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Method for preparing vanadium dioxide powder

A technology of vanadium dioxide and powder, which is applied in the field of preparation of vanadium dioxide powder, can solve the problems of high cost of vanadium dioxide raw materials, complex process, large environmental pollution, etc. The effect of low temperature and low price

Inactive Publication Date: 2012-08-15
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] As mentioned above, most of the raw materials used in the production of vanadium dioxide powder are vanadium pentoxide, or various complex precursors prepared with vanadium pentoxide as raw materials, resulting in higher raw material costs for the preparation of vanadium dioxide. The use of acid and alkali also produces corresponding environmental costs, and the process becomes complicated
In addition, V2O5 is produced by heating and oxidatively decomposing ammonium metavanadate or poly(poly)ammonium vanadate, which itself has a relatively high cost, and the current industrialized production of vanadium pentoxide is relatively polluting to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] The operation steps of this preparation method are:

[0028]First, powder vanadate is added to the pressure-resistant reactor, and then the reaction medium is added to the reactor, and the reactor is heated to make the temperature of the reactor reach 50-250 °C and the pressure reach 0.1-45.0 Mpa. Under the conditions for 0.1~10.0 h, then release the reactor pressure to 0~5.0 Mpa within 0.1~2.0 h while maintaining 50~250 °C, then cool the reactor to room temperature, wash and vacuum dry The vanadium dioxide powder can be obtained.

[0029] Among them, the vanadate is one or a mixture of ammonium metavanadate and poly(poly)ammonium vanadate; the reaction medium is one or two mixtures of low-carbon alcohol, CO2 and H2; the reaction temperature is controlled at 50~250 ℃; the reaction pressure is controlled at 0.1-45.0 Mpa; the reaction time is controlled at 0.1-10.0 h; the time for releasing the pressure in the reactor is controlled at 0.1-2.0 h. The following are specif...

Embodiment 1

[0031] Weigh 10.0 g of ammonium metavanadate and place it in a reactor with a capacity of 1 L, add 345 mL of absolute ethanol, seal the reactor, heat, and react at 220 °C and 5.2 Mpa for 1.5 h, and slowly The reactor pressure was reduced, and after two hours the reactor pressure became 0, and the reactor was allowed to cool naturally. The solid powder was separated, washed three times with absolute ethanol, and dried under vacuum at 80°C for 2.0 to obtain 5.6 g of powdery vanadium dioxide.

Embodiment 2

[0033] 20.0 g poly (poly) ammonium vanadate is placed in the reactor, and the reactor volume is 1 L, and 150 mL of ethanol is added, and the reactor is heated to 200 ° C, and CO2 gas is introduced into the reactor at the same time, and the pressure in the reactor Keep it at 26.3 Mpa, and after reacting under this condition for 4.0 h, the reactor pressure was reduced to 0.4 Mpa within 1.6 h, and the reactor was naturally cooled to room temperature. The solid product in the reactor was separated, washed three times with absolute ethanol, and then vacuum-dried at 80 °C for 1.0 h to obtain 11.4 g of vanadium dioxide blue-black powder.

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PUM

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Abstract

The invention discloses a method for preparing vanadium dioxide powder, which belongs to a method for preparing a chemical material. The method comprises the following process: adding powdered vanadate serving as a raw material into a high-pressure-resistance reactor; adding liquid or gas reaction media into the reactor at the same time; heating the reactor to a temperature of 50 to 250 DEG C; keeping the pressure in the reactor between 0.1 and 45.0Mpa for 0.1 to 10.0 hours; relieving the pressure in the reactor to 0 to 0.5Mpa; decreasing the temperature in the reactor to normal temperature; separating out solid powder; and washing, drying under vacuum and obtaining powdered vanadium dioxide. In the method, the vanadium dioxide is prepared in a supercritical fluid system, the reaction time is short and the reaction temperature is low; the operation in the preparation process is simple and easy; the raw material and reagents are cheap and readily available; and the product can be separated easily in a production process, and thus, purer vanadium dioxide can be obtained.

Description

technical field [0001] The invention belongs to a preparation method of chemical materials, in particular to a preparation method of vanadium dioxide powder. Background technique [0002] Vanadium dioxide (VO2) is a kind of vanadium oxide, which belongs to thermally induced phase change metal compound, and a sudden change occurs from a high temperature metal phase to a low temperature semiconductor phase around 68 °C. In the process of phase transition, the optical, electrical, magnetic and other properties of materials will change dramatically. Therefore, VO2 is widely used in many aspects such as photoelectric switch materials, storage media, photonic crystals, infrared imaging simulation, gas sensors and smart glass. At present, there are many studies on the preparation of vanadium dioxide thin film materials, and there are many preparation methods. There are few simple methods for preparing vanadium dioxide powder from cheap and easy-to-obtain raw materials. Compared ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02
CPCY02P20/54
Inventor 于三三李文秀李双明
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY