Method for preparing vanadium trioxide powder by using one-step hydrothermal method

A vanadium trioxide and hydrothermal technology, applied in the direction of vanadium oxide, etc., can solve environmental pollution and other problems, and achieve the effects of easy control of reaction conditions, low reaction temperature and good crystallinity

Active Publication Date: 2019-02-01
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing ammonium metavanadate and ammonium polyvanadate by ammonium salt precipitation, a large amount of ammonia nitrogen wastewater will be produced, and the process of thermally decomposing ammonium metavanadate and ammonium polyvanadate to prepare vanadium pentoxide will release a large amount of ammonia gas , these wastewater and waste gas will cause serious pollution to the environment; in addition, using ammonium metavanadate or ammonium polyvanadate as raw material, a large amount of ammonia gas will be decomposed in the process of preparing vanadium trioxide, and unreacted ammonia The release of gas into the atmosphere will also pollute the environment
Therefore, there is serious problem of environmental pollution in existing vanadium trioxide preparation technology

Method used

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  • Method for preparing vanadium trioxide powder by using one-step hydrothermal method
  • Method for preparing vanadium trioxide powder by using one-step hydrothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Weigh 1.218g Na 3 VO 4 Dissolved in 40mL of water under the action of magnetic stirring to obtain a clear and transparent solution, and then added 1.67g of C 2 h 2 o 4 2H 2 O, the color of the solution turned yellow. Transfer the reaction solution to a high-pressure reactor, heat it to 270°C, react for 48 hours, stop heating, and when the temperature of the reactor drops to room temperature, centrifuge to separate the solid powder and dry it to obtain vanadium trioxide micron powder. 10-20 μm.

Embodiment 2

[0039] Weigh 1.218g Na 3 VO 4 Dissolved in 40mL of water under the action of magnetic stirring to obtain a clear and transparent solution, and then added 1.67g of C 2 h 2 o 4 2H 2 O, the color of the solution turned yellow. Transfer the reaction solution to a high-pressure reactor, heat it to 300°C, react for 6 hours, stop heating, and when the temperature of the reactor drops to room temperature, centrifuge to separate the solid powder and dry it to obtain vanadium trioxide micron powder. 1 to 10 μm.

Embodiment 3

[0041] Weigh 1.218g Na 3 VO 4 Dissolved in 40mL of water under the action of magnetic stirring to obtain a clear and transparent solution, and then added 3.34g of C 2 h 2 o 4 2H 2 0, the solution color turns yellow, then adds 0.165g tungstic acid wherein. Transfer the reaction solution to a high-pressure reactor, heat it to 200°C, react for 48 hours, stop heating, and when the temperature of the reactor drops to room temperature, centrifuge to separate the solid powder and dry it to obtain micron powder of tungsten-doped vanadium trioxide , the particle size is 5-20 μm.

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Abstract

The invention relates to a method for preparing vanadium trioxide powder by using a one-step hydrothermal method, wherein the method comprises: adding a reducing agent to a vanadium source aqueous solution, transferring to a closed reactor, carrying out a hydrothermal reaction for 6-48 h at a temperature of 200-300 DEG C under a pressure of 0.1-20 MPa, and carrying out centrifugal separation to obtain the vanadium trioxide powder, wherein the vanadium source is orthovanadate (V) or/and a vanadyl salt (IV), preferably at least one selected from Na3VO4, K3VO4, Rb3VO4, Cs3VO4, VOSO4, VOCl2, vanadyl acetylacetonate and vanadyl oxalate, the reducing agent is at least one selected from oxalic acid, hydrazine and alcohol, and preferably the alcohol is at least one selected from methanol, ethanol,n-propanol, isopropanol, n-butanol and isobutanol.

Description

technical field [0001] The invention relates to a method for one-step hydrothermal preparation of vanadium trioxide, which belongs to the technical field of chemical material synthesis and functional materials. Background technique [0002] Vanadium trioxide V 2 o 3 It has the property of metal-nonmetal transition (also known as MST or MIT). It has good phase transition characteristics at low temperature, and the resistance mutation can reach 6 orders of magnitude. It is also accompanied by changes in lattice and antiferromagnetism. It is a monoclinic antiferromagnetic semiconductor at low temperature. state, which has two phase transition points: 150-170K and 500-530K, and the magnetic susceptibility, light transmittance and reflectance also change abruptly during the phase transition. Due to its excellent optical, electrical and magnetic properties, in the series of vanadium oxides, vanadium trioxide (V 2 o 3 ) is a very important product, which has broad application p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2004/03C01P2004/61C01P2004/62
Inventor 黄爱彬赵书文纪士东金平实周奕杰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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