CN1600424A - Photocatalyst responding to visible light, and preparation method and application - Google Patents
Photocatalyst responding to visible light, and preparation method and application Download PDFInfo
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Abstract
A semiconductor photocatalyst responsive to visual light is composed of the particles of metallic oxide chosen from iron oxide, nickel oxide, cabolt oide, copper oxide, etc, the non-metal element chosen from N, C, S, B and P and semiconductor nanoparticles chosen frmo TiO2, SnO2, ZnO, CdS and WO3.
Description
Technical field
The present invention relates to a kind of photochemical catalyst, particularly relate to a kind of visible light-responded photochemical catalyst that has.
The invention still further relates to above-mentioned Preparation of catalysts method.
The invention still further relates to the purposes of above-mentioned catalyst.
Background technology
As everyone knows, along with industrial expansion, problem of environmental pollution is very serious.In China, nearly 1/2 river is polluted, and 1.64 hundred million people drink the serious water of organic contamination, and indoor-outdoor air is seriously polluted.The wherein difficult proportion that decomposes toxic organic pollutant is also in rapid increase, and many toxic organic pollutants can't be handled with existing microbial technique, or can't thoroughly remove.
In recent years, the Nano semiconductor photocatalysis technology has been obtained very big progress, and many nano semiconductor materials are as titanium dioxide (TiO
2), tin ash (SnO2), zinc oxide (ZnO), cadmium sulfide (CdS), tungsten oxide (WO
3), metatianate and composite semiconductor etc. all are found this type of difficult toxic organic pollutant that decomposes of can degrading effectively, this type of document has " organic chemistry " magazine, 1999,64, the article of delivering on the 8509-8524 " photocatalytic degradation 4-chlorophenol " (X.J.Li, J.W.Cubbage, T.A.Tetzlaff, W.S.Jenks, Photocatalytic Degradation of 4-Chlorophenol.l.The Hydroquinone Pathway, J.Org.Chem.), " Lang Gemiuer " magazine, 1998,14, the article of delivering on the 3551-3555 " photo catalytic reduction of nitro organic matter in illumination titanium dioxide system " (J.L.Ferry Photocatalytic Reduction ofNitro Organics over Illuminated Titanium Dioxide:Role ofthe TiO
2Surface.Langmuir), " chemistry summary " magazine, 1995,95, the article of delivering on the 69-96 " environmental applications of conductor photocatalysis " (M.R.Hoffmann, S.T.Martin, W.Choi, D.W.Bahnemann, Environmental Application of Semniconductor Photocatalysis, Chem.Rev.).Wherein titanium deoxide catalyst has the photocatalysis efficiency height because of it, good stability, advantage such as low price and be subjected to extensive studies and application.But because titanium dioxide has the energy gap of 3.2eV, make the ultraviolet light that has only wavelength to be less than 385nm effectively to excite, and ultraviolet light only occupies the ratio of 3-5% in sunshine, as use artificial ultraviolet source can expend a large amount of electric energy, therefore, attempt purifying air or handling waste water to environmental protection with energy-conservationly all have and important meaning with low price, visible light with low cost or sunshine.It is visible light-responded that photochemical catalyst is had, and can is a difficult problem that needs to be resolved hurrily by excited by visible light effectively.Some researchers have taked the method for dye sensitization, the dye load that can absorb visible light effectively utilizes visible light at catalyst surface, this type of document has " Chinese science " magazine, 2002,45, the article of delivering on the 421-425 " 2; 4-two chlorophenols are at the semiconductor surface visible light photocatalytic degradation of sensitization " (X.Z.Li, W.Zhao, J.C.Zhao, Visible light-sensitized semiconductorphotocatalytic degradation of 2,4-dichlorophenol, Sci.China B), the semiconductor (as cadmium sulfide) that will have less bandwidth loads on titanium dioxide surface, this type of document has " physical chemistry " magazine, 1995,99, the article of delivering on the 10329-10335 " with titanium dioxide key cadmium sulfide nano-particles even " (D.Lawless with dual-use function block, S.Kapoor, D.Meisel, Bifunctional capping of Cds nanoparticles and Binding to TiO
2J.Phys.Chem.) or with some metal ion load on semiconductor surface, this type of document has " JACS " magazine, 1982,104, the article of delivering on the 2996-3002 " water-splitting of visible light-inducing in the colloidal tio 2 solution of chromium load " (E.Borgarello, J.Kiwi, M.Gratzel, E.Pelizzetti, M.Visca, Visible light induced water cleavage in colloidalsolutions of chromium-doped titanium dioxide particles, J.Am.Chem.Soc.).Ubiquity foreign ion is introduced system, catalyst easily by photoetch, problem that photocatalysis efficiency is low though these methods can be utilized titanium dioxide under visible light radiation.In the world the phase-doped modified semiconductor catalyst of non-metallic body was particularly paid close attention in recent years, represent document that " science " magazine, 2001,293 are arranged, the article of delivering on the 269-271 " the TiO 2 visible light photocatalysis that nitrogen mixes " (R.Asahi, T.Morikawa, T.Ohwaki, K.Aoki, T.Taga, Visible-light photocatalysis in nitrogen-doped titanium oxides, Science), at N
2Utilize the method for the titanium dioxide target of ion sputtering to prepare the titanium deoxide catalyst that nitrogen mixes in/Ar the atmosphere, but these methods exist complex manufacturing technology, the cost of manufacture problem of higher.
Summary of the invention
The object of the present invention is to provide a kind of visible light-responded photochemical catalyst that has, this bulk phase-doped semiconductor nano photochemical catalyst, can be effectively by excited by visible light, can keep the stability of semiconductor nano photochemical catalyst again and keep advantages of high catalytic activity, manufacturing process is simple simultaneously, cost is lower.
Catalyst provided by the invention is made up of metal oxide particle, nonmetalloid, semi-conductor nano particles, it is characterized in that non-metallic atom is replaced part body phase atom, at catalyst surface loading section metal oxide.
Wherein metal oxide is materials such as iron oxide, rubidium oxide, nickel oxide, cobalt oxide, and its particle diameter is between 1 nanometer to 10 micron, and the mass ratio of metal oxide and semiconductor carrier is 0.5-100mg/g.
Nonmetalloid is nitrogen, carbon, sulphur, boron, phosphorus etc., and the mass ratio of nonmetal oxide and semiconductor carrier is 0.5-100mg/g.
Semi-conductor nano particles is titanium dioxide (TiO
2), tin ash (SnO
2), zinc oxide (ZnO), cadmium sulfide (CdS), tungstic acid (WO
3), metatianate and composite semiconductor etc. have the material of photocatalytic activity, its particle diameter is between 5 nanometer to 1 microns.
Preparation method with visible light-responded photochemical catalyst of the present invention is as follows:
(1) preparation of metal oxide and nonmetalloid storing solution
Prepare the slaine of 0.01-0.1M and the methanol solution of non-metal salt respectively, standby.This solution compound method belongs to conventional compound method.
(2) preparation of semi-conductor nano particles
Compound that preparation titanium dioxide semiconductor nano material is required is as titanium dioxide (TiO
2), tin ash (SnO
2), zinc oxide (ZnO), cadmium sulfide (CdS), tungstic acid (WO
3) wait material with photocatalytic activity, get in the methanol solution of 0.1～0.5 mole of slaine that under vigorous stirring, in 10 minutes-30 minutes, is added to the 0.001～0.1M for preparing in advance and non-metal salt, in this mixed solution, added the HNO of 0.1ml 5M every 5～10 minutes
3The aqueous solution is hydrolyzed, and stirs at normal temperatures 5～12 hours, obtains semiconductor nano colloidal sol, places sedimentation aging 1～10 day, and after the dry out solvent, roasting must have visible light-responded photochemical catalyst semi-conductor nano particles powder in 300～900 ℃ of high temperature.
The present invention has the photocatalysis treatment that visible light-responded photochemical catalyst can be used for organic pollution, heavy metal ion etc. in air, waste water, surface water and the drinking water, also can be used for light-catalyzed reactions such as photocatalysis is synthetic, photocatalysis fixed nitrogen.
Of the present invention have visible light responsive photocatalyst can be effectively by excited by visible light, Application of Catalyst is extended to the visible region, utilize visible light to realize organic pollution in the deodorizing of family and hospital or other public arena, sterilization and the decomposition air, manufacturing process is simple simultaneously, cost is lower, promotes light-catalyzed reaction further to push practicability to.
Description of drawings
Specify effect of the present invention below in conjunction with accompanying drawing.
Fig. 1,2,4,6-trichlorophenol 1 * 10
-4The photocatalytic degradation reaction result of M under radiation of visible light, among the figure:
Curve 1-does not have photochemical catalyst;
Blank titanium dioxide/the l of curve 2-1g;
Curve 3-dark reaction, 1g sample/liter (by preparation among the embodiment 2);
Curve 4-1g sample/liter (by preparation among the embodiment 2);
Illumination experiment condition a: halogen lamp is placed in the double glazing condensation sleeve pipe, on every side around recirculated cooling water.(λ＞420nm) places the chuck outside to excise the following light of 420nm fully and guarantee that reaction only carries out under visible light for cut-off type optical filter.Following experiment condition is identical.
Fig. 2, dichlorobenzoic acid 1 * 10
-4The photocatalytic degradation reaction result of M under radiation of visible light, among the figure:
Curve 1-does not have photochemical catalyst;
Blank titanium dioxide/the l of curve 2-1g;
Curve 3-dark reaction, 1g sample/liter (by preparation among the embodiment 5);
Curve 4-1g sample/liter (by preparation among the embodiment 5).
Fig. 3, catalyst (the 1g sample/liter) (by preparation among the embodiment 2) 5 oxidative degradation 2,4 that circulates continuously, 6-trichlorophenol (1 * 10
-4M) photocatalytic activity result.
Fig. 4,2,4,6-trichlorophenol 1 * 10
-4M under radiation of visible light in the photocatalytic degradation dechlorination result on catalyst (in preparation) surface by embodiment 6.
The specific embodiment
In the 30ml absolute methanol solution, add 50mg copper sulphate (0.01 mol) and 50mg boric acid (0.027 mol), fully dissolving.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 100 ℃ and is drying to obtain photochemical catalyst.
In the 30ml absolute methanol solution, add 50mg nickelous sulfate (0.01 mol) and 50mg boric acid (0.024 mol), fully dissolving.With syringe with 10ml titanium salt solution (0.29 mole) solution about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
In the 30ml absolute methanol solution, add 50mg four hydration indium trichlorides (5.6 * 10
-3Mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
In the 30ml absolute methanol solution, add 50mg cobaltous sulfate (1 * 10
-2Mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 5
In the 30ml absolute methanol solution, add 100mg copper sulphate (0.02 mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 6
In the 30ml absolute methanol solution, add 50mg nickelous sulfate (0.01 mol) and 100mg boric acid (0.048 mol), fully dissolving.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 7
In the 30ml absolute methanol solution, add 50mg bismuth chloride (5 * 10
-3Mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 8
In the 30ml absolute methanol solution, add 50mg frerrous chloride (0.0 1 mol) and 50mg boric acid (0.027 mol), fully dissolving.With syringe with 10ml tin chloride solution (0.35 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 100 ℃ and is drying to obtain photochemical catalyst.
Embodiment 9
In the 30ml absolute methanol solution, add 55mg caddy (0.01 mol) and 50mg sodium phosphate (0.0 12 mol), fully dissolving.With syringe with 1 0ml titanium salt solution (0.29 mole) solution about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 10
In the 30ml absolute methanol solution, add 50mg silver nitrate (0.01 mol) and 50mg sodium carbonate (0.016 mol), fully dissolving.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The hydrogen sulfide of 0.1 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 11
In the 30ml absolute methanol solution, add 50mg rubidium chloride (0.009 mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 12
In the 30ml absolute methanol solution, add 100mg copper sulphate (0.02 mol) and vulcanized sodium (0.021 mol), fully dissolving.With syringe with 10ml titanium salt solution (0.29 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 13
In the 30ml absolute methanol solution, add 50mg nickelous sulfate (0.01 mol) and 100mg boric acid (0.048 mol), fully dissolving.With syringe with 10ml tungsten salt solution (0.20 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
Embodiment 14
In the 30ml absolute methanol solution, add 50mg bismuth chloride (5 * 10
-3Mol) and 50mg ammonium chloride (3 * 10
-2Mol), dissolving fully.With syringe with 10ml caddy (0.20 mole) about 20 fens clock times, under the vigorous stirring, slowly be added drop-wise in this storing solution, add the back that finishes and continue to stir 2 hours.The salpeter solution of 5 mol is joined in the reactant liquor with the speed every 10 minutes 0.1ml, through making colloidal sol in 12 hours, and placed aging 7 days.The solid that this colloidal sol solvent evaporates is obtained is deposited in 120 ℃ of dryings, is heated to 700 ℃ and kept 5 hours in Muffle furnace, promptly obtains photochemical catalyst after the cooling.
In conjunction with the accompanying drawings: the curve 1 among Fig. 1 is the blank light reaction of catalyst-free under the radiation of visible light, photodissociation 180min 2,4, and the concentration of 6-trichlorophenol almost there is not variation.Curve 2 is that blank titanium dioxide (Degussa Co.P25) exists down, and the degraded of trichlorophenol almost there is not generation yet.Curve 3 is in the dark reaction of no visible light photograph, and through the 180min reaction, the concentration of trichlorophenol does not almost change in the presence of catalyst (preparation in by embodiment 2).Curve 4 is in the presence of catalyst (preparation in by embodiment 2), and radiation of visible light 150min trichlorophenol has degraded about 90%.
Fig. 3 has provided catalyst (1g sample/liter) (by preparation among the embodiment 2) circulation 5 times 2,4, the degradation results of 6-trichlorophenol.First three time circulation light reaction 240min, the trichlorophenol degraded can reach more than 90%, and the catalytic activity of catalyst does not have to reduce substantially.Latter two circulation light reaction 240min, 2,4, the degraded of 6-trichlorophenol slightly reduces, and can reach more than 80%, if prolong optical response time to 300min, then the degraded of trichlorophenol also can reach more than 90%.
Fig. 4 has provided 2,4,6-trichlorophenol 1 * 10
-4M under radiation of visible light in the photocatalytic degradation dechlorination result on catalyst (in preparation) surface by embodiment 6.Chlorine through illumination 240min trichlorophenol is taken off about 80%, is free in the solution with the form of chlorion.
Claims (4)
1, a kind of have a visible light-responded photochemical catalyst, is made up of metal oxide particle, nonmetalloid, semi-conductor nano particles, it is characterized in that non-metallic atom is replaced part body phase atom, at catalyst surface loading section metal oxide;
Wherein said metal oxide is iron oxide, rubidium oxide, nickel oxide, cobalt oxide, cadmium oxide, cupric oxide, silver oxide, indium oxide, bismuth oxide, the mass ratio of metal oxide and semiconductor carrier is 0.5～100mg/g, and its metallic particles diameter is between 1 nanometer to 1 micron;
Wherein said nonmetalloid is nitrogen, carbon, sulphur, boron or phosphorus, and the mass ratio of nonmetalloid and semiconductor carrier is 0.5～100mg/g.
Wherein said semi-conductor nano particles is the material with photocatalytic activity: titanium dioxide, tin ash, zinc oxide, cadmium sulfide, tungstic acid, its particle diameter is between 5 nanometer to 10 microns.
2, according to a kind of photochemical catalyst of claim 1, it is characterized in that: light reaction is carried out under visible light, ultraviolet light or sunshine.
3, a kind of method for preparing the described photochemical catalyst of claim 1 the steps include:
A) preparation of metal oxide and nonmetalloid storing solution
Prepare the slaine of 0.001-0.1M and the methanol solution of non-metal salt respectively, standby;
B) preparation of semi-conductor nano particles
0.1～0.5 mole of the compound of semiconductor nano material was added in 10 minutes-30 minutes under vigorous stirring in the methanol solution of the slaine of the 0.001～0.1M for preparing in advance and non-metal salt, in this mixed solution, added the HNO of 0.1ml 5M every 5～10 minutes
3The aqueous solution is hydrolyzed, and stirs at normal temperatures 5～12 hours, obtains semiconductor nano colloidal sol, places sedimentation aging 1～10 day, and after the dry out solvent, roasting in 300～900 ℃ of high temperature obtains having visible light-responded photochemical catalyst semi-conductor nano particles powder.
4, the photocatalysis treatment that is used for air, waste water, surface water and drinking water organic pollution, heavy metal ion according to the described photochemical catalyst of above-mentioned each claim; Be used for that photocatalysis is synthetic, the light-catalyzed reaction of photocatalysis fixed nitrogen.
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