CN104383903A - Preparation method of titanium dioxide microsphere photocatalyst - Google Patents
Preparation method of titanium dioxide microsphere photocatalyst Download PDFInfo
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- CN104383903A CN104383903A CN201410661332.4A CN201410661332A CN104383903A CN 104383903 A CN104383903 A CN 104383903A CN 201410661332 A CN201410661332 A CN 201410661332A CN 104383903 A CN104383903 A CN 104383903A
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Abstract
The invention discloses a preparation method of a titanium dioxide microsphere photocatalyst. The preparation method comprises the following steps: adding ammonium fluorotitanate in deionized water or alcohol; adding boric acid (H3BO3) in a solution obtained in the precious step, then adding a polymer template agent, mixing until the polymer template agent is completely dissolved; placing a solution at a temperature of 30-80 DEG C for 10-24h, washing for 5 times respectively by using the deionized water and the alcohol, drying at a temperature of 60 DEG C for 12h; and annealing the dried powder at a temperature of 400-600 DEG C for 1-5h, wherein the obtained white powder is the titanium dioxide microsphere photocatalyst. The preparation method is simple, is free from complicated and expensive equipment, mild in synthesis conditions, and beneficial to largely popularize; TiO2 microspheres prepared by adopting the preparation method can be used in the fields such as photocatalysis and solar cell photo-anodes.
Description
Technical field
The present invention relates to the technology of preparing of metal oxide micro-nano material, specifically refer to a kind of preparation method of the titanium dioxide microballoon sphere for photochemical catalyst.
Background technology
Along with developing rapidly of modern industrial technology, problem of environmental pollution is day by day serious, the challenge that the Faced In Sustainable Development of human society is huge, effectively utilizes sunshine pollution administration to show wide application prospect.In recent years, Photocatalitic Technique of Semiconductor has become one of most active research field, TiO
2enjoy the favor of scientific research personnel owing to having high, the cheap and advantages such as non-secondary pollution of stable chemistry and optical property, catalytic efficiency, can photochemical catalyst be made into, purify air.Nano-TiO conventional at present
2technology of preparing comprise hydro-thermal method, sol-gel process, hydro-thermal method reaction needed is carried out in high-temperature high-pressure reaction kettle, and course of reaction influence factor is more; Sol-gel process preparation technology is comparatively loaded down with trivial details, and cost is high.For current Problems existing, we propose a kind of chemical solution method and prepare TiO
2the way of microballoon, Ti presoma and template are stirred to dissolve completely and form microballoon presoma by the method at a lower temperature, and then high annealing forms anatase TiO
2, the method preparation technology is simple, consuming time short, TiO
2powder output is high, due to experimental facilities no requirement (NR), is expected to realize producing in enormous quantities; The TiO generated
2microsphere surface is made up of a large amount of nano level particle, makes material have larger specific area.TiO prepared by the method
2microballoon can be used for photocatalysis degradation organic contaminant, solar battery photoanode, environmental monitoring and improvement.
Summary of the invention
The object of this invention is to provide one and simply prepare TiO
2the preparation method of microballoon, the method does not need to use expensive equipment, and preparation condition is gentle, is expected to produce in enormous quantities.
A preparation method for titanic oxide microsphere photocatalyst, is characterized in that, concrete steps are as follows:
Ammonium titanium fluoride is added in deionized water or ethanol; Boric acid (H is added in above-mentioned solution
3bO
3), then add polymer template agent, be stirred to and dissolve completely; Solution is placed 10 ~ 24 hours at 30 ~ 80 DEG C, then respectively washes 5 times with deionized water, alcohol, 60 DEG C of dryings 12 hours; By 400 ~ 600 DEG C dried, powder annealing 1 ~ 5 hour, gained white powder was titanic oxide microsphere photocatalyst.
The concentration of described ammonium titanium fluoride is 0.1 ~ 0.5 mol/L; Described boric acid and the mol ratio of ammonium titanium fluoride are 5:1 ~ 1:2.
Described polymer template agent is APEO or triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene or bi-block copolymer polystyrene-polyoxyethylene; The mass percent of described polymer template agent is 0.1 ~ 0.5%.
The present invention utilizes chemical solution method to synthesize TiO
2microballoon, utilizes polymer for template, induces titanium precursors to form ammonium titanium fluoride microballoon under mild conditions, makes microballoon crystallization form anatase TiO under the high temperature conditions
2; TiO prepared by the present invention
2microballoon can be used for the catalyst of degradable organic pollutant, environmental monitoring and improvement, solar battery photoanode; Preparation method of the present invention is simple, is conducive to large-scale popularization.
Accompanying drawing explanation
Fig. 1 is TiO of the present invention
2the SEM figure of microballoon.
Fig. 2 is TiO of the present invention
2the high power SEM figure of microballoon.
Fig. 3 is TiO of the present invention
2the XRD figure of microballoon.
Fig. 4 is TiO of the present invention
2microballoon and methyl blue mixed solution under UV Light condition, dye strength and its initial concentration ratio (C/C
o) graph of a relation over time.
Detailed description of the invention
Embodiment 1:
The ammonium titanium fluoride of 0.99g is added in 50 ml ionized waters; The H of 0.6183 g is added in above-mentioned solution
3bO
3; In above-mentioned solution, add the APEO of 10 g, be stirred to and dissolve completely; Placed 24 hours at 40 DEG C by solution, then respectively wash 5 times with deionized water, alcohol, 60 degree dry 12 hours; By 450 DEG C dried, powder annealing 2 hours, obtain white TiO
2powder.
Fig. 1 and Fig. 2 is respectively TiO
2sEM figure and the high power SEM figure of microballoon, as seen from the figure, TiO
2microsphere Size 1 microns, microsphere surface is assembled by nano particle; Fig. 3 is TiO
2the XRD collection of illustrative plates of microballoon, as can be seen from Fig., each diffraction maximum is substantially corresponding with standard card anatase tio2 (JCPDS, 21-1272), and nano-TiO is described
2crystal formation is single high-purity Detitanium-ore-type.This is TiO
2the application in photocatalysis of mesoporous microsphere is laid a good foundation; Fig. 4 is the photocatalysis effect of TiO2 microballoon, and as seen from the figure, TiO2 microballoon can reach 99.7 % to the degradation efficiency of methyl blue.
Embodiment 2:
The ammonium titanium fluoride of 3g is added in 50 ml ionized waters; The H of 1.86 g is added in above-mentioned solution
3bO
3; In above-mentioned solution, add the APEO of 3 g, be stirred to and dissolve completely; Placed 20 hours at 60 DEG C by solution, then respectively wash 5 times with deionized water, alcohol, 60 degree dry 12 hours; By 500 DEG C dried, powder annealing 2 hours, obtain white TiO
2powder.
Embodiment 3:
The ammonium titanium fluoride of 0.99g is added in 50 ml ionized waters; The H of 2 g is added in above-mentioned solution
3bO
3; In above-mentioned solution, add the polyoxyethylene-poly-oxypropylene polyoxyethylene of 15 g, be stirred to and dissolve completely; Placed 10 hours at 50 DEG C by solution, then respectively wash 5 times with deionized water, alcohol, 60 degree dry 12 hours; By 600 DEG C dried, powder annealing 1 hour, obtain white TiO
2powder.
Embodiment 4:
The ammonium titanium fluoride of 3g is added in 50 ml ionized waters; The H of 0.6183 g is added in above-mentioned solution
3bO
3; In above-mentioned solution, add the APEO of 5 g, be stirred to and dissolve completely; Placed 24 hours at 40 DEG C by solution, then respectively wash 5 times with deionized water, alcohol, 60 degree dry 12 hours; By 400 DEG C dried, powder annealing 3 hours, obtain white TiO
2powder.
Claims (3)
1. a preparation method for titanic oxide microsphere photocatalyst, is characterized in that, concrete steps are as follows:
Ammonium titanium fluoride is added in deionized water or ethanol; Boric acid (H is added in above-mentioned solution
3bO
3), then add polymer template agent, be stirred to and dissolve completely; Solution is placed 10 ~ 24 hours at 30 ~ 80 DEG C, then respectively washes 5 times with deionized water, alcohol, 60 DEG C of dryings 12 hours; By 400 ~ 600 DEG C dried, powder annealing 1 ~ 5 hour, gained white powder was titanic oxide microsphere photocatalyst.
2. the preparation method of a kind of titanic oxide microsphere photocatalyst according to claim 1, is characterized in that, the concentration of described ammonium titanium fluoride is 0.1 ~ 0.5 mol/L; Described boric acid and the mol ratio of ammonium titanium fluoride are 5:1 ~ 1:2.
3. the preparation method of a kind of titanic oxide microsphere photocatalyst according to claim 1, it is characterized in that, described polymer template agent is APEO or triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene or bi-block copolymer polystyrene-polyoxyethylene; The mass percent of described polymer template agent is 0.1 ~ 0.5%.
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| CN201410661332.4A CN104383903A (en) | 2014-11-19 | 2014-11-19 | Preparation method of titanium dioxide microsphere photocatalyst |
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| CN201410661332.4A CN104383903A (en) | 2014-11-19 | 2014-11-19 | Preparation method of titanium dioxide microsphere photocatalyst |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102354606A (en) * | 2011-09-24 | 2012-02-15 | 东莞电子科技大学电子信息工程研究院 | Preparation method of photoanode of dye-sensitized solar cell |
-
2014
- 2014-11-19 CN CN201410661332.4A patent/CN104383903A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102354606A (en) * | 2011-09-24 | 2012-02-15 | 东莞电子科技大学电子信息工程研究院 | Preparation method of photoanode of dye-sensitized solar cell |
Non-Patent Citations (3)
| Title |
|---|
| SHIGEHITO DEKI ET AL.: "High Quality Monodispersed Oxide Nanoparticles Prepared by the Liquid Phase Deposition Method in Aqueous Polymer Solution", 《ECS TRANSACTIONS》, vol. 3, no. 9, 31 December 2006 (2006-12-31), pages 29 - 35 * |
| YOSHITAKE MASUDA ET AL.: "Nanocrystal Assembled TiO2 Particles Prepared from Aqueous Solution", 《CRYSTAL GROWTH & DESIGN》, vol. 8, no. 9, 26 July 2008 (2008-07-26), pages 3213 - 3218 * |
| 杨儒等: "锐钛矿型纳米TiO2粉体的精细结构及其光催化降解苯酚的活性", 《催化学报》, vol. 24, no. 8, 31 August 2003 (2003-08-31), pages 629 - 634 * |
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Application publication date: 20150304 |
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