CN1806916A - Composite bismuth vanadium photocatalyst supported by nickel oxide and preparation method thereof - Google Patents
Composite bismuth vanadium photocatalyst supported by nickel oxide and preparation method thereof Download PDFInfo
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- CN1806916A CN1806916A CNA2006100240937A CN200610024093A CN1806916A CN 1806916 A CN1806916 A CN 1806916A CN A2006100240937 A CNA2006100240937 A CN A2006100240937A CN 200610024093 A CN200610024093 A CN 200610024093A CN 1806916 A CN1806916 A CN 1806916A
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- pucherite
- nickel oxide
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention relates the method for preparation of pucherite composite photocatalyst loaded on nickel oxide. The photocatalyst comprises semi-conductor pucherite particle and nickel oxide particle. The pucherite is monoclinic crystal system scheelite structure, and the diameter is 100nm-5mum. The grain diameter of nickel oxide is 10nm-100nm. The mass ratio of nickel oxide and pucherite is 1-100mg/g. The specific surface area of composite photocatalyst is 0.5-5m2/g. The said photocatalyst can effectively degrade the noxious and harmful chemical under the ultraviolet light, visible light and natural light radiating. And the photocatalyst is easy to separate and recover.
Description
Technical field
The present invention relates to a kind of nickel oxide loaded composite bismuth vanadium photocatalyst and preparation method thereof, the composite photo-catalyst of preparation is at a kind of powder that comprises that pucherite and nickel oxide are formed, under visible light, have photocatalytic activity, can high efficiency photocatalysis degraded toxic and harmful substance.Belong to the inorganic nano field of photocatalytic material.
Background technology
The mankind face serious environmental problem day by day in recent years.Comprise in a large amount of pollutants that discharge in the productive life and have three persistent pollutants that cause effect in a large number, these toxic organicses show the characteristic of difficult degradation in conventional water treatment, to its elimination is the difficult point that the environmentalist pays close attention to, and energy shortage also is another bottleneck of restriction human development.How to utilize solar energy solution environment and energy problem to become the focus of research.Photocatalysis technology has the potentiality that solve environment and energy problem; because by being that the photodissociation water technology of clean Hydrogen Energy will thoroughly solve the crisis of fossil energy exhaustion with conversion of solar energy, and the photocatalysis Decomposition toxic organic pollutant will become an approach that cheapness is feasible that solves environmental problem.
Photocatalysis technology degraded environmental contaminants are expected to utilize fully solar energy, and have that energy consumption is low, reaction condition is gentle, easy and simple to handle, can reduce outstanding feature such as secondary pollution and come into one's own day by day, have broad application prospects.Conductor photocatalysis has become one of research focus of environment and energy field in recent years, studies show that in a large number nearly all organic pollution can both be the inorganic molecules material by photocatalytic degradation, decolouring, detoxification, mineralising effectively, thereby eliminate pollution and harm environment.In actual applications, catalysis material has been used for fields such as the purifier, self-cleaning glass surface, antibiotic photocatalysis ceramics face brick of water and air, has produced huge economy, environment and social benefit.
The mechanism of light-catalyzed reaction is the photon that the valence band Electron absorption energy of photochemical catalyst surpasses the corresponding energy of band gap, generation excites and generates photohole and electronics, and then moves to the organic pollution of catalyst surface and absorption or the process that hydrone carries out redox reaction.The band gap width that this shows semiconductor light-catalyst has determined the scope of response light wavelength.Use more TiO at present
2Only work Deng the wide band gap semiconducter compound in ultraviolet light range, and solar energy mainly concentrates on the visible-range of 400-700nm, therefore current photocatalysis technology still can not make full use of sunshine, and the light source of people for providing must be provided, this has just used electric energy indirectly, has improved the cost of using virtually.Photocatalysis technology still fails to realize the efficient cheap solar energy that transforms at present, has hindered its large-scale promotion and application in real life and production.Develop the novel semi-conductor catalysis material that can carry out light-catalyzed reaction under visible light-responded even the indoor natural light condition, be to improve solar energy utilization ratio, reduce cost, widen the range of application of photocatalysis technology, finally realize the key of photocatalysis technology commercial application.
The research of in the recent period visible light-responded semiconductor light-catalyst has obtained remarkable progress, and main achievement can be divided into two big classes.One class is to TiO
2Carry out doping vario-property, can expand TiO as introducing nonmetalloids such as N, C, I, F, Cl
2Absorbing wavelength to visible-range.Though doped Ti O
2Demonstrate the photocatalytic activity under certain visible light, but a little less than its light absorption, catalytic activity is generally lower, and has inactivation problems such as doped chemical loss.Another kind of is the non-TiO of development
2The novel photocatalysis material, reporting more novel photocatalysis material at present has BiVO
4, Bi
2WO
6, CaBi
2O
4Composite oxides Deng containing metal element bismuth.China's bismuth metal aboundresources accounts for 84% of world's gross reserves, and the compound oxide photocatalyst tool of therefore studying bismuth-containing has great advantage.Yet this class novel photocatalysis agent of development at present though a provisioning response is arranged in visible-range, owing to more weak visible absorption performance with than the diameter of particle of large scale, causes single photocatalyst activity lower.Because particle diameter is relatively large on the one hand, cause specific area not high, because growing, light induced electron hole migration distance causes easy compound inactivation on the other hand.There is report to adopt carried noble metal such as Ag to promote that electronics separates with the hole, on behalf of document, it " applied catalysis B: environment " magazine 2005 is arranged, 58, " BiVO4 photochemical catalyst photooxidation polycyclic aromatic hydrocarbon pure and the Ag load the " (S.Kohtani that delivers on the 265-272, M.Tomohiro, K.Tokumura, R.Nakagaki, Photooxidation reactions of polycyclicaromatic hydrocarbons over pure and Ag-loaded BiVO
4Photocatalysts, AppliedCatalysts B:Environmemal), Ag-BiVO
4The simple relatively BiVO of photocatalytic activity
4Be greatly improved, but adopt this noble metal of Ag to make cost higher on the one hand, it is still very low after Ag modifies on the other hand for the degradation efficient such as phenol that are difficult for absorption, so adopt cheap raw material to develop the more practical catalysis material of high visible activity, be researcher's common objective.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of nickel oxide loaded composite bismuth vanadium photocatalyst and preparation method thereof is provided, manufacturing process is simple, with low cost, the composite photo-catalyst of preparation can carry out light-catalyzed reaction efficiently under visible light or natural daylight, have good stability and advantage such as easily separated in liquid phase reactor.
The present invention is achieved by the following technical solutions, composite photo-catalyst provided by the invention is by semiconductor pucherite particle and load on that its surperficial nickel oxide particulate forms, the photochemical catalyst pucherite area load of micro-meter scale the nickel oxide particle of nanoscale of certain form existence.The feature of its preparation method is that the compound with pucherite (BiVO4) pressed powder and metallic nickel is a raw material, by the composite photo-catalyst of immersion process for preparing nickel-loaded, wherein the compound of nickel can be one or more combinations of nickel chloride, nickel nitrate, nickelous sulfate or organic nickel such as nickel acetate etc.
Conventional single photochemical catalyst light induced electron and hole are difficult for migration, particularly for the bigger particle of particle diameter such as the pucherite particle of micro-meter scale, photo-generated carrier is moved to the surface, and that time of light-catalyzed reaction takes place is longer, and also the no show surface is with regard to because compound and ineffective.Behind the overload nickel oxide, because the two has different band structures, can be with the different meetings in position to produce potential energy difference, impel light induced electron effectively to separate with the hole.The present invention utilizes nickel oxide loaded pucherite to obtain visible light-responded high efficiency photocatalysis performance.
The preparation method of composite photo-catalyst of the present invention is specific as follows:
1, the solution deposit of pucherite preparation:
By etc. mol ratio take by weighing bismuth nitrate and ammonium metavanadate, be dissolved in respectively in the nitric acid of 1-4M, after being stirred to dissolving fully two kinds of solution are mixed, and add urea therein, the mol ratio of each component is a bismuth salt in the mixed solution: vanadic salts: nitric acid: urea=1: 1: 5-20: 1-10, kept 5-20 hour at 60-100 ℃ of constant temperature, the while vigorous stirring, make urea hydrolysis gradually, along with precipitating gradually, the rising pucherite of pH value of solution value separates out, sediment is washed till neutrality with deionized water, through absolute ethanol washing for several times, places the 50-100 ℃ of dry 12-48 of constant temperature oven hour again.Can make the pucherite powder of monoclinic system scheelite-type structure.
2, the preparation of composite photo-catalyst
The nickel salt solution of preparation 0.01-0.1M is 0.1-10% by nickel element and pucherite mass ratio, and pucherite powder and nickel salt solution mixing are obtained paste mixture; Perhaps according to quality than nickel: pucherite: urea: deionized water=0.001-0.1: 1: 0.002-0.2: 5, earlier with the nickel salt pressed powder with deionized water dissolving after, adding pucherite and urea are placed under the 60-80 ℃ of water-bath and stirred 5-10 hour, make the abundant hydrolysis of nickel salt, obtain paste mixture.Then this above-mentioned paste mixture that obtains is placed constant temperature oven, to constant weight, grind into powder was put into Muffle furnace again, at 200-500 ℃ of roasting 1-4 hour, promptly prepares the composite bismuth vanadium photocatalyst of load nickel oxide 80 ℃ of dryings 24 hours.
Nickel salt described in the present invention can be one or more combinations of nickel chloride, nickel nitrate, nickelous sulfate or organic nickel such as nickel acetate etc.
The solvent of preparation nickel salt solution can be absolute ethyl alcohol or deionized water among the present invention.
The composite photo-catalyst that the present invention obtains is at pucherite (BiVO
4) oxide (CoO of particle surface nickel-loaded
x) visible light responsive photocatalyst, wherein, pucherite is monoclinic scheelite-type structure, the pucherite particle diameter is 100nm-5 μ m, the nickel oxide particle diameter of area load is 10nm-100nm, the mass ratio of nickel oxide and pucherite particle is 1-100mg/g, and the specific area of composite photo-catalyst is 0.5-5m
2/ g.
Nickel oxide loaded composite bismuth vanadium photocatalyst of the present invention, adopted cheap elemental nickel as loaded article, costs such as precious metals ag, Pt and Ru reduce greatly relatively, and this composite photo-catalyst density is bigger, can reclaim by precipitate and separate after liquid phase reactor finishes, the photochemical catalyst after the recovery can continue to use by dry regeneration.
The photochemical catalyst of the present invention's preparation has photocatalytic activity efficiently in the wave-length coverage of broad, can be at ultraviolet light, high efficiency photocatalysis degraded toxic and harmful substance under manual simulation's sunshine or the natural daylight radiation, realized wide range response to sunshine, make its application be extended to visible region, can be applied to air, waste water, the removal of organic pollution in surface water and the drinking water, or the photocatalysis that is used for heavy metal ion is removed, photochemical catalyzing, photo catalytic reduction nitrate, fixed nitrogen and family, the sanitary apparatus sterilization of hospital and other public arena.The present invention has promoted the practicability of photocatalysis technology.
Description of drawings
Fig. 1 is for the pattern of nickel oxide loaded composite bismuth vanadium photocatalyst under transmission electron microscope of the present invention's preparation, and is nickel oxide loaded as can be seen at the pucherite particle surface.
Photo is to the result of the methylene blue decolorization experiment of 100 milliliters of 15mg/L under composite photo-catalyst (by the embodiment 1 preparation) visible light of 3g/L among Fig. 2.Left side figure is the photo before the illumination, and solution is tangible blueness.Right figure is that certain water sample is got in illumination after 3 hours, precipitates the photo after 60 minutes.
The specific embodiment
Specify technical scheme of the present invention and effect below in conjunction with accompanying drawing.
Embodiment 1
Adopt deionized water to prepare the nickel nitrate solution of 0.085 mol, this solution contains nickel 0.005 gram for every milliliter.Take by weighing pucherite powder 1 gram with little evaporating dish, add 6 milliliters of nickel nitrate solutions, after stirring with glass bar, placed 80 ℃ of dryings of constant temperature oven 12 hours, it is last to pulverize then, put into 250 ℃ of roastings of Muffle furnace 1.5 hours, promptly make the composite photo-catalyst of visible light-responded nickel oxide loaded pucherite.
Phenol under the photocatalysis performance experiment of composite photo-catalyst of the present invention can be shone by visible light in the degradation water is tested.The mensuration process is as follows: add phenol solution and 0.3 gram composite photo-catalyst that 100 ml concns are about 20mg/L in 250 milliliters photo catalysis reactor, (amount of this absorption is very little to stir the balance that reaches adsorbing phenol half an hour before the illumination earlier, can ignore), (optical filter that has 400nm makes that radiation wavelength λ 〉=400nm), magnetic agitation is fully mixed in the course of reaction to open the 1000W xenon lamp.Every sampling in 20 minutes, adopt 4-amino-antipyrine spectrophotometry phenol concentration, photocatalytic degradation phenol clearance is initial phenol concentration and remains the phenol concentration difference divided by initial phenol concentration ((C
0-C
t) * 100/C
0).
The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 180min phenol clearance reaches 72.6%, far above the degradation effect of independent pucherite.
Fig. 1 is the pattern of nickel oxide loaded composite bismuth vanadium photocatalyst under transmission electron microscope that the present invention prepares, as seen from the figure, dark main body catalyst pucherite particle diameter is at micro-meter scale, and edge color more shallow be the nickel oxide of area load, its particle size is at tens nanometer.
Two results that photo is the methylene blue decolorization experiment among Fig. 2.The decolorization experiment of methylene blue is the methylene blue solution that adopts 100 milliliters 15mg/L, and in the presence of the composite photo-catalyst (being prepared by embodiment 1) of 3g/L, radiation of visible light carries out the decolored degradation reaction.Wherein left side figure is the photo before the illumination, and solution is tangible blueness.Right figure be that certain water sample is got in illumination after 3 hours, precipitate the photo after 60 minutes, therefrom react 3 hours as can be seen after, solution decolours fully, and to precipitate the upper strata be the transparent stillness of night, the bottom is the yellow-green light catalyst precipitation, shows the catalyst precipitation separation well.
Embodiment 2
Adopt deionized water to prepare the nickel nitrate solution of 0.085 mol, this solution contains nickel 0.005 gram for every milliliter.Take by weighing pucherite powder 1 gram with little evaporating dish, add 8 milliliters of nickel nitrate solutions, after stirring with glass bar, placed 80 ℃ of dryings of constant temperature oven 12 hours, it is last to pulverize then, put into 250 ℃ of roastings of Muffle furnace 2 hours, promptly make the composite photo-catalyst of visible light-responded nickel oxide loaded pucherite.The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 180min phenol clearance reaches 62.8%, is higher than the degradation effect of independent pucherite far away, and photocatalysis performance improves greatly behind the visible load nickel oxide.
Embodiment 3
Adopt deionized water to prepare the nickel nitrate solution of 0.085 mol, this solution contains nickel 0.005 gram for every milliliter.Take by weighing pucherite powder 1 gram with little evaporating dish, add 4 milliliters of nickel nitrate solutions, after stirring with glass bar, placed 80 ℃ of dryings of constant temperature oven 12 hours, it is last to pulverize then, put into 450 ℃ of roastings of Muffle furnace 1 hour, promptly make the composite photo-catalyst of visible light-responded nickel oxide loaded pucherite.
The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 180min phenol clearance reaches 30.7%, the degradation effect (180min phenol clearance only is 4.2%) that is higher than independent pucherite far away, also far above the photocatalytic degradation effect of commodity titanium dioxide P-25, photocatalysis performance improves behind the visible load nickel oxide.
Embodiment 4
Take by weighing nickel nitrate 0.1 gram, add 5 ml waters and be stirred to dissolving fully, add 0.2 gram urea and 1 gram pucherite powder then, under 80 ℃ of water-baths, stirred 8 hours, placed 80 ℃ of constant temperature ovens then dry 24 hours, the pressed powder that obtains is put into 250 ℃ of roastings of Muffle furnace 1.5 hours after grinding, promptly make the composite photo-catalyst of visible light-responded nickel oxide loaded pucherite.The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 180min phenol clearance reaches 87.0%, is higher than the degradation effect of independent pucherite far away.
Claims (5)
1, a kind of nickel oxide loaded composite bismuth vanadium photocatalyst, it is characterized in that being visible light responsive photocatalyst at the oxide of pucherite particle surface nickel-loaded, wherein, pucherite is monoclinic scheelite-type structure, the pucherite particle diameter is 100nm-5 μ m, the nickel oxide particle diameter of area load is 10nm-100nm, and the mass ratio of nickel oxide and pucherite particle is 1-100mg/g, and the specific area of composite photo-catalyst is 0.5-5m
2/ g.
2, a kind of preparation method of nickel oxide loaded composite bismuth vanadium photocatalyst is characterized in that comprising the steps:
1) solution deposit of pucherite preparation: will wait the bismuth nitrate of mol ratio and ammonium metavanadate to be dissolved in respectively in the nitric acid of 1-4M, after being stirred to dissolving fully two kinds of solution are mixed, and add urea therein, the mol ratio of each component is a bismuth salt in the mixed solution: vanadic salts: nitric acid: urea=1: 1: 5-20: 1-10, kept 5-20 hour at 60-100 ℃, sediment deionized water and absolute ethanol washing, at 50-100 ℃ of dry 12-48 hour, promptly make the pucherite powder of monoclinic system scheelite-type structure.
2) preparation of composite photo-catalyst: the nickel salt solution of preparation 0.01-0.1M is 0.1-10% by nickel element and pucherite mass ratio, and pucherite powder and nickel salt solution mixing are obtained paste mixture; Perhaps according to quality than nickel: pucherite: urea: deionized water=0.001-0.1: 1: 0.002-0.2: 5, earlier with the nickel salt pressed powder with deionized water dissolving after, adding pucherite and urea are placed under the 60-80 ℃ of water-bath and stirred 5-10 hour, make the abundant hydrolysis of nickel salt, obtain paste mixture; Then paste mixture is placed constant temperature oven, to constant weight, grind into powder was put into Muffle furnace again, at 200-500 ℃ of roasting 1-4 hour, promptly prepares the composite bismuth vanadium photocatalyst of load nickel oxide 80 ℃ of dryings 24 hours.
3, according to the preparation method of the nickel oxide loaded composite bismuth vanadium photocatalyst of claim 2, it is characterized in that described nickel salt is one or more combinations of nickel chloride, nickel nitrate, nickelous sulfate or organic nickel.
4, according to the preparation method of the nickel oxide loaded composite bismuth vanadium photocatalyst of claim 2, the solvent that it is characterized in that described preparation nickel salt solution is absolute ethyl alcohol or deionized water.
5, a kind of application of nickel oxide loaded composite bismuth vanadium photocatalyst of claim 1, it is characterized in that being applied to the removal of organic pollution in air, waste water, surface water and the drinking water, or be used for photocatalysis removal, photochemical catalyzing, photo catalytic reduction nitrate, fixed nitrogen and the sanitary apparatus sterilization of heavy metal ion.
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