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Process for preparing crystal vanadium trioxide

A technology of vanadium trioxide and vanadium pentoxide, which is applied in the field of preparing vanadium trioxide with crystal form and preparing vanadium trioxide, and can solve the problems of high reaction temperature and calcination temperature, harsh reaction conditions, and high reaction temperature , to achieve the effect of short reaction route, low reaction temperature and simple raw materials

Inactive Publication Date: 2006-01-25
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantage of high reaction temperature and calcination temperature
[0004] CN1118765A discloses a kind of industrial gas reduction ammonium vanadate or vanadium pentoxide to prepare V 2 o 3 Powder method, but the reaction temperature is 550-650°C, which also has the disadvantage of high reaction temperature
[0005] SU1006375 discloses a method of reducing vanadium pentoxide with metal vanadium to prepare V 2 o 3 In the method, although 100% of V can be obtained within 2-3 minutes 2 o 3 , but the reaction conditions of 1200-1600°C and 7-9Pa are too harsh

Method used

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  • Process for preparing crystal vanadium trioxide

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Experimental program
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Effect test

Embodiment 1

[0019] The 4.51 g V 2 o 5 The powder was dispersed in 250mL of methanol, then transferred to an autoclave, and after sealing, the temperature was gradually raised to 248°C, and the pressure was 9.8Mpa at this time. After keeping this condition for 28.5 hours, the solvent methanol in the kettle was drained at 248°C within 5.4 hours, and the temperature at this time was 245°C. Turn off the heating, cool naturally to room temperature, obtain 3.82g black V with a certain crystal form 2 o 3 powder. The XRD spectrogram of gained black powder sees attached figure 1 . From attached figure 1 It can be seen that the new V 2 o 3 The powder is already well crystalline.

Embodiment 2

[0021] The 10.92 g V 2 o 5 The powder was dispersed into 250mL of absolute ethanol, then transferred to an autoclave, and after sealing, the temperature was gradually raised to 260°C, and the pressure was 9.0MPa at this time. After maintaining this condition for 3 hours, the solvent ethanol in the kettle was drained within 1.3 hours under constant temperature conditions. When the solvent was about to be exhausted, the temperature of the kettle rose sharply, reaching 300°C. Turn off heating, cool to room temperature naturally, obtain 8.72g black V 2 o 3 powder. From attached figure 1 It can be seen that the new V 2 o 3 The powder is already well crystalline.

Embodiment 3

[0023] The 10.44 g V 2 o 5 Disperse it in 250mL of n-propanol, then transfer it to an autoclave, and after sealing it, gradually raise the temperature to 262°C, and the pressure at this time is 9.5Mpa. After keeping this condition for 3 hours, the solvent in the kettle, n-propanol, was drained at 262°C within 3.3 hours. When the solvent was about to be exhausted, the kettle temperature rose sharply and reached 298°C. Turn off the heating, cool naturally to room temperature, and obtain 8.02g of black V with a certain crystal form. 2 o 3 powder.

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Abstract

A process for preparing crystalline V2O3 includes such steps as dispersing V2O5 powder in proper organic solvent, adding to high-pressure tubular reactor, reacting at a certain temp under a certain pressure, and removing solvent.

Description

technical field [0001] The invention provides a method for preparing vanadium trioxide, specifically a method for preparing vanadium trioxide with a crystal form. It belongs to the technical field of inorganic chemistry and also belongs to the technical field of functional materials. Background technique [0002] Vanadium trioxide (V 2 o 3 ) is a black powder at room temperature. When the temperature reaches 730°C, the amorphous vanadium trioxide can be transformed into crystal form vanadium trioxide. Vanadium trioxide has two temperature-dependent phase transitions. Near -113°C, a first-order phase transition from low-temperature antiferromagnetic insulating phase (AFI) to high-temperature paramagnetic metallic phase (PM) occurs, and the resistivity change shows NTC characteristics, and the single crystal resistivity mutation reaches 7 orders of magnitude. At about 277 ° C, a secondary phase transition from a low-temperature paramagnetic metal phase (PM) to a high-temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
Inventor 黄驰易生平
Owner WUHAN UNIV
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