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Method for preparing titanium-tungsten co-doped vanadium dioxide powder from vanadium extraction solution

A vanadium dioxide and co-doping technology, which is applied in the direction of vanadium oxide, etc., can solve the problems of increasing the production cost of vanadium dioxide, being unfavorable for large-scale preparation, and complex preparation processes, etc., achieving excellent sunlight regulation ability, and is beneficial to The effect of wide application and simple process

Pending Publication Date: 2021-10-15
ANSTEEL BEIJING RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method takes a long time and consumes a lot of energy, which is not conducive to large-scale preparation
At present, the preparation of vanadium dioxide powder mainly uses vanadium pentoxide, ammonium metavanadate, vanadyl sulfate, etc. as raw materials. The preparation process of these raw materials is complicated, and the price is often high, which greatly increases the production cost of vanadium dioxide.

Method used

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  • Method for preparing titanium-tungsten co-doped vanadium dioxide powder from vanadium extraction solution
  • Method for preparing titanium-tungsten co-doped vanadium dioxide powder from vanadium extraction solution
  • Method for preparing titanium-tungsten co-doped vanadium dioxide powder from vanadium extraction solution

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Effect test

Embodiment 1

[0036]Measure 70mL of vanadium extraction solution, adjust the pH value to 2 with 10% hydrochloric acid solution by mass fraction; measure the concentration of pentavalent vanadium ions by potentiometric titration to 40g / L, that is, the total molar mass of vanadium ions is 0.055mol. Slowly add 4mL hydrazine hydrate (mass fraction is 85%) wherein, promptly the molar weight of reducing agent hydrazine hydrate is 0.068mol, and the molar ratio of vanadium ion and reducing agent is 0.81, and this moment solution turns blue; Add 0.42g of ammonium tungstate and 0.21g of titanium tetrachloride solution to the solution, and use ultrasonic to mix evenly; transfer the mixed solution to a hydrothermal reaction kettle with a volume of 100mL; then, hydrothermally react at 280°C for 15h; after natural cooling , the solution was centrifuged at high speed; then the solid precipitate was washed with ethanol and deionized water; the solid was freeze-dried to obtain 2at% Ti and 3at% W co-doped van...

Embodiment 2

[0043] Measure 70mL of vanadium extraction solution, adjust the pH value to 2 with 10% hydrochloric acid solution by mass fraction; measure the concentration of pentavalent vanadium ions by potentiometric titration to 40g / L, that is, the total molar mass of vanadium ions is 0.055mol. Slowly add 4mL hydrazine hydrate (mass fraction is 85%) wherein, promptly the molar weight of reducing agent hydrazine hydrate is 0.068mol, and the molar ratio of vanadium ion and reducing agent is 0.81, and this moment solution turns blue; Add 0.28g of ammonium tungstate and 0.10g of titanium tetrachloride solution to the solution, and use ultrasonic waves to mix evenly; transfer the mixed solution to a hydrothermal reaction kettle with a volume of 100mL; then conduct a hydrothermal reaction at 280°C for 15h; after natural cooling , the solution was centrifuged at high speed; then the solid precipitate was washed with ethanol and deionized water; the solid was freeze-dried to obtain 1% Ti and 2% W...

Embodiment 3

[0049] Measure 70mL of vanadium extraction solution, adjust the pH value to 2 with 10% hydrochloric acid solution by mass fraction; measure the concentration of pentavalent vanadium ions by potentiometric titration to 40g / L, that is, the total molar mass of vanadium ions is 0.055mol. Slowly add 4mL hydrazine hydrate (mass fraction is 85%) wherein, promptly the molar weight of reducing agent hydrazine hydrate is 0.068mol, and the molar ratio of vanadium ion and reducing agent is 0.81, and this moment solution turns blue; Add 0.14g of ammonium tungstate and 0.10g of titanium tetrachloride solution to the solution, and use ultrasonic waves to mix evenly; transfer the mixed solution to a hydrothermal reaction kettle with a volume of 100mL; then conduct a hydrothermal reaction at 280°C for 15h; after natural cooling , the solution is centrifuged at high speed; then the solid precipitate is washed with ethanol and deionized water; the solid is freeze-dried to obtain 1% Ti and 1% W co...

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Abstract

The invention discloses a method for preparing titanium-tungsten co-doped vanadium dioxide powder from a vanadium extraction solution, wherein the method comprises the steps: a, adding an acid solution into the vanadium extraction solution, and adjusting the pH value; b, measuring the concentration of vanadium ions in the vanadium extraction solution, and adding a reducing agent; c, adding a tungsten compound and a titanium compound into the solution obtained in the step b, carrying out hydrothermal reaction, and separating to obtain a precipitate; and d, washing and drying the precipitate obtained in the step c to obtain the titanium-tungsten co-doped vanadium dioxide powder. According to the method, the vanadium extraction solution is adopted as the vanadium source, the cost is effectively reduced, the phase change temperature of the vanadium dioxide is reduced through tungsten element doping, meanwhile, the optical property and stability of the vanadium dioxide are improved through titanium element doping, and wide application of the vanadium dioxide in the field of phase change energy saving is promoted.

Description

technical field [0001] The invention belongs to the technical field of temperature-induced phase change materials, and in particular relates to a method for preparing titanium-tungsten co-doped vanadium dioxide powder from a vanadium extraction solution. Background technique [0002] Vanadium dioxide has become one of the ideal materials in the field of temperature-induced phase change and energy saving because of the obvious difference in the transmittance of near-infrared light before and after the phase change. The shortcomings of high temperature-induced phase transition temperature (68°C), poor stability, low visible light transmittance, and weak near-infrared light regulation ability prevent vanadium dioxide from being widely used. In order to solve these shortcomings, researchers have proposed many solutions, including element doping, composite technology, introducing defects, structural regulation, ordered arrays, etc. Among them, element doping is considered to be ...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/52C01P2006/60
Inventor 尹翔鹭杨晓高荣荣曾泽华刘天豪
Owner ANSTEEL BEIJING RES INST
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