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Microwave-assisted synthesis method for titanium dioxide nanotube with high catalytic activity

A high catalytic activity, titanium dioxide technology, applied in the direction of titanium dioxide, catalyst activation/preparation, chemical instruments and methods, etc., can solve the problems of long time, large energy consumption, etc., and achieve the effect of short process, less reaction equipment and mild reaction conditions

Inactive Publication Date: 2014-04-02
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many preparation methods for titanium dioxide nanotube materials, and the concentrated alkali hydrothermal method is the best way to prepare TiO 2 The common method of nanotubes, but the TiO after one hydrothermal treatment with concentrated alkali 2 Nanotubes need to be transformed before they can be used as photocatalytic materials. The usual treatment method is to undergo secondary hydrothermal or calcination to transform the crystal form into anatase phase TiO 2 , in the above two methods, the secondary hydrothermal is the TiO 2 The nanotube precursor powder is placed in a high-pressure reactor equipped with an acid solution, but this operation process takes a long time, generally 4 to 48 hours, and the calcination method requires the precursor TiO 2 Nanotubes are calcined at high temperature (400-500°C), which consumes a lot of energy

Method used

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  • Microwave-assisted synthesis method for titanium dioxide nanotube with high catalytic activity
  • Microwave-assisted synthesis method for titanium dioxide nanotube with high catalytic activity
  • Microwave-assisted synthesis method for titanium dioxide nanotube with high catalytic activity

Examples

Experimental program
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Effect test

Embodiment 1

[0010] Anatase TiO as a precursor 2 Preparation of primary hydrothermal TiO by concentrated alkali hydrothermal method 2 Nanotubes (TNT for short). 0.1g primary water heating TiO 2 Nanotubes placed in 50mL0.01mol / L HNO 3 In the solution, after ultrasonic mixing, transfer the solution to a high-pressure microwave reactor and seal it, place it in a microwave digestion instrument, and react at a microwave water temperature of 2.0 MPa for 15 minutes. After the reaction, the reactor is naturally cooled to room temperature, and the reaction product Carry out centrifugation, wash the obtained solid matter with deionized water to pH = 7, and then dry the obtained precipitate in an oven at a drying temperature of 80°C for 30 minutes to obtain the anatase phase TiO 2 Nanotubes (abbreviated as WTNTs).

Embodiment 2

[0012] Anatase TiO as a precursor 2 Preparation of primary hydrothermal TiO by concentrated alkali hydrothermal method 2 Nanotubes (TNT for short). 0.2g primary water heating TiO 2 Nanotubes placed in 30mL0.02mol / L HNO 3 In the solution, after ultrasonic mixing, transfer it to a high-pressure microwave reactor and seal it, place it in a microwave digestion instrument, and react at a microwave water temperature of 2.0 MPa for 10 minutes. After the reaction, the reactor is naturally cooled to room temperature, and the reaction product is centrifuged Separation, washing the obtained solid matter with deionized water to pH = 7, filtering and drying the obtained precipitate in an oven at a drying temperature of 60°C and a drying time of 20 minutes to obtain anatase phase TiO 2 Nanotubes (abbreviated as WTNTs).

Embodiment 3

[0014] Anatase TiO as a precursor 2 Preparation of primary hydrothermal TiO by concentrated alkali hydrothermal method 2 Nanotubes (TNT for short). 0.1g primary water heating TiO 2 Nanotubes placed in 25mL0.04mol / L HNO 3 In the solution, after ultrasonic mixing, transfer it to a high-pressure microwave reactor to seal, place it in a microwave digestion instrument, and react at a microwave water temperature of 1.5MPa for 15 minutes. After the reaction, the reactor is naturally cooled to room temperature, and the reaction product is centrifuged. Separation, washing the obtained solid matter with deionized water to pH = 7, filtering and drying the obtained precipitate in an oven at a drying temperature of 70°C and a drying time of 30 minutes to obtain anatase phase TiO 2 nanotube.

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Abstract

The invention discloses a microwave-assisted synthesis method for a titanium dioxide nanotube with high catalytic activity. The microwave-assisted synthesis method comprises the steps as follows: preparing a one-time hydrothermal TiO2 nanotube by anatase phase TiO2 according to a concentrated alkaline hydrothermal method; and placing the one-time hydrothermal TiO2 nanotube into an HNO3 solution under the condition that the ratio of the one-time hydrothermal TiO2 nanotube to the HNO3 solution is 1g to 0.003-0.01mol, ultrasonically and uniformly mixing, sealing the mixture in a high-pressure microwave reaction kettle, placing the microwave reaction kettle into a microwave digestion instrument, ultrasonically reacting for 10-20min at the water temperature at the pressure of 1.5-3.0MPa, after the reaction is ended, naturally cooling the reaction kettle to room temperature, centrifuging and separating reaction products, cleaning the obtained solid matters by de-ionized water until the pH value is 7, filtering and drying the obtained deposition by an oven for 20-30min at the temperature of 60-80 DEG C so as to obtain the anatase phase TiO2 nanotube. The microwave-assisted synthesis method is simple, easy to implement, short in preparation time and low in energy consumption.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano-adsorption-photocatalytic materials, and in particular relates to a microwave-assisted synthesis method of titanium dioxide nanotubes with high catalytic activity. Background technique [0002] TiO 2 Nanotube photocatalytic materials have become TiO due to their large specific surface area. 2 A hot topic in the field of photocatalyst preparation research. At present, there are many preparation methods for titanium dioxide nanotube materials, and the concentrated alkali hydrothermal method is the best way to prepare TiO 2 The common method of nanotubes, but the TiO after one hydrothermal treatment with concentrated alkali 2 Nanotubes need to be transformed before they can be used as photocatalytic materials. The usual treatment method is to undergo secondary hydrothermal or calcination to transform the crystal form into anatase phase TiO 2 , in the above two methods, the secondary h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047B01J21/06B01J37/34
Inventor 钮金芬姚秉华彭超张凡宏张玩涛
Owner XIAN UNIV OF TECH