CN104108753A - Preparation for visible-light responsible BiVO4 catalyst - Google Patents
Preparation for visible-light responsible BiVO4 catalyst Download PDFInfo
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- CN104108753A CN104108753A CN201310138022.XA CN201310138022A CN104108753A CN 104108753 A CN104108753 A CN 104108753A CN 201310138022 A CN201310138022 A CN 201310138022A CN 104108753 A CN104108753 A CN 104108753A
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Abstract
The invention discloses a preparation method for a visible-light responsible BiVO4 catalyst. The method comprises: taking a bismuth compound and a vanadium compound respectively as a bismuth source and a vanadium source, taking mixtures of water and an organic alcohol with different ratios as reaction solvents, and performing a hydro-thermal synthesis reaction, so as to obtain a catalytic material in the forms of a nanometer small particle, a nanometer ellipsoid, a flower-shaped structure or a branch structure. The visible-light responsible catalyst containing BiVO4 with different morphologies helps to greatly improve the photocatalysis degradation efficiency when being applied to the field of photocatalytic degradation of pollutants. The preparation method has the advantages of simple operation, mild reaction conditions, low equipment cost, relatively strong visible-light absorption, good visible-light catalytic performance and the like.
Description
Technical field
The present invention relates to visible light-responded BiVO
4field of nano material preparation and photocatalysis technology field, be specifically related to hydrothermal synthesis method and prepare nano particle, nanometer ellipsoid, flower-like structure and dendritic structure BiVO
4material, and by the visible light-responded BiVO of different-shape
4as photocatalyst, rhodamine B degradation.
Background technology
Along with global environmental pollution and energy dilemma are day by day serious, can fully effectively utilize the sun power of environmental protection to realize preparation and the Application and Development of visible light-responded catalysis technique and the material thereof of photocatalytic degradation pollutent or hydrogen manufacturing, become the hot research problem in the fields such as chemistry, materialogy and environmental science.Find TiO from Fujishima in 1972
2under illumination since catalytic decomposition water oxygen gas and hydrogen, nontoxic, good stability, TiO cheap and easy to get
2attract widespread attention.But, TiO
2photocatalytic activity does not but reach the effect of practical application, and this mainly exists two problems: the one, and due to TiO
2greater band gap (3.0～3.2eV), spectral response range is narrow, can only absorbing wavelength be less than the photon of 387nm, can only absorb the UV-light that accounts for sunlight total energy 3～4%, cannot utilize fully sunlight to carry out light-catalyzed reaction; The photic electron-hole pair of another key reason produces less, and complex reaction probability is larger.Solar energy mainly concentrates on the visible region of 400～700nm, accounts for 43% of total energy.As can be seen here, the highest to the solar energy utilization ratio of visible light-responded photocatalyst, the semiconductor light-catalyst of preparing synthesizing visible light response will finally be realized the commercial application of photocatalysis technology.
Semi-conductor BiVO
4because can realize photolysis water and degradable organic pollutant under visible ray and become a focus of current research.BiVO
4mainly contain cubic zircon phase, monocline sheelite phase and three kinds of crystal formations of cubic sheelite facies pattern.The wherein BiVO of oblique system scheelite-type structure
4biVO with other two kinds of structures
4compare, have better visible light photocatalysis active, this has caused the concern of vast researcher.Monoclinic phase BiVO
4energy gap be 2.3～2.4eV, its sufficiently high valence band can realize hole (h
+) degraded to organic pollutant, and its valence band oxidizing potential is positioned near 2.4eV, simultaneously its conduction band position is also conducive to the reduction of light induced electron, has higher oxidation capacity, provides theoretical foundation for realize degrade organic pollutant and water of decomposition under visible ray.Monoclinic phase BiVO at present
4the research field that has been applied to photolysis water hydrogen, degradation of contaminant and photoelectrochemistry water of decomposition shows more wide application prospect.
Hydrothermal synthesis method is to utilize the aqueous solution of High Temperature High Pressure to make the substance dissolves of those insoluble or insolublies under atmospheric condition, or resultant of reaction is dissolved, make to produce convection current by the temperature of solution in control autoclave and separate out the method for growing crystal to form hypersaturated state.This process is relatively simple, and the formation of thing phase, the size of particle diameter, pattern also can be controlled.And dispersiveness and the circulation ratio of product are better.Under hydrothermal condition, the character (composition, density, viscosity, dissemination) of solvent influences each other, alter a great deal, and differ greatly under its character and usual conditions, dissolving, dispersiveness and the chemical reactivity of corresponding reactant improve greatly or strengthen, and this just makes reaction at lower temperature, to occur.
Summary of the invention
It is a kind of efficient convenient and can obtain the visible light-responded BiVO of different-shape to the object of the present invention is to provide
4the preparation method of nano material, and be applied to photocatalysis field with this type material.
The object of the invention is achieved through the following technical solutions:
The visible light-responded BiVO of different-shape
4preparation method of nano material, comprises the steps: that (1) takes appropriate Bismuth trinitrate and ammonium meta-vanadate is dissolved in the glycol ether and water mixed solvent of different ratios; (2) after magnetic agitation number minute, mixing solutions is transferred in reactor, after sealing, put into baking oven and carry out hydrothermal synthesis reaction; (3) collect product, through washing, alcohol wash for several times, high speed centrifugation separates successively; (4) product of washing is put into baking oven, dry a few hours.
The present invention utilizes hydrothermal synthesis method to prepare the visible light-responded BiVO of different-shape
4nano material.
As a kind of preferred version, in above-mentioned preparation method, described bismuth source is sodium bismuthate, Bismuth trinitrate, bismuth tungstate, bismuth sulfate, Bismuth Subcarbonate or bismuth subsalicylate etc., and the amount of substance in titanium source is 0.001～0.1mol.Described vanadium source is ammonium meta-vanadate, Vanadium Pentoxide in FLAKES, vanadous oxide, ammonium meta-vanadate, sodium metavanadate, potassium metavanadate, sodium vanadate, sodium pyrovanadate, vanadylic sulfate, oxalic acid vanadyl, vanadium tetrachloride, and the amount of substance in vanadium source is 0.001～0.1mol.
As a kind of preferred version, in above-mentioned preparation method, described organic solvent is methyl alcohol, ethanol, Virahol, propyl carbinol, ethylene glycol, glycerine etc.
As a kind of preferred version, in above-mentioned preparation method, described glycol ether and water ratio control were at 40: 0～0: 40.
As a kind of preferred version, in above-mentioned preparation method, the temperature of reaction of described hydrothermal synthesis reaction is arranged on 60-250 DEG C.
As a kind of preferred version, in above-mentioned preparation method, the time of described hydrothermal synthesis reaction is 1～72h.
As a kind of preferred version, in above-mentioned preparation method, described dry temperature is 20～100 DEG C.
The visible light-responded BiVO of the different-shape that the inventive method makes
4nano material utilizes X-ray powder diffraction (XRD), scanning electron microscope (SEM), ultraviolet-visible spectrum etc. to carry out detailed sign.
Based on the visible light-responded BiVO of different-shape
4nanomaterial photocatalytic degradation rhodamine B (RhB) comprises the following steps: (1) accurately takes appropriate photocatalyst BiVO
4put into beaker, pipette the appropriate RhB aqueous solution, lucifuge magnetic agitation number minute, sets up adsorption-desorption balance and dark state molecular balance.(2) adopt xenon long-arc lamp stabilized current supply as light source, be placed in the cold hydrazine with recirculated water, appropriate Sodium Nitrite is filled to glass clamp shell type isothermal reactor to filter out UV-light, utilize radiation of visible light RhB solution.(3) in walls of beaker and reactor, xenon lamp is at a distance of suitable distance, and RhB solution continues to stir, and gets sample one time at interval of certain hour, and the solution centrifugal of obtaining separates.(4) adopt uv-spectrophotometric instrument to test the absorbancy (maximum absorption wavelength of RhB is 553.8nm) of RhB, parameters is: sweep limit 400～700nm, slit 1.0cm.
As a kind of preferred version, in above-mentioned photocatalytic degradation pollutent experiment, described degradation product comprises methylene blue, rhodamine B, tropeolin-D, Reactive blue M-2GE etc.
As a kind of preferred version, in above-mentioned photocatalytic degradation pollutent experiment, required catalyst levels is controlled between 0.02～1.0g.
As a kind of preferred version, in above-mentioned photocatalytic degradation pollutent experiment, described Pollutant levels are controlled between 1～20mg/L.
As a kind of preferred version, in above-mentioned photocatalytic degradation pollutent experiment, described Sodium Nitrite concentration is controlled between 0.1～10mol/L.
The visible light-responded BiVO of different-shape prepared by the inventive method
4nano material can be widely used in the fields such as photochemical catalysis, photodissociation water, air-sensitive, lithium ion battery, sensor, makeup.Especially, during as photocatalytic degradation pollutent field, greatly improved photocatalysis efficiency.
Compared with prior art, tool of the present invention has the following advantages:
(1) the present invention utilizes hydrothermal synthesis method to prepare the visible light-responded BiVO of different-shape
4nano material, this preparation method has simply, easily and fast and high repeatability and other advantages;
(2) utilize the visible light-responded BiVO of the different-shape of synthesized
4application of micron has Visible Light Induced Photocatalytic at photocatalytic degradation pollutent, and degradation rate improves greatly;
(3) the visible light-responded BiVO of the different-shape of preparation method's gained of the present invention
4application of micron is at photocatalytic degradation pollutent; its main advantage has: starting material abundance, cost is low, Technology is relatively simple; in suitability for industrialized production, there is larger advantage; all raw material and production technique are all nontoxic, free of contamination simultaneously, and the exploitation to new forms of energy and renewable energy source and to protect mankind living environment have great importance.
Brief description of the drawings
The BiVO making under Fig. 1 different solvents ratio
4xRD figure;
The BiVO making under Fig. 2 different solvents ratio
4transmission electron microscope picture;
Fig. 3 BiVO
4uv-visible absorption spectra spectrogram;
The BiVO making under Fig. 4 different solvents ratio
4(α h υ)
2h υ is schemed;
The BiVO that Fig. 5 different solvents ratio makes
4the degradation rate of RhB in photocatalytic process.
Embodiment
Further explain the present invention below in conjunction with specific embodiment, but embodiment does not limit in any form to the present invention.
Embodiment
The visible light-responded BiVO of different-shape
4the preparation of nano material:
Take 0.968g Bismuth trinitrate, 0.058g ammonium meta-vanadate, measure solvent glycol ether, water, both ratios are 20: 20, and cumulative volume is 160mL.Under the condition of 55～65 DEG C of heated and stirred, ammonium meta-vanadate is dissolved in to 40mL water, Bismuth trinitrate is dissolved in to the mixing solutions of the glycol ether-water being formed by glycol ether and remaining water.Be cooled to after room temperature, stir simultaneously on limit, slowly ammonium metavanadate solution is poured in bismuth nitrate solution, stir 30 minutes, then reaction mixture is transferred to reactor, put into electric oven, at 140 DEG C, constant temperature keeps reaction 12h.Naturally cool to room temperature, collect powder-product, water and washing with alcohol precipitation three times successively, centrifugation.Finally, by the powder-product of collecting, dry 10h at 70 DEG C.
According to above-mentioned condition, by glycol ether and volume of water ratio be adjusted to 40: 0,35: 5,30: 10,10: 30,5: 35,0: 40, keep under condition that solvent cumulative volume is 160mL the BiVO of synthetic different-shape
4nano material.Wherein ammonium meta-vanadate optimum solvation is in 40mL water, if the not enough 40mL of water supplies 40mL with glycol ether, remaining solvent is used for dissolving Bismuth trinitrate.
Dried white powder is directly used in powdery diffractometry test, judges its crystal formation, and result shows that 40: 0,35: 5,30: 10,10: 30 prepared products are monocline BiVO
4nano material, and 5: 35,0: 40th, the mixed crystal (seeing Fig. 1) of monocline and tetragonal structure.
Characterize its pattern with scanning radio mirror, work as V
glycol ether: V
water=40: 0 o'clock (Fig. 2 .a), BiVO
4powder is nanometer fine texture, and uniform particles is consistent, and size is about 35nm.Work as V
glycol ether: V
water=35: 5 o'clock (Fig. 2 .b), BiVO
4powder is similar ellipsoid structure, short radius 400～440nm, major radius 850～900nm, and association nanometer small-particle.Work as V
glycol ether: V
water=30: 10 o'clock (Fig. 2 .c), BiVO
4powder is ellipsoid structure, granule-morphology uniformity, short radius 900～950nm, major radius 1300-1450nm.Work as V
glycol ether: V
water=20: 20 o'clock (Fig. 2 .d), BiVO
4powder is flower-like structure, center indent, and uniform particles is consistent, wide 3.5～3.8 μ m that are about in footpath.Work as V
glycol ether: V
water=10: 30 o'clock (Fig. 2 .e), BiVO
4the existing sheet structure of powder, also has branch sheet structure, and size is inhomogeneous, is about 4～5 μ m left and right.Work as V
glycol ether: V
water=5: 35 o'clock (Fig. 2 .f), BiVO
4powder is dendritic structure, and limb is about 3～4 μ m, has a large amount of small size bifurcateds.Work as V
glycol ether: V
water=0: 40 o'clock (Fig. 2 .g), BiVO
4powder is independent limb sheet structure, with one or two bifurcateds, and uniformity, limb length is about 800nm, the wide 170nm that is about.
All products all have obvious absorbing phenomenon in the visible region of 400～500nm.35: 5 similar to the spectrogram of 5: 35 to 30: 10,10: 30, and known according to their SEM figure, they have respectively similar structure.With respect to 30: 10 there is blue-shifted phenomenon at 35: 5, blue-shifted phenomenon with respect to 10: 30 occurs at 5: 35, blue-shifted phenomenon (seeing Fig. 3) with respect to 25: 15 occurs at 20: 20.In the time that glycol ether and water ratio are 40: 0,35: 5,30: 10,20: 20,10: 30,5: 35,0: 40, the BiVO making
4the energy gap value of photocatalyst is sequentially 2.83,2.46,2.50,2.40,2.45,2.46,2.50.From energy gap, they all have good response (seeing Fig. 4) to visible ray.
BiVO
4the research of photocatalytic degradation RhB efficiency:
Accurately take the photocatalyst BiVO of 0.200g
4put into 50mL beaker, pipetting 50mL concentration is the RhB aqueous solution of 5mg/L, and lucifuge magnetic agitation 30min sets up adsorption-desorption balance and dark state molecular balance by dark reaction.Adopt xenon long-arc lamp stabilized current supply as light source, be placed in the cold hydrazine with recirculated water, with elimination UV-light, utilize radiation of visible light RhB solution with 1.0mol/L sodium nitrite solution.In walls of beaker and reactor, xenon lamp is at a distance of 10cm, and solution keeps stirring.Utilize 5mL disposable syringe interval 30min sampling, centrifugation, obtains clarifying the RhB aqueous solution.Every sub-sampling 4mL, adopts Shimadzu UV-Vis3150 type spectrophotometer to detect the absorbancy of RhB, and parameters is: sweep limit 400～700nm, slit 1.0cm.According to there being good linear relationship between low strength range internal absorbance A and concentration C, meet Law of Lambert-Beer.Weigh the photocatalytic degradation degree of RhB with degradation rate (R).
R(％)＝(A
0-A)/A
0×100％＝(C
0-C)/C
0×100％
Fig. 5 is the BiVO that different pH values make
4the degradation rate figure of RhB different time in photocatalytic process, wherein ordinate zou is degradation rate, X-coordinate is the reaction times.Through the light-catalyzed reaction of 210min, the ratio of glycol ether and water is sequentially 40: 0,35: 5,30: 10,20: 20,10: 30,5: 35,0: the 40 o'clock BiVO making
4the efficiency of photocatalytic degradation RhB is respectively 64.57%, 73.08%, 53.95%, 52.53%, 33.70%, 73.18%, 99.29%.Therefore, best glycol ether and water proportioning are 40: 0, and through the light-catalyzed reaction of 210min, catalysis degradation modulus reaches 100%.
Claims (8)
1. a visible light-responded BiVO
4catalyzer, is characterized in that being prepared from by the following method: (1) takes appropriate Bismuth trinitrate and ammonium meta-vanadate is dissolved in the glycol ether and water mixed solvent of different ratios; (2) after magnetic agitation number minute, reaction mixture is transferred in reactor, after sealing, put into baking oven and carry out hydrothermal synthesis reaction; (3) collect product, through washing, alcohol wash for several times, high speed centrifugation separates successively; (4) product of washing is put into baking oven, dry a few hours.
2. visible light-responded BiVO according to claim 1
4catalyzer preparation, is characterized in that the described V that works as
glycol ether: V
water=40: 0 o'clock, BiVO
4powder is nanometer fine texture, and uniform particles is consistent, and size is about 35nm.Work as V
glycol ether: V
water=35: 5 o'clock, BiVO
4powder is similar ellipsoid structure, short radius 400～440nm, major radius 850～900nm, and association nanometer small-particle.Work as V
glycol ether: V
water=30: 10 o'clock, BiVO
4powder is ellipsoid structure, and uniform particles is consistent, short radius 900～950nm, major radius 1300-1450nm.Work as V
glycol ether: V
water=20: 20 o'clock, BiVO
4powder is flower-like structure, center indent, and uniform particles is consistent, wide 3.5～3.8 μ m that are about in footpath.Work as V
glycol ether: V
water=10: 30 o'clock, BiVO
4the existing sheet structure of powder, also has branch sheet structure, and size is inhomogeneous, is about 4～5 μ m left and right.Work as V
glycol ether: V
water=5: 35 o'clock, BiVO
4powder is dendritic structure, and limb is about 3～4 μ m, has a large amount of small size bifurcateds.Work as V
glycol ether: V
water=0: 40 o'clock, BiVO
4powder is independent limb sheet structure, with one or two bifurcateds, and uniformity, limb length is about 800nm, the wide 170nm that is about.In view of this, the pattern of solvent ratios remarkably influenced product.
3. visible light-responded BiVO according to claim 1
4catalyzer preparation, is characterized in that step (1) bismuth source is sodium bismuthate, Bismuth trinitrate, bismuth tungstate, bismuth sulfate, Bismuth Subcarbonate or bismuth subsalicylate etc., and the amount of substance in bismuth source is 0.001～0.1mol.Described vanadium source is ammonium meta-vanadate, Vanadium Pentoxide in FLAKES, vanadous oxide, ammonium meta-vanadate, sodium metavanadate, potassium metavanadate, sodium vanadate, sodium pyrovanadate, vanadylic sulfate, oxalic acid vanadyl, vanadium tetrachloride, and the amount of substance in vanadium source is 0.001～0.1mol.Organic solvent is methyl alcohol, ethanol, Virahol, propyl carbinol, ethylene glycol, glycerine etc.Described glycol ether and water ratio control are between 40: 0～0: 40.
4. visible light-responded BiVO according to claim 1
4catalyzer preparation, is characterized in that, in step (2), the temperature of reaction of described hydrothermal synthesis reaction is 60～250 DEG C, and the time is 1～72h.
5. visible light-responded BiVO according to claim 1
4catalyzer preparation, is characterized in that, in step (4), described dry temperature is 20～100 DEG C.
6. visible light-responded BiVO
4catalyzed degradation RhB, is characterized in that comprising in claim 1～5 visible light-responded BiVO described in any claim
4catalyzer.
7. visible light-responded BiVO according to claim 6
4catalysis RhB, its feature: accurately take appropriate photocatalyst BiVO
4put into beaker, pipette the appropriate RhB aqueous solution, lucifuge magnetic agitation, sets up adsorption-desorption balance and dark state molecular balance.Adopt xenon long-arc lamp stabilized current supply as light source, be placed in the cold hydrazine with recirculated water, appropriate Sodium Nitrite is filled to glass clamp shell type isothermal reactor to filter out UV-light, utilize radiation of visible light RhB solution.In walls of beaker and reactor, xenon lamp is at a distance of suitable distance, and solution continues to stir, and gets sample one time at interval of certain hour, and centrifugation obtains clarifying the RhB aqueous solution.Adopt Shimadzu UV-Vis3150 type spectrophotometer to detect the absorbancy of RhB, parameters is: sweep limit 400～700nm, slit 1.0cm.
8. visible light-responded BiVO according to claim 7
4catalyzed degradation RhB, is characterized in that described degradation product comprises methylene blue, rhodamine B, tropeolin-D, Reactive blue M-2GE.Required catalyst levels is controlled between 0.02～1.00g.Described Pollutant levels are controlled between 1～20mg/L.
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Application publication date: 20141022 |