concentration is 2mol / L), then add 10mmol NH 4 VO 3 , after being completely dissolved, a transparent brown-yellow solution is obtained, and the pH value of the mixed solution is adjusted to 7 with 14wt% ammonia water, and the resulting suspension is transferred to an autoclave equipped with a polytetrafluoroethylene liner (a volume of 100 mL) (Volume filling degree 80%) was treated at a constant temperature of 180 ° C for 6 h, filtered by suction, washed with deionized water and absolute ethanol three times and dried at 100 ° C for 12 h, and then placed in a muffle furnace at 1 ° C / The rate of min is increased from room temperature to 600 °C and maintained at this temperature for 6 h, that is, the triclinic phase FeVO 4 Mesoporous microrods.

Embodiment 3

[0022] Embodiment 3: under stirring condition, 10mmol Fe(NO 3 ) 3 9H 2 O was added to 50mL HNO 3 Solution (concentration is 2mol / L), then add 10mmol NH 4 VO 3 , after being completely dissolved, a transparent brownish-yellow solution is obtained, and the pH value of the mixed solution is adjusted to 4 with 14wt% ammonia water, and the resulting suspension is transferred to an autoclave equipped with a polytetrafluoroethylene liner (volume is 100mL) (Volume filling degree 80%) was treated at a constant temperature of 180 ° C for 2 h, filtered by suction, washed with deionized water and absolute ethanol three times and dried at 100 ° C for 12 h, and then placed in a muffle furnace under an air atmosphere at 1 ° C / The rate of min is increased from room temperature to 600 °C and maintained at this temperature for 6 h, that is, the triclinic phase FeVO 4 Non-porous micron block.

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Abstract

The invention discloses a hydrothermal method for preparing triclinic-phase FeVO4 micro particles. The method comprises the following steps of: mixing ferric nitrate nonahydrate, ammonium metavanadate and nitric acid solution in a molar ratio of 1:1:10, adjusting the pH value to 4 or 7 by using 14 weight percent of aqueous ammonia, transferring the solution to a stainless steel self-pressure kettle of which a lining is made of polytetrafluoroethylene, treating the solution for 2 or 6 hours at the constant temperature of 180 DEG C, filtering the solution, washing and drying the filtrate, and heating the filtrate to 600 DEG C from room temperature at the speed of 1 DEG C per minute under air atmosphere and keeping the temperature for 6 hours, wherein when the pH is 4 or 7 and the hydrothermal treatment is performed for 6 hours, the obtained product is a triclinic-phase FeVO4 mesoporous micro bar, and when the pH is 4 and the hydrothermal treatment is performed for 2 hours, the obtained product is a triclinic-phase FeVO4 imperforate micro block. The method is convenient to operate, the raw materials are cheap, and the topography, crystalline phase structure and specific surface area of the target product particles are controllable.

Description

technical field [0001] The invention relates to a preparation technology of a solid material with regular appearance, in particular to the preparation of triclinic phase FeVO 4 The hydrothermal method of micron particles belongs to the technical field of solid catalytic materials. Background technique [0002] Iron vanadate is an n-type semiconductor material with unique electrical, magnetic and catalytic properties, and has broad application prospects in the oxidation of hydrocarbons and lithium battery electrode materials. Compared with non-porous iron vanadate, mesoporous iron vanadate has the advantages of large specific surface area and high porosity, so its performance is superior and its application is more extensive. [0003] Ferric vanadate mainly has four crystal forms, namely triclinic phase, orthorhombic (I), orthorhombic (II) and monoclinic phase. Among them, triclinic ferric vanadate has attracted much attention due to its high thermal stability and catalytic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
Inventor 戴洪兴蒋海燕张磊邓积光刘雨溪石凤娟王芳何洪
Owner BEIJING UNIV OF TECH
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