CN101791564B - High-activity TiO2-based photocatalyst and method for preparing same - Google Patents

High-activity TiO2-based photocatalyst and method for preparing same Download PDF

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CN101791564B
CN101791564B CN2010101142001A CN201010114200A CN101791564B CN 101791564 B CN101791564 B CN 101791564B CN 2010101142001 A CN2010101142001 A CN 2010101142001A CN 201010114200 A CN201010114200 A CN 201010114200A CN 101791564 B CN101791564 B CN 101791564B
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tio
based photocatalyst
tio2
room temperature
activity
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CN101791564A (en
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丛野
李轩科
别望望
董志军
袁观明
崔正威
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to high-activity TiO2-based photocatalyst and a method for preparing the same. According to the technical scheme, the method for preparing the high-activity TiO2-based photocatalyst comprises the following steps: mixing 0.5-20 percent by weight of carbon material with 80-99.5 percent by weight of metal salt, adding metallic titanium powder to the mixture according to the molar ratio of 0.5-10:1 of C and Ti, grinding evenly the new mixture, putting the ground mixture to an alumina crucible, heating the ground mixture to 600-1200 DEG C at the heating rate of 0.5-20 DEG C per minute under the protection of argon, preserving the heat of the ground mixture for 0.1-50h, cooling the ground mixture to room temperature, washing and filtering the product of reaction in the alumina crucible, drying the product of reaction, putting the product of reaction in a tube furnace, oxidizing the product of reaction at 100-500 DEG C for 0.1-48h in the atmosphere of oxidative gas, and cooling the oxidized product of reaction to room temperature to obtain the high-activity TiO2-based photocatalyst. The process for preparing the TiO2-based photocatalyst needs low cost, and the TiO2-based photocatalyst prepared with the process has controllable structure, shape and components and high visible light and ultraviolet light catalyzing activity, can strongly absorb organic pollutant and is easy to recycle. The TiO2 and the carrier are combined firmly and are not easy to be separated from each other.

Description

A kind of highly active TiO 2Based photocatalyst and preparation method thereof
Technical field
The invention belongs to a kind of preparation method of photochemical catalyst, be specifically related to a kind of highly active TiO 2Based photocatalyst and preparation method thereof.
Background technology
Along with The development in society and economy, environmental problem has been put on the agenda of national governments as a unavoidable major issue.Photocatalysis is with its room temperature deep reaction and can directly utilize solar energy to drive special performances such as reaction as light source, becomes a kind of ideal environment pollution control technology and clear energy sources production technology.TiO 2With its high activity, safety non-toxic, chemical property stable (chemically-resistant and photoetch), low cost and other advantages, be acknowledged as the environment-friendly type catalysis material of the tool exploitation future in environment pollution treatment field.
But will the optically catalytic TiO 2 technical development be become the environmental pollution treatment technology of a practicality, following problem also needs to be resolved hurrily: (1) photo-quantum efficiency is low, simple TiO 2The height of combined efficiency again that the light induced electron-hole of photochemical catalyst is right, photocatalysis performance is outstanding, therefore is difficult to industrial waste gas and the waste water that treating capacity is big and concentration is higher; (2) solar energy utilization ratio is low, and promptly photocatalytic activity is lower under the visible light effect, and this is because TiO 2Energy gap broad (anatase is 3.2eV, and rutile is 3.0eV), only can absorb the ultraviolet light of sunshine medium wavelength, yet the energy of sunshine medium ultraviolet light only accounts for 3-5% less than 380nm; (3) single titanium dioxide is relatively poor to the organic pollutant adsorption ability; And pending pollutant levels are lower in the general water; Pollutant and titanium dioxide contact frequency are low during photocatalytic degradation, cause reaction rate slower, need the long time just can reach light-catalysed purpose; (4) fixing condition is harsh, because titanium dioxide optical catalyst is prone to cohesion, is difficult for reclaiming, after therefore need being carried on the appropriate carriers or being fixed to the surface of base material with suitable process for fixation, and the competence exertion photocatalysis.The method of conventional employing sol-gel or hydro-thermal at some carrier surfaces, exists coating inhomogeneous and easy from problems such as carrier come off titanium dioxide-coated; Or adopt methods such as powder sintering, heat spray that titania powder is sprayed on substrate surface, and production of coatings is complicated, and process conditions are harsh, and cost is higher.
Summary of the invention
The present invention is intended to overcome the prior art defective, and purpose provides the low highly active TiO of a kind of cost 2The preparation method of based photocatalyst; Prepared photocatalyst structure, form and composition are controlled, and it is active to have higher visible light and a ultraviolet catalytic, strong to the organic pollutant adsorption ability, combine firmly to be not easy to come off between titanium dioxide and the carrier, and catalyst recovery makes things convenient for.
For realizing above-mentioned purpose; The technical scheme that the present invention adopts is: earlier the raw material of wood-charcoal material of 0.5～20wt% and the slaine of 80～99.5wt% are mixed, the mol ratio of in above-mentioned compound, pressing C: Ti is (0.5～10): 1 adds metallic titanium powder, grinds evenly; Place in the alumina crucible; Heating rate with 0.5～20 ℃/min under argon shield is heated to 600～1200 ℃, and insulation 0.1～50h is cooled to room temperature; With product washing and filtration in the crucible, be placed on after the drying in the tube furnace, in the oxidizing gas atmosphere, oxidation 0.1～48h under 100～500 ℃ of conditions is cooled to room temperature then, obtains highly active TiO again 2Based photocatalyst.This photochemical catalyst is TiO 2/ TiC/C ternary composite photo-catalyst, TiO 2/ C binary composite photo-catalyst, TiO 2/ TiC binary composite photo-catalyst, TiO 2A kind of in the monobasic photochemical catalyst.
Wherein: the raw material of wood-charcoal material is a kind of in CNT, charcoal fiber, carbon black, the graphite powder; Washing is with distilled water washing or in water, boils, and is washed till not observe till the white precipitate in filtrating with the titration of 0.05mol/L liquor argenti nitratis ophthalmicus; Slaine is more than one in alkali-metal chloride, fluoride, nitrate, the sulfate; Oxidizing gas is a kind of in air, oxygen, the steam.
Because adopt technique scheme, the present invention compares with prior art, has the following advantages:
1, the method for the first fused salt rear oxidation of the present invention's employing, cost is low;
2, prepared photocatalyst structure, form and the composition of the present invention is controlled, can be prepared into forms such as nanotube, fiber, powder, structure and composition or with TiO 2/ TiC/C ternary is main or with TiO 2/ C binary is main or with TiO 2/ TiC binary is main or with TiO 2Monobasic is main;
3, the prepared photochemical catalyst of the present invention strengthens the organic pollutant adsorption ability, under visible light and ultraviolet light, all has higher photocatalytic activity, has improved the utilization ratio of solar energy, the organic pollution of certain kind of effectively degrading;
4, titanium dioxide is even in the carbon matrix surface distributed;
5, titanium dioxide combines with chemical bond with carbon matrix, is connected firmly, and can not come off, and catalyst recovery is convenient.
The specific embodiment
Below in conjunction with the specific embodiment the present invention being described further, is not the restriction to the scope of protection.
Below the described washing of each embodiment all be with distilled water washing or in water, boil that be washed till and do not observe till the white precipitate in filtrating with the titration of 0.05mol/L liquor argenti nitratis ophthalmicus, each embodiment will not give unnecessary details.
Embodiment 1:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 0.5～5wt% mixes with the lithium chloride of 95～99.5wt% earlier; The mol ratio of in above-mentioned compound, pressing C: Ti is (1～5): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 0.5～5 ℃/min under argon shield is heated to 600～800 ℃; Insulation 0.1～5h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 100～250 ℃ of conditions oxidation 1～5h, be cooled to room temperature then, obtain TiO 2/ TiC/C ternary composite photo-catalyst.At structure expression TiO 2C is a CNT among the/TiC/C; TiO 2Be anatase phase, TiO 2Be evenly distributed in carbon nano tube surface, densification.
Embodiment 2:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 10～20wt% mixes with potassium chloride and two kinds of salt of lithium chloride of 80～90wt% earlier, and wherein the mass ratio of potassium chloride and lithium chloride is (50～60): (40～50).The mol ratio of in the compound of above-mentioned CNT and two kinds of salt, pressing C: Ti is (5～10): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 20～50h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 250～400 ℃ of conditions oxidation 5～12h, be cooled to room temperature then, obtain TiO 2/ C binary composite photo-catalyst.At structure expression TiO 2C is a CNT among the/C; TiO 2Be anatase phase, TiO 2Be evenly distributed in carbon nano tube surface, densification.
Embodiment 3:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 5～10wt% mixes with potassium chloride and two kinds of salt of lithium chloride of 90～95wt% earlier, and wherein the mass ratio of potassium chloride and lithium chloride is (50～60): (40～50).The mol ratio of in the compound of above-mentioned CNT and two kinds of salt, pressing C: Ti is (0.5～1): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 1000～1200 ℃; Insulation 5～10h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 250～400 ℃ of conditions oxidation 12～24h, be cooled to room temperature then, obtain TiO 2The monobasic photochemical catalyst.TiO 2Be anatase phase.
Embodiment 4:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 0.5～5wt% mixes with potassium chloride and two kinds of salt of sodium sulphate of 95～99.5wt% earlier, and wherein the mass ratio of potassium chloride and sodium sulphate is (80～90): (10～20).The mol ratio of in the compound of above-mentioned CNT and two kinds of salt, pressing C: Ti is (0.5～1): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 0.5～5 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 10～20h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 100～250 ℃ of conditions oxidation 0.1～1h, be cooled to room temperature then, obtain TiO 2/ TiC binary composite photo-catalyst.TiO 2Be anatase phase.
Embodiment 5:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 5～10wt% mixes with four kinds of salt of potassium chloride, lithium chloride, lithium nitrate, potassium fluoride of 90～95wt% earlier, and wherein the mass ratio of potassium chloride, lithium chloride, lithium nitrate, potassium fluoride is (45～55): (25～35): (15～25): (5～10).The mol ratio of in the compound of above-mentioned CNT and four kinds of salt, pressing C: Ti is (0.5～1): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 1000～1200 ℃; Insulation 5～10h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 250～400 ℃ of conditions oxidation 24～48h, be cooled to room temperature then, obtain TiO 2The monobasic photochemical catalyst.TiO 2Be anatase phase.
Embodiment 6:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.CNT with 5～10wt% mixes with potassium chloride and two kinds of salt of lithium chloride of 90～95wt% earlier, and wherein the mass ratio of potassium chloride and lithium chloride is (50～60): (40～50).The mol ratio of in the compound of above-mentioned CNT and two kinds of salt, pressing C: Ti is (5～10): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 10～20 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 5～10h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in steam under 250～400 ℃ of conditions oxidation 1～5h, be cooled to room temperature then, obtain TiO 2/ TiC/C ternary composite photo-catalyst.At structure expression TiO 2C is a CNT among the/TiC/C; TiO 2Be anatase phase, TiO 2Be evenly distributed in carbon nano tube surface, densification.
Embodiment 7:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.Charcoal fiber with 0.5～5wt% mixes with three kinds of salt of potassium chloride, lithium chloride, potassium fluoride of 95～99.5wt% earlier, and wherein the mass ratio of potassium chloride, lithium chloride and potassium fluoride is (45～55): (40～50): (1～5).The mol ratio of in the compound of above-mentioned charcoal fiber and three kinds of salt, pressing C: Ti is (1～5): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 0.1～5h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in oxygen under 250～400 ℃ of conditions oxidation 0.1～1h, be cooled to room temperature then, obtain TiO 2/ TiC/C ternary composite photo-catalyst.At structure expression TiO 2C is the charcoal fiber among the/TiC/C; TiO 2Be anatase phase, TiO 2Be evenly distributed at carbon fiber surface, densification.
Embodiment 8:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.Charcoal fiber with 5～10wt% mixes with two kinds of salt of sodium chloride, potassium fluoride of 90～95wt% earlier, and wherein the mass ratio of sodium chloride and potassium fluoride is (70～90): (10～30).The mol ratio of in the compound of above-mentioned charcoal fiber and two kinds of salt, pressing C: Ti is (1～5): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 0.5～5 ℃/min under argon shield is heated to 1000～1200 ℃; Insulation 5～10h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 100～250 ℃ of conditions oxidation 12～24h, be cooled to room temperature then, obtain TiO 2/ TiC/C ternary composite photo-catalyst.At structure expression TiO 2C is the charcoal fiber among the/TiC/C; TiO 2Be anatase phase, TiO 2Be evenly distributed at carbon fiber surface, densification.
Embodiment 9:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.Charcoal fiber with 0.5～5wt% mixes with two kinds of salt of potassium chloride, potassium fluoride of 95～99.5wt% earlier, and wherein the mass ratio of potassium chloride and potassium fluoride is (80～90): (10～20).The mol ratio of in the compound of above-mentioned charcoal fiber and two kinds of salt, pressing C: Ti is (5～10): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 0.1～5h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 400～500 ℃ of conditions oxidation 24～48h, be cooled to room temperature then, obtain TiO 2The monobasic photochemical catalyst.TiO 2Be anatase phase.
Embodiment 10:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.Carbon black with 5～10wt% mixes with two kinds of salt of potassium chloride, lithium chloride of 90～95wt% earlier, and wherein the mass ratio of potassium chloride and lithium chloride is (50～60): (40～50).The mol ratio of in the compound of above-mentioned carbon black and two kinds of salt, pressing C: Ti is (1～5): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 5～10 ℃/min under argon shield is heated to 600～800 ℃; Insulation 5～10h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 250～400 ℃ of conditions oxidation 1～5h, be cooled to room temperature then, obtain TiO 2/ C binary composite photo-catalyst.At structure expression TiO 2C is a carbon black among the/C; TiO 2Be anatase phase, TiO 2Be evenly distributed at carbon blacksurface, densification.
Embodiment 11:
A kind of highly active TiO 2Based photocatalyst and preparation method thereof.Graphite powder with 0.5～5wt% mixes with two kinds of salt of potassium chloride, lithium chloride of 95～99.5wt% earlier, and wherein the mass ratio of potassium chloride and lithium chloride is (50～60): (40～50).The mol ratio of in the compound of above-mentioned graphite powder and two kinds of salt, pressing C: Ti is (1～5): 1 adds metallic titanium powder; Grind evenly, place in the alumina crucible, the heating rate with 0.5～5 ℃/min under argon shield is heated to 800～1000 ℃; Insulation 0.1～5h is cooled to room temperature; With product washing in the crucible with filter, be placed on after the drying in the tube furnace again, in air under 100～250 ℃ of conditions oxidation 5～12h, be cooled to room temperature then, obtain TiO 2/ TiC/C ternary composite photo-catalyst.At structure expression TiO 2C is a graphite powder among the/TiC/C; TiO 2Be anatase phase, TiO 2Even, fine and close in the graphite powder surface distributed.
In the above-mentioned specific embodiment, according to the ratio of 1.5g/L, respectively that each embodiment is prepared TiO 2Based photocatalyst joins in the methylene blue or rhodamine B organic dyestuff solution of 20mg/L, with radiation of visible light 5h or use UV-irradiation 2h.Experiment shows, prepared TiO 2Based photocatalyst all shows than the high activity of commercial Degussa P25 type titanium dioxide methylene blue light and rhodamine B catalysis decolouring.
This specific embodiment has the following advantages:
The method of the first fused salt rear oxidation that 1, adopts, cost is low;
2, prepared photocatalyst structure, form and composition are controlled, can be prepared into forms such as nanotube, fiber, powder, structure and composition or with TiO 2/ TiC/C ternary is main or with TiO 2/ C binary is main or with TiO 2/ TiC binary is main or with TiO 2Monobasic is main;
3, prepared photochemical catalyst strengthens the organic pollutant adsorption ability, under visible light and ultraviolet light, all has higher photocatalytic activity, has improved the utilization ratio of solar energy, the organic pollution of certain kind of effectively degrading;
4, titanium dioxide is even in the carbon matrix surface distributed;
5, titanium dioxide combines with chemical bond with carbon matrix, is connected firmly, and can not come off, and catalyst recovery is convenient.

Claims (2)

1. highly active TiO 2The preparation method of based photocatalyst; It is characterized in that: earlier the CNT of 0.5～20wt% and the slaine of 80～99.5wt% are mixed, the mol ratio of in above-mentioned compound, pressing C: Ti is (0.5～10): 1 adds metallic titanium powder, grinds evenly; Place in the alumina crucible; Heating rate with 0.5～20 ℃/min under argon shield is heated to 600～1200 ℃, and insulation 0.1～50h is cooled to room temperature; With product washing and filtration in the crucible, be placed on after the drying in the tube furnace, in the oxidizing gas atmosphere, oxidation 0.1～48h under 100～500 ℃ of conditions is cooled to room temperature then, obtains highly active TiO again 2Based photocatalyst;
Described slaine is more than one in alkali-metal chloride, fluoride, nitrate, the sulfate;
Described oxidizing gas is a kind of in air, oxygen, the steam.
2. highly active TiO according to claim 1 2The preparation method of based photocatalyst is characterized in that described washing is with distilled water washing or in water, boils, and is washed till not observe till the white precipitate in filtrating with the titration of 0.05mol/L liquor argenti nitratis ophthalmicus.
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US9278337B2 (en) * 2011-05-19 2016-03-08 Nanoptek Corporation Visible light titania photocatalyst, method for making same, and processes for use thereof
CN110227527A (en) * 2018-03-05 2019-09-13 武汉大学 It is a kind of to prepare visible light-responded doping TiO2High-temperature fusion salt method
CN109847734B (en) * 2018-11-30 2021-10-29 黄山学院 Preparation method of carbon fiber loaded titanium dioxide nanotube composite material
CN111036254B (en) * 2019-12-31 2021-06-22 中南大学 Preparation method of titanium dioxide and titanium carbide loaded carbon fiber composite catalytic functional material
CN110975904B (en) * 2019-12-31 2021-06-22 中南大学 CFs @ TiC/TiO2Composite material and preparation method and application thereof

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