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Method for preparing vanadium trioxide through liquid-phase hydrogen reduction

A technology of vanadium trioxide and liquid phase, applied in vanadium oxide, chemical recovery and other directions, can solve the problems of limited industrial application, high price of palladium chloride, and high production cost, and achieves low production cost, high purity, and high production cost. Efficient effect

Pending Publication Date: 2022-03-04
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, although the method of liquid-phase synthesis of vanadium trioxide can greatly reduce energy consumption, the reaction time is too long and the efficiency is low, which seriously limits the industrial application; although the research of Zhang Guobin et al. shortened the reaction time to 2h , but the price of palladium chloride is as high as 1500 yuan / g, and the production cost is high

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  • Method for preparing vanadium trioxide through liquid-phase hydrogen reduction

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Embodiment 1

[0028] A method for preparing vanadium trioxide by liquid-phase hydrogen reduction. The specific steps of the method described in this embodiment are as follows:

[0029] Step 1. Completely dissolve the pentavalent vanadium compound with sodium hydroxide solution, and then adjust the pH value to 5-5.5 to obtain a vanadium-enriched liquid; the vanadium concentration of the vanadium-enriched liquid is 0.1-0.4 mol / L.

[0030] Step 2. According to the filling rate of the vanadium-rich liquid in the autoclave is 50-60%, the vanadium-rich liquid is placed in the autoclave; then the solid-liquid ratio is 10-20g / L, and the Add nickel powder into the vanadium-rich liquid as a catalyst; then, under the conditions of temperature 250-260°C, hydrogen partial pressure 3-4MPa and rotation speed 300-400r / min, stir for 2-3h, cool, and release the pressure to obtain Vanadium trioxide slurry.

[0031] Step 3, subjecting the vanadium trioxide slurry to wet magnetic separation under the conditio...

Embodiment 2

[0037] A method for preparing vanadium trioxide by liquid-phase hydrogen reduction. The specific steps of the method described in this embodiment are as follows:

[0038] Step 1. Completely dissolve the pentavalent vanadium compound with sodium hydroxide solution, and then adjust the pH value to 4.5-5 to obtain a vanadium-enriched liquid; the vanadium concentration of the vanadium-enriched liquid is 0.3-0.6 mol / L.

[0039] Step 2. According to the filling rate of the vanadium-rich liquid in the autoclave is 50-60%, the vanadium-rich liquid is placed in the autoclave; then the solid-liquid ratio is 20-30g / L, and the Add nickel powder into the vanadium-rich liquid as a catalyst; then, under the conditions of temperature 260-270°C, hydrogen partial pressure 4-5MPa and rotation speed 400-500r / min, stir for 3-4h, cool, and release the pressure to obtain Vanadium trioxide slurry.

[0040] Step 3, subjecting the vanadium trioxide slurry to wet magnetic separation under the conditio...

Embodiment 3

[0046]A method for preparing vanadium trioxide by liquid-phase hydrogen reduction. The specific steps of the method described in this embodiment are as follows:

[0047] Step 1. Completely dissolve the pentavalent vanadium compound with sodium hydroxide solution, and then adjust the pH value to 4-4.5 to obtain a vanadium-enriched liquid; the vanadium concentration of the vanadium-enriched liquid is 0.5-0.8 mol / L.

[0048] Step 2. According to the filling rate of the vanadium-rich liquid in the autoclave is 40-50%, the described vanadium-rich liquid is placed in the autoclave; then the solid-liquid ratio is 30-40g / L, and the Add nickel powder into the vanadium-rich liquid as a catalyst; then, under the conditions of temperature 270-290°C, hydrogen partial pressure 5-6MPa and rotation speed 500-600r / min, stir for 4-5h, cool, and release the pressure to obtain Vanadium trioxide slurry.

[0049] Step 3, subjecting the vanadium trioxide slurry to wet magnetic separation under the...

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Abstract

The invention discloses a method for preparing vanadium trioxide through liquid phase hydrogen reduction. According to the technical scheme, the method comprises the following steps: dissolving a pentavalent vanadium compound by using a sodium hydroxide solution, adjusting the pH value to 4-6, putting the obtained vanadium-rich liquid into a high-pressure kettle, adding nickel powder as a catalyst, and stirring, cooling and releasing the pressure under the conditions that the temperature is 250-300 DEG C, the hydrogen partial pressure is 3-6 MPa and the speed is 300-600 r / min to obtain vanadium trioxide slurry; and then carrying out wet magnetic separation to obtain magnetic concentrate slurry and magnetic tailing slurry. Carrying out solid-liquid separation on the magnetic concentrate slurry, carrying out vacuum drying, and returning the obtained magnetic concentrate to the step 2 to be recycled as a catalyst; carrying out solid-liquid separation on the magnetic separation tailing slurry to obtain wet magnetic separation tailings and alkali liquor; the wet magnetic separation tailings are subjected to vacuum drying, and vanadium trioxide is prepared; and returning the alkali liquor to the step 1 for recycling so as to dissolve the pentavalent vanadium compound. The method is high in safety, low in energy consumption and low in production cost, the catalyst can be recycled, and the prepared product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of preparing vanadium trioxide. In particular, it relates to a method for preparing vanadium trioxide by liquid-phase hydrogen reduction. Background technique [0002] Vanadium trioxide is an important vanadium oxide, which can be used to prepare flake vanadium or powder vanadium, vanadium iron alloy, vanadium nitride and vanadium carbide, etc. In addition, since the temperature will cause a phase change of vanadium trioxide, the resistivity, magnetic susceptibility, light projection rate and reflectivity will all change suddenly during the phase change, so it is used in thermoelectric switches, magnetic switches, optical switches, sensors and thin film materials. has important applications. At present, the preparation methods of vanadium trioxide are roughly divided into reduction roasting and liquid phase synthesis: [0003] Reduction roasting is currently the most common method for preparing vanadium t...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2006/80Y02P20/584
Inventor 张一敏胡艺博薛楠楠胡鹏程
Owner WUHAN UNIV OF SCI & TECH
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