CN1806915A - Composite bismuth vanadium photocatalyst supported by cobalt oxide and preparation method thereof - Google Patents
Composite bismuth vanadium photocatalyst supported by cobalt oxide and preparation method thereof Download PDFInfo
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- CN1806915A CN1806915A CN 200610024092 CN200610024092A CN1806915A CN 1806915 A CN1806915 A CN 1806915A CN 200610024092 CN200610024092 CN 200610024092 CN 200610024092 A CN200610024092 A CN 200610024092A CN 1806915 A CN1806915 A CN 1806915A
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Abstract
The invention relates the method for preparation of pucherite composite photocatalyst loaded on cobalt oxide. The photocatalyst comprises semi-conductor pucherite particle and cobalt oxide particle. The pucherite is monoclinic crystal system scheelite structure, and the diameter is 100nm-5mum. The grain diameter of cobalt oxide is 10nm-1mum. The mass ratio of cobalt 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 composite bismuth vanadium photocatalyst of a kind of supported by cobalt oxide and preparation method thereof, the photochemical catalyst of preparation has photocatalytic activity in the wave-length coverage of broad, can be under ultraviolet light, visible light or natural daylight radiation high efficiency photocatalysis degraded toxic and harmful substance.Belong to the inorganic nano field of photocatalytic material.
Background technology
Current environment problem and energy crisis become two big bottlenecks of restriction human development; 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.Therefore the conductor photocatalysis technology is subjected to various countries' environment and energy research person's common concern.
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.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.
Yet use more TiO at present
2Only work Deng the wide band gap semiconducter compound, and solar energy mainly concentrates on the visible-range of 400-700nm, utilize sunshine degraded toxic organic pollutant and photodissociation water to be significant for environmental protection and energy development in ultraviolet light range.Therefore photocatalysis technology still is difficult to realize the conversion of solar energy of Cheap highly effective 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, this type of document has " applied catalysis B: environment " magazine 2003,46, deliver on the 573-586 " visible light of solar simulator adopts down BiVO
4Photochemical catalyst light degradation 4-alkyl phenol " (S.Kohtani; M.Koshiko; et al.; Photodegradationof 4-alkylphenols using BiVO4 photocatalyst under irradiation with visible light froma solar simulator; Applied Catalysts B:Environmental) etc., this article adopts pucherite (BiVO
4) alkyl phenol of under visible light, effectively having degraded, and the raw material of its preparation is easy to get, and method is simple, and price is suitable.The visible light-responded photochemical catalyst that this class is novel, though have certain visible light-responded performance, but single pucherite photocatalytic activity is lower, on the one hand because the particle diameter of micro-meter scale is relatively large, cause specific area not high, cause easy compound inactivation because light induced electron hole migration distance is grown on the other hand.There is report to adopt carried noble metal such as Ag to promote that electronics separates with the hole, but the composite photo-catalyst cost that adopts noble metal to obtain is higher, and this class modification back is very low for the degradation efficient such as phenol that are difficult for absorption, so need to develop the more catalysis material of highlight catalytic active comparatively speaking.By retrieval, domestic patent is relevant for the report of pucherite: contain bismuth composite oxide BiMO
4And Bi
2NO
6Type semiconductor light-catalyst and preparation and application, application number: 200410041284.5.But the preparation method of its pucherite is a solid phase reaction, relates to some ball-grinding machines etc., and does not relate to the content of pucherite modification aspect, and simple pucherite activity is not suitable for practical application.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, composite bismuth vanadium photocatalyst of a kind of supported by cobalt oxide 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 cobalt oxide particulate forms, the photochemical catalyst pucherite area load of micro-meter scale the cobalt oxide particle of nanoscale of certain form existence.
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 cobalt 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 the pucherite of supported by cobalt oxide to obtain visible light-responded high efficiency photocatalysis performance.
The preparation method of composite photo-catalyst of the present invention is specific as follows:
(a) 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.
(b) preparation of composite photo-catalyst
The cobalt salt solution of preparation 0.01-0.1M, by cobalt oxide and pucherite mass ratio is 0.1-10%, solid pucherite powder and cobalt salt solution are mixed, after stirring, mixture is placed constant temperature oven, made it to reach abundant drying at 50-80 ℃ of dry 12-24 hour, the last Muffle furnace of putting into of pulverizing again, 200-500 ℃ following roasting 1-4 hour, can obtain the composite bismuth vanadium photocatalyst of supported by cobalt oxide.
Cobalt salt described in the present invention can be one or more combinations of cobalt chloride, cobalt nitrate, cobaltous sulfate or organic cobalt such as cobalt acetate etc.
The solvent of preparation cobalt 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 load cobalt
x) visible light responsive photocatalyst, wherein, pucherite is monoclinic scheelite-type structure, the pucherite particle diameter is 100nm-5 μ m, the cobalt oxide particle diameter of area load is 10nm-1 μ m, the mass ratio of cobalt oxide and pucherite particle is 1-100mg/kg, and the specific area of composite photo-catalyst is 0.5-5m
2/ g
The composite bismuth vanadium photocatalyst of supported by cobalt oxide of the present invention, adopted cheap element cobalt 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, realize family, the deodorizing of hospital and other public arena, persistent organic pollutants in sterilization and decomposition liquid phase or the gas phase, and the photocatalysis of heavy metal ion is removed, photochemical catalyzing, photo catalytic reduction nitrate and relevant photocatalytic applications fields such as fixed nitrogen.The present invention has promoted the practicability of photocatalysis technology.
Description of drawings
Fig. 1 is the pattern of composite bismuth vanadium photocatalyst under transmission electron microscope of the supported by cobalt oxide of the present invention's preparation, and supported by cobalt oxide is at the pucherite particle surface as can be seen.
Fig. 2 is the degradation reaction result of employing catalyst Pyrogentisinic Acid of the present invention under visible light shines, among the figure:
Degussa P-25 (the commodity TiO of curve 1:1g/L
2),
The pucherite of curve 2:3g/L (by preparation among the embodiment 1),
Cobalt oxide/composite bismuth vanadium photocatalyst of curve 3:1g/L (by preparation among the embodiment 1).
The specific embodiment
Specify technical scheme of the present invention and effect below in conjunction with accompanying drawing.
Take by weighing 9.5g bismuth nitrate and 2.3396g ammonium metavanadate, use the 1.84M nitric acid dissolve of 25ml and 75ml respectively, mix then, add 3.75g urea, after the stirring and dissolving, place 90 ℃ oil bath pan constant temperature 8 hours, the precipitation that generates is centrifugal, be washed till neutrality with deionized water, wash 3 times with absolute ethyl alcohol again, placed 80 ℃ of oven dryings 24 hours.Take by weighing the pucherite powder 1g of method for preparing with little evaporating dish, adding is with 2 milliliters of the cobalt nitrates of 19.42 grams per liters of deionized water configuration, after stirring, place constant temperature oven 80 ℃ of dryings 24 hours, it is last to pulverize then, place 300 ℃ of roastings of Muffle furnace 2 hours, promptly make the composite bismuth vanadium photocatalyst of visible light-responded supported by cobalt oxide.
The pattern of the composite photo-catalyst that makes under transmission electron microscope as shown in Figure 1, supported by cobalt oxide is at the pucherite particle surface as can be seen.Among the figure, dark main body catalyst pucherite particle diameter is at micro-meter scale, and edge color more shallow be the cobalt oxide of area load, its particle size is at tens nanometer.
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 cobalt oxide/composite bismuth vanadium photocatalyst 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 is seen Fig. 2, under the radiation of visible light of wavelength greater than 400nm, 120min phenol clearance reaches 79.8%, the degradation effect that is higher than independent pucherite far away, also far above the photocatalytic degradation effect of commodity titanium dioxide P-25, photocatalysis performance improves greatly behind the visible load cobalt oxide.Curve 1 is 1g/L Degussa P-25 (commodity TiO among Fig. 2
2) exist the time, radiation of visible light 120min phenol degrading seldom, only be 11%, curve 2 is under the existence of independent pucherite of 3g/L, radiation of visible light 120min phenol is degraded hardly, only be 3.1%, and curve 3 is in the presence of the 1g/L composite photo-catalyst, radiation of visible light 120min phenol degrading about 79.8%.
Embodiment 2
Take by weighing 4.8507g bismuth nitrate and 1.1698g ammonium metavanadate, use the 1.84M nitric acid dissolve of 25ml respectively, mix then, add 1.875g urea, after the stirring and dissolving, place 90 ℃ oil bath pan constant temperature 8 hours, the precipitation that generates is centrifugal, be washed till neutrality with deionized water, wash 3 times with absolute ethyl alcohol again, placed 60 ℃ of oven dryings 48 hours.Take by weighing the pucherite powder 2g of method for preparing with little evaporating dish, adding is with 4 milliliters of the cobalt nitrates of 19.42 grams per liters of absolute ethyl alcohol configuration, after stirring, place constant temperature oven 80 ℃ of dryings 24 hours, it is last to pulverize then, place 200 ℃ of roastings of Muffle furnace 2 hours again, promptly make the composite bismuth vanadium photocatalyst of visible light-responded supported by cobalt oxide.The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 120min phenol clearance reaches 56.6%, far above the photocatalytic degradation effect of pucherite and commodity titanium dioxide P-25.
Take by weighing the 1.84M nitric acid dissolve of 4.8507g bismuth nitrate with 50ml, add the 1.1698g ammonium metavanadate again, after mixing, add 1.875g urea, after the stirring and dissolving, place 90 ℃ oil bath pan constant temperature 8 hours, the precipitation that generates is centrifugal, be washed till neutrality with deionized water, wash 3 times with absolute ethyl alcohol again, placed 80 ℃ of oven dryings 24 hours.Take by weighing the pucherite powder 1g of method for preparing with little evaporating dish, adding is with 4 milliliters of the cobalt nitrates of 19.42 grams per liters of deionized water configuration, after stirring, place constant temperature oven 80 ℃ of dryings 12 hours, it is last to pulverize then, place 300 ℃ of roastings of Muffle furnace 2 hours again, promptly make the composite bismuth vanadium photocatalyst of visible light-responded supported by cobalt oxide.The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 120min phenol clearance reaches 63.3%, is better than the photocatalytic degradation effect of pucherite and commodity titanium dioxide P-25.
Embodiment 4
Take by weighing 9.5g bismuth nitrate and 2.3396g ammonium metavanadate, use the 1.84M nitric acid dissolve of 50ml respectively, mix then, add 3.75g urea, after the stirring and dissolving, place 90 ℃ oil bath pan constant temperature 8 hours, the precipitation that generates is centrifugal, be washed till neutrality with deionized water, wash 3 times with absolute ethyl alcohol again, placed 80 ℃ of oven dryings 24 hours.Take by weighing the pucherite powder 1g of method for preparing with little evaporating dish, adding is with 1 milliliter of the cobalt chloride of 0.065 mol of deionized water configuration, after stirring, place constant temperature oven 80 ℃ of dryings 12 hours, it is last to pulverize then, place 300 ℃ of roastings of Muffle furnace 2 hours again, make the composite bismuth vanadium photocatalyst of visible light-responded supported by cobalt oxide.The The performance test results of degradation of phenol: under the radiation of visible light of wavelength greater than 400nm, 120min phenol clearance reaches 46.2%, also is better than the photocatalytic degradation effect of pucherite and commodity titanium dioxide P-25.
Claims (5)
1, a kind of composite bismuth vanadium photocatalyst of supported by cobalt oxide, it is characterized in that being visible light responsive photocatalyst at the oxide of pucherite particle surface load cobalt, wherein, pucherite is monoclinic scheelite-type structure, the pucherite particle diameter is 100nm-5 μ m, the cobalt oxide particle diameter of area load is 10nm-1 μ m, and the mass ratio of cobalt 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 composite bismuth vanadium photocatalyst of supported by cobalt oxide is characterized in that comprising the steps:
(a) 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;
(b) preparation of composite photo-catalyst: the cobalt salt solution of preparation 0.01-0.1M, by cobalt oxide and pucherite mass ratio is 0.1-10%, solid pucherite powder and cobalt salt solution are mixed, stir and be placed in the constant temperature oven, made it abundant drying at 50-80 ℃ of dry 12-24 hour, the last Muffle furnace of putting into of pulverizing again, 200-500 ℃ roasting 1-4 hour, promptly obtain the composite bismuth vanadium photocatalyst of supported by cobalt oxide.
3, according to the preparation method of the composite bismuth vanadium photocatalyst of the supported by cobalt oxide of claim 2, it is characterized in that described cobalt salt is one or more combinations of cobalt chloride, cobalt nitrate, cobaltous sulfate or organic cobalt.
4, according to the preparation method of the composite bismuth vanadium photocatalyst of the supported by cobalt oxide of claim 2, the solvent that it is characterized in that described preparation cobalt salt solution is absolute ethyl alcohol or deionized water.
5, a kind of application of composite bismuth vanadium photocatalyst of supported by cobalt oxide of claim 1, it is characterized in that being applied to deodorizing, the sterilization of family, hospital and various public arenas, be applied to decompose the persistent organic pollutants in liquid phase or the gas phase, and the photocatalysis removal, photochemical catalyzing, photo catalytic reduction nitrate, fixed nitrogen and the relative photo catalytic applications that are applied to heavy metal ion.
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