Titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine and preparation method of material

A photocatalytic material, titanium dioxide technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of long reaction time, difficult to popularize and apply, and achieve high reuse rate and high practicality The effect of value and process is simple and easy to control

Inactive Publication Date: 2014-07-02
PUTIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, hydrothermal method, solvothermal method, precipitation method, etc. can be used to prepare doped catalysts with morphology, but these usually

Method used

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  • Titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine and preparation method of material
  • Titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine and preparation method of material
  • Titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine and preparation method of material

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Experimental program
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preparation example Construction

[0042] The preparation method is an ultrasonic atomization method, which includes the following steps:

[0043] 1) Dissolving titanium tetrafluoride in a hydrochloric acid solution with a concentration of 1.0 mol / L and stirring for 1-3 hours to obtain a transparent precursor;

[0044] 2) The precursor liquid is atomized in the reaction bottle under the action of an ultrasonic atomizer, and forms an aerosol rich in tiny droplets together with ammonia gas, the frequency of the ultrasonic atomizer is 1.7 MHz;

[0045] 3) The aerosol is driven by the vacuum pump into the high-temperature tube furnace. Each aerosol forms a microreactor in the tube furnace. The reaction temperature is 500-600 ℃, and the ammonia flow rate is 10-30 L / min. The reaction process The middle titanium tetrafluoride is hydrolyzed to form titanium dioxide. Nitrogen and fluorine are doped into the titanium dioxide crystal and form spherical granular solid powder;

[0046] 4) Driven by the vacuum pump, the solid powder...

Embodiment 1

[0051] 1.5 g of titanium tetrafluoride was dissolved in a hydrochloric acid solution with a concentration of 1.0 mol / L. After 2 hours of stirring, a transparent solution was obtained; the solution was atomized in an ultrasonic atomizer with a frequency of 1.7 MHz, and the carrier gas The aerosol belt enters the high temperature tube furnace (500 ℃) to react; the flow rate of the carrier gas is 10 L / min, the carrier gas does not pass through the ammonia solution, and the solid powder generated is collected with distilled water after the tube furnace, washed, centrifuged Drying at 85°C; the obtained solid powder is continuously calcined in a muffle furnace at 550°C for 2.5 hours at a heating rate of 5°C / min to obtain a fluorine-doped titanium dioxide mesoporous microsphere photocatalytic material, which is used as a fluorine and nitrogen co- Comparative example of doped titanium dioxide mesoporous microspheres.

Embodiment 2

[0053] 1.5 g of titanium tetrachloride was dissolved in a hydrochloric acid solution with a concentration of 1.0 mol / L, and after 2 hours of stirring, a transparent solution was obtained; the solution was atomized in an ultrasonic atomizer with a frequency of 1.7 MHz, The aerosol is carried by the carrier gas into the high temperature tube furnace (500 ℃) for reaction; the flow rate of the carrier gas is 10 L / min, and the carrier gas first passes through the ammonia aqueous solution with the concentration of 5 mol / L to make the carrier gas rich in ammonia ; After the tube furnace, collect the resulting solid powder with distilled water, wash it, centrifuge and dry it at 85°C; the obtained powder solid will continue to be calcined in the muffle furnace at 550°C for 2.5 hours at a heating rate of 5°C / min To obtain a yellow nitrogen-doped titanium dioxide mesoporous microsphere photocatalytic material, which is used as a comparative example of fluorine and nitrogen co-doped titaniu...

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Abstract

The invention discloses a titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine in response to visible light and a preparation method of the material. The preparation method of the material comprises the following steps: firstly dissolving titanium tetrafluoride in hydrochloric acid to obtain a reaction precursor solution, atomizing the precursor solution in an ultrasonic atomizer to generate aerosol rich in tiny droplets, introducing the aerosol into a high-temperature tubular furnace in the presence of ammonia gas to react and generate solid powder, collecting the solid powder by using distilled water, washing, centrifuging and then drying at the temperature of 75-85 DEG C to obtain the solid powder, sequentially roasting for 1.5-2.5 hours in a muffle furnace at the temperature of 450-550 DEG C to prepare the titanium dioxide mesoporous microsphere photocatalytic material co-doped with nitrogen and fluorine. A crystalline phase of the material is an anatase phase; the material comprises the following components by weight percent: 1.5-3.0% of fluorine, 0.8-5.2% of nitrogen and the balance being titanium dioxide; the titanium dioxide co-doped with nitrogen and fluorine has a mesoporous microsphere particle shape; an ultraviolet-visible light spectrum begins to absorb when being below 600nm. The preparation method of the material is simple, practicable and capable of continuously producing, and facilitating the large-scale production and application in industrialization.

Description

Technical field [0001] The invention belongs to the field of material preparation and environmental photocatalysis, and specifically relates to a photocatalytic material of nitrogen and fluorine co-doped titanium dioxide mesoporous microspheres and a preparation method thereof. Background technique [0002] TiO 2 Abundant sources, non-toxic, tasteless, stable physical and chemical properties, and good biocompatibility have become the most common photocatalyst. However, TiO 2 In the process of photocatalytic reaction, photo-generated electrons and photo-generated holes have extremely short lifetimes, and they are very easy to recombine during the photocatalytic reaction, which makes their quantum efficiency in the photocatalytic process low; TiO 2 The energy band width of TiO2 is about 3.2 eV, which cannot respond to visible light. Less than 5% of the sunlight energy can be used, which makes TiO 2 Extensive industrial applications are greatly restricted. In order to solve these pr...

Claims

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Application Information

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IPC IPC(8): B01J27/24
Inventor 黄建辉陈建琴林伟
Owner PUTIAN UNIV
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