CN102728342A - Preparation method of bismuth vanadate visible light photocatalysis material - Google Patents
Preparation method of bismuth vanadate visible light photocatalysis material Download PDFInfo
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- CN102728342A CN102728342A CN2012101078112A CN201210107811A CN102728342A CN 102728342 A CN102728342 A CN 102728342A CN 2012101078112 A CN2012101078112 A CN 2012101078112A CN 201210107811 A CN201210107811 A CN 201210107811A CN 102728342 A CN102728342 A CN 102728342A
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Abstract
The invention discloses a method for synthesizing a Eu<3+>-doped BiVO4 visible light photocatalysis material by using a citric acid complexed sol-gel method. The preparation method is simple, and the visible light activity of the obtained photocatalyst is high. According to the invention, Bi(NO3)3.5H2O (97%) and NH4VO3 (98.5%) are adopted as source materials; citric acid (99.5%) is adopted as a chelating agent; Eu(NO3)3 is adopted as a doping source material; the pH value is regulated by using ammonia water, and a deep blue sol is prepared; the sol is dried by baking, and is calcined for 5h under the temperature of 500 DEG C, such that the Eu<3+>-doped bismuth vanadate photocatalysis material is obtained. Compared with non-doped bismuth vanadate, oxygen vacancies and V<4+> with catalytic activities in the Eu<3+>-doped bismuth vanadate crystals are increased. After doping, red shift occurs in the light absorption performance of the sample, the band gap can be narrowed, such that the visible light photocatalytic activity is substantially improved. The method provided by the invention is advantaged in simple process, mild condition, and good repeatability. The method can be widely applied in photocatalytic degradation of organic pollutants, and has a good application prospect in environment treatment.
Description
Technical field
The invention belongs to the environmental pollution treatment technology field, relate to a kind of preparation method of pucherite visible-light photocatalysis material.
Background technology
Along with the mankind are constantly developed, the control of environmental pollution is the key subjects that human society faces and is badly in need of solving with administering.In numerous environmental pollution treatment technologies; With the semiconductor is the multiphase photocatalysis process of catalyst, reacts, can directly utilize sunshine to drive advantage such as oxidation-reduction reaction as light source at ambient temperature and become a kind of ideal environment pollution control technology with it.BiVO
4As one type of novel semi-conductor catalysis material; Because of its band gap narrower (about 2.4eV), wavelength response range expands to about 520nm, and photochemical properties is stable; Advantages such as redox ability is strong, and is nontoxic, inexpensive are becoming the focus of visible light photocatalysis research field.Research report BiVO
4Mainly contain 3 kinds of crystal structures, comprise tetragonal crystal system scheelite type (high temperature phase), tetragonal crystal system zirconium silicate type and monoclinic system distortion scheelite type (fergusonite type).The monomers B iVO of monocrystalline scheelite-type structure wherein
4Photocatalytic activity is the highest relatively.But because BiVO
4The conduction band limit be positioned at 0V, its light induced electron is not easy to be caught and in catalyst surface accumulation, increased the recombination probability in electronics and hole by airborne oxygen, causes the organic ability of under visible light, degrading relatively poor.Therefore catch the optical excitation electronics in this case fast, suppress the compound of itself and high energy holes, most important to the efficient that improves this type of photochemical catalyst catalyzing and degrading pollutant by visible light.
For this reason, the researcher has taked multiple means that it is modified and modification, and wherein nonmetal and metal ion mixing is one of conventional means.Zhang etc. adopt the synthetic Si doping BiVO of improved MOD method
4Film Pyrogentisinic Acid's degradation rate obviously improves.Rope waits quietly through the synthetic Cu-BiVO of hydro-thermal method
4Can make ultraviolet/visible light absorption band generation red shift, the clearance of gaseous state toluene is reached 90%.The WO that the method for employing spin coatings such as Chatchai is prepared in the FTO substrate
3/ BiVO
4The photoelectric efficiency of film under visible light obviously strengthens.The synthetic Ag of employing high-temperature calcinations such as Zhang Xiufang supports BiVO
4Film Pyrogentisinic Acid's visible light catalytic efficient and photoelectrocatalysis efficient have improved 61% and 40.5%.The Co doping BiVO that old identical employing template Hydrothermal Preparation goes out
4Have higher visible light activity, irradiation 120min Pyrogentisinic Acid's clearance reaches 75%.Employing hydrothermal synthesis methods such as Zhang Aiping have prepared the BiVO of coin family metal (Cu, Ag and Au) and rare earth metal Ln (Ln=Eu, Gd, Er) doping
4Photochemical catalyst.Its result shows, the BiVO that this two metalloid mixes
4The visible absorption scope of photochemical catalyst has red shift in various degree, and the percent of decolourization of methyl orange is improved greatly.But there are some researches show, influence meeting for mixing with a kind of metal pair photocatalyst activity and there are differences because of different preparation methods.
Summary of the invention
The objective of the invention is deficiency to the low and existing modification technology of pucherite catalysis material visible light catalytic efficient; And a kind of preparation method who prepares the low pucherite visible-light photocatalysis material of simple, the easy operation of process, cost and equipment requirements who provides; The photochemical catalyst that this method obtains has very high visible light catalysis activity, fast the organic pollution in the degradation of dye waste water.
The technical scheme that adopts is:
A kind of preparation method of pucherite visible-light photocatalysis material is characterized in that may further comprise the steps:
1) with Bi (NO
3)
35H
2O (97%), NH
4VO
3(98.5%) be the source material, citric acid (99.5%) is as chelating agent.Molar ratio by 1:2 takes by weighing 0.01 mol, the Bi (NO of 4.8580 g
3)
35H
2O and 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), Citric Acid Mono is joined the 50mL Bi (NO that uses suitable dilute nitric acid dissolution in advance
3)
35H
2In the O solution, get A liquid.Molar ratio by 1:2 takes by weighing 0.01 mol, the NH of 1.1698 g
4VO
3With 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), be dissolved in B liquid in the distilled water of 50mL boiling.Press Bi:V=1:1 mixed in molar ratio A liquid and B liquid, again according to Eu
3+With Bi
3+Mol ratio is respectively 0.1%, 0.2%, 1.0% and 2.0% and adds Eu (NO
3)
3Go into mixed solution, regulate pH value to 6.5 with ammoniacal liquor again, continue to stir down at 80 ℃, evaporation obtains navy blue pucherite precursor colloidal sol at last.
2) the difference amount that the contains Eu that will dry
3+Pucherite precursor colloidal sol, under the air atmosphere condition, in Muffle furnace under 500 ℃ of degree the calcining 4-6 hour, obtain Eu
3+The pucherite catalysis material that mixes.
3) prepared Eu
3+The catalytic effect of doping pucherite visible-light photocatalysis material adopts methyl orange solution to verify.
Eu described in the step 1) of the present invention
3+With Bi
3+Mol ratio is respectively 0.1%, 0.2%, 1.0% and 2.0%.
In order to check the photocatalysis performance of the pucherite that the present invention prepares, it is carried out the experiment of photocatalytic degradation methyl orange.In 250 mL beakers, add 0.01g BiVO
4Photochemical catalyst, 50 mL concentration are the methyl orange solution of 10 mg/L, lucifuge magnetic agitation 20 min are to reach adsorption equilibrium.250 W metal halide lamps are light source, and lamp is apart from 14 cm irradiation methyl orange solution, change the evaluation photocatalyst activity with the absorbance of the methyl orange solutions of 721 type spectrophotometric determination different light times.
The beneficial effect that the present invention has:
1) one of advantage of the present invention is, compares with other preparation methods, and sol-gel process for preparing has following characteristics: synthetic powder is difficult for reuniting good dispersion; Cost is low, easy to operate, is applicable to large-scale commercial production.
2) the present invention provides a kind of efficient, economic and simple preparation method for improving the photocatalytic activity of pucherite at visible-range, selects Eu (NO
3)
3Prepare Eu as doped source
3+Doping pucherite photochemical catalyst can effectively improve photocatalytic activity, promotes the degraded of organic pollution.
3) the UV-vis characterization result shows, Eu
3+Doping narrows down the pucherite energy gap, and its photoresponse scope prolongs, and shows higher photocatalytic activity, has effectively improved the direct utilization to solar energy source.
4) the XPS characterization result shows, doping Eu
3+Make oxygen defect increase in the pucherite, active material V
4+Increase, thereby strengthened the pucherite visible light catalysis activity.6) the inventive method is raw materials used cheaply is easy to get, and utilizes the sol-gal process under the normal temperature and pressure, and calcining obtains Eu in air atmosphere
3+The doping pucherite is separated methyl orange solution in visible light decline and is shown good degradation effect.
Preparation method of the present invention also provides significant reference for the exploitation and the large-scale application of other doping vario-property pucherite catalysis materials.
Description of drawings
Fig. 1 is the prepared pucherite photochemical catalyst UV-vis spectrogram of embodiment 1,2,3,4,5.
Fig. 2 is the prepared pucherite photochemical catalyst XRD figure of embodiment 1,2,3,4,5.
Fig. 3 is that embodiment 1 and 3 prepared pucherite photochemical catalyst SEM scheme.
Fig. 4 is embodiment 1 and 3 prepared pucherite photochemical catalyst V2p XPS resolution figure.
Fig. 5 is embodiment 1 and 3 prepared pucherite photochemical catalyst O2s XPS resolution figure.
Fig. 6 is the prepared pucherite photocatalyst for degrading methyl orange efficiency chart of embodiment 1,2,3,4,5,6.
The specific embodiment
How further specify the present invention below in conjunction with concrete embodiment realizes:
Embodiment 1
The preparation method of the pucherite of present embodiment may further comprise the steps:
1) with Bi (NO
3)
35H
2O (97%), NH
4VO
3(98.5%) be the source material, citric acid (99.5%) is as chelating agent.Molar ratio by 1:2 takes by weighing 0.01 mol, the Bi (NO of 4.8580 g
3)
35H
2O and 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), Citric Acid Mono is joined the 50mL Bi (NO that uses suitable dilute nitric acid dissolution in advance
3)
35H
2In the O solution, get A liquid.Molar ratio by 1:2 takes by weighing 0.01 mol, the NH of 1.1698 g
4VO
3With 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), be dissolved in B liquid in the distilled water of 50mL boiling.Press Bi:V=1:1 mixed in molar ratio A liquid and B liquid, regulate about pH value to 6.5 with ammoniacal liquor, continue to stir down at 80 ℃, evaporation obtains navy blue pucherite precursor colloidal sol at last.
2) the pucherite precursor colloidal sol of oven dry is put into Muffle furnace calcining 5h under 500 ℃, obtain pure pucherite catalysis material.
Fig. 1 (a) is the UV-vis collection of illustrative plates of product, the BiVO that this instance is synthetic
4The light absorption threshold value be 541nm, energy gap is 2.29 eV.Fig. 2 (a) is the XRD figure spectrum of product, the BiVO that this instance is synthetic
418.7
0, 28.8
0, 30.5
0, 34.5
0, 35.1
0, 37.8
0, 39.8
0, 42.4
0, 47.2
0, 53.2
0, 59.8
0, 63.6
0, 69.3
0The characteristic peak that diffraction maximum is the monocline type pucherite appears in the position, and crystalline phase purity is higher, and unit cell volume is 309.21 nm
3Fig. 3 (a) is the SEM figure of product, and by the spheroidal graininess of product shape characteristic type of being of scheming to find out preparation, and particle surface is comparatively smooth, but reunion is arranged slightly.Fig. 4 (a) is that the V2p XPS of product differentiates figure, can find out that by figure the asymmetrical peak dissymmetric peak of V2p appears respectively in sample at Eb=516.09 and 516.78eV, and ownership is V respectively
4+And V
5+Through the XSPEAK match, calculate V
4+/ V
5+Mol ratio is 0.85.Fig. 5 (a) is that the O2s XPS of product differentiates figure, can find out that by figure sample occurs two asymmetrical peak dissymmetric peaks 529.60 with 531.43eV respectively, and ownership is the Lattice Oxygen (O of sample respectively
Latt) and surface adsorbed oxygen (O
Ads), through the XSPEAK match, calculate O
Ads/ O
LattMol ratio is 0.14.
Photocatalysis performance for the pucherite of checking this Experiment Preparation carries out the experiment of photocatalytic degradation methyl orange to it.In 250 mL beakers, add 0.01 g BiVO
4Photochemical catalyst, 50 mL concentration are the methyl orange solution of 10 mg/L, lucifuge magnetic agitation 20 min are to reach adsorption equilibrium.250 W metal halide lamps are light source, and lamp shines methyl orange solution apart from 14 cm, illumination 50min, and the photocatalytic degradation rate of methyl orange reaches 38.45% (Fig. 6 (a)).
Embodiment 2
With Bi (NO
3)
35H
2O (97%), NH
4VO
3(98.5%) be the source material, citric acid (99.5%) is as chelating agent.Molar ratio by 1:2 takes by weighing 0.01 mol, the Bi (NO of 4.8580 g
3)
35H
2O and 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), Citric Acid Mono is joined the 50mL Bi (NO that uses suitable dilute nitric acid dissolution in advance
3)
35H
2In the O solution, get A liquid.Molar ratio by 1:2 takes by weighing 0.01 mol, the NH of 1.1698 g
4VO
3With 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), be dissolved in B liquid in the distilled water of 50mL boiling.Press Bi:V=1:1 mixed in molar ratio A liquid and B liquid, according to Eu
3+With Bi
3+Mol ratio is 0.1% to add Eu (NO
3)
3In mixed solution, regulate about pH value to 6.5 with ammoniacal liquor again, continue to stir down at 80 ℃, evaporation obtains navy blue pucherite precursor colloidal sol at last.
2) the pucherite precursor colloidal sol of oven dry is put into Muffle furnace calcining 5h under 500 ℃, obtain 0.1% Eu
3+Doping pucherite catalysis material.
Fig. 1 (b) is the UV-vis collection of illustrative plates of product, the BiVO that this instance is synthetic
4The light absorption threshold value be 546nm, energy gap is 2.28 eV.Fig. 2 (b) is the XRD figure spectrum of product, the BiVO that this instance is synthetic
418.7
0, 28.8
0, 30.5
0, 34.5
0, 35.1
0, 37.8
0, 39.8
0, 42.4
0, 47.2
0, 53.2
0, 59.8
0, 63.6
0, 69.3
0The characteristic peak that diffraction maximum is the monocline type pucherite appears in the position, but characteristic peak is significantly to low-angle skew, and unit cell volume is 310.07nm
3
Detect the photocatalysis performance of the pucherite that is synthesized according to the described method of embodiment 1, the photocatalytic degradation rate of methyl orange is 51.37% (Fig. 6 (b)) during 50min.
Embodiment 3
According to the preparation method of the present invention of embodiment 2, just with the Eu among the embodiment 2
3+With Bi
3+Mol ratio changes 0.2% into, prepares 0.1% Eu
3+Doping pucherite catalysis material.The product UV-vis collection of illustrative plates that obtains is seen Fig. 1 (c), the BiVO that this instance is synthetic
4The light absorption threshold value be 556nm, energy gap is 2.19 eV.Fig. 2 (c) is the XRD figure spectrum of product, the BiVO that this instance is synthetic
418.7
0, 28.8
0, 30.5
0, 34.5
0, 35.1
0, 37.8
0, 39.8
0, 42.4
0, 47.2
0, 53.2
0, 59.8
0, 63.6
0, 69.3
0The characteristic peak that diffraction maximum is the monocline type pucherite appears in the position, but characteristic peak is significantly to low-angle skew, and unit cell volume is 310.85 nm
3Fig. 3 (b) is the SEM figure of product, and can be found out by figure in the product sample of generation has the part particle by refinement, and grain surface is more coarse, and this may make its specific area increase.Fig. 4 (a) is that the V2p XPS of product differentiates figure, can find out that by figure the asymmetrical peak dissymmetric peak of V2p appears respectively in sample at 516.20eV and 516.94eV, and ownership is V respectively
4+And V
5+Through the XSPEAK match, calculate V
4+/ V
5+Mol ratio is 1.45.Fig. 5 (a) is that the O2s XPS of product differentiates figure, can find out that by figure sample occurs two asymmetrical peak dissymmetric peaks 529.35 with 530.09eV respectively, and ownership is the Lattice Oxygen (O of sample respectively
Latt) and surface adsorbed oxygen (O
Ads), through the XSPEAK match, calculate O
Ads/ O
LattMol ratio is 0.43.
Detect the photocatalysis performance of the pucherite that is synthesized according to the described method of embodiment 1, the photocatalytic degradation rate of methyl orange is 95.02% ((Fig. 6 (c)) during 50min.
Embodiment 4
According to the preparation method of the present invention of embodiment 2, just with the Eu among the embodiment 2
3+With Bi
3+Mol ratio changes 1.0% into, prepares 1.0% Eu
3+Doping pucherite catalysis material.The product UV-vis collection of illustrative plates that obtains is seen Fig. 1 (d), the BiVO that this instance is synthetic
4The light absorption threshold value be 564nm, energy gap is 2.24 eV.Fig. 2 (d) is the XRD figure spectrum of product, the BiVO that this instance is synthetic
418.7
0, 28.8
0, 30.5
0, 34.5
0, 35.1
0, 37.8
0, 39.8
0, 42.4
0, 47.2
0, 53.2
0, 59.8
0, 63.6
0, 69.3
0The characteristic peak that diffraction maximum is the monocline type pucherite appears in the position, but characteristic peak is significantly to low-angle skew, and unit cell volume is 310.79 nm
3By finding out in the table 1, the pucherite of doping 6% is than oxygen defect and V in the pure pucherite crystal of preparation in the instance 1
4+Increase.
Detect the photocatalysis performance of the pucherite that is synthesized according to the described method of embodiment 1, the photocatalytic degradation rate of methyl orange is 88.85 % ((Fig. 6 (d)) during 50min.
Embodiment 5
According to the preparation method of the present invention of embodiment 2, just with the Eu among the embodiment 2
3+With Bi
3+Mol ratio changes 2.0% into,, prepare 2.0% Eu
3+Doping pucherite catalysis material.The product UV-vis collection of illustrative plates that obtains is seen Fig. 1 (e), the BiVO that this instance is synthetic
4The light absorption threshold value be 554 nm, energy gap is 2.27 eV.Fig. 2 (e) is the XRD figure spectrum of product, the BiVO that this instance is synthetic
418.7
0, 28.8
0, 30.5
0, 34.5
0, 35.1
0, 37.8
0, 39.8
0, 42.4
0, 47.2
0, 53.2
0, 59.8
0, 63.6
0, 69.3
0The characteristic peak that diffraction maximum is the monocline type pucherite appears in the position, but characteristic peak begins gradually to the wide-angle skew, and unit cell volume is 309.03 nm
3
Detect the photocatalysis performance of the pucherite that is synthesized according to the described method of embodiment 1, the photocatalytic degradation rate of methyl orange is 60.42 % ((Fig. 6 (e)) during 50min.
Claims (3)
1. the preparation method of a pucherite visible-light photocatalysis material is characterized in that may further comprise the steps:
1) with Bi (NO
3)
35H
2O (97%), NH
4VO
3(98.5%) be the source material, citric acid (99.5%) is as chelating agent; Molar ratio by 1:2 takes by weighing 0.01 mol, the Bi (NO of 4.8580 g
3)
35H
2O and 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), Citric Acid Mono is joined the 50mL Bi (NO that uses suitable dilute nitric acid dissolution in advance
3)
35H
2In the O solution, get A liquid; Molar ratio by 1:2 takes by weighing 0.01 mol, the NH of 1.1698 g
4VO
3With 0.02 mol, the Citric Acid Mono (C of 4.2028 g
6H
8O
7H
2O), be dissolved in B liquid in the distilled water of 50mL boiling; Press Bi:V=1:1 mixed in molar ratio A liquid and B liquid, again according to Eu
3+With Bi
3+Mol ratio is respectively 0.1%, 0.2 0%, and 1.0%, 2.00%, add Eu (NO
3)
3Go into mixed solution, regulate about pH value to 6.5 with ammoniacal liquor, continue to stir down at 80 ℃, evaporation obtains navy blue pucherite precursor colloidal sol at last;
What 2) will dry contains Eu
3+Pucherite precursor colloidal sol install with crucible, put into Muffle furnace in down calcining 4-6 hour of 500 ℃ of degree, obtain Eu
3+The BiVO that mixes
4Catalysis material.
2. the preparation method of a kind of pucherite visible-light photocatalysis material according to claim 1 is characterized in that Eu described in the step 1)
3+With Bi
3+Mol ratio be 0-2.00%.
3. the preparation method of a kind of pucherite visible-light photocatalysis material according to claim 1 is characterized in that the catalytic effect of described high-efficiency photocatalysis material adopts methyl orange solution to verify.
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| CN103170353A (en) * | 2013-04-17 | 2013-06-26 | 东华大学 | Preparation method of heterogeneous visible photocatalyst |
| CN103240107A (en) * | 2013-04-27 | 2013-08-14 | 天津大学 | Silver phosphate-bismuth vanadate multiplex photocatalyst and preparation method thereof |
| CN103950978A (en) * | 2014-04-09 | 2014-07-30 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
| CN107185522A (en) * | 2017-05-26 | 2017-09-22 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of monoclinic form tungsten oxide is combined pucherite high-performance optical catalysis material and its preparation method and application |
| CN107469807A (en) * | 2017-09-08 | 2017-12-15 | 郑州轻工业学院 | A kind of monoclinic phase BiVO4：The high pressure method for preparing of Re catalysis materials |
| CN108927140A (en) * | 2018-04-04 | 2018-12-04 | 山东大学 | It is a kind of with upper conversion Shan Hong light emitting and the rear-earth-doped vanadic acid bismuth material of photocatalysis double function characteristic and its preparation method and application |
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| CN109985618A (en) * | 2019-05-08 | 2019-07-09 | 陕西科技大学 | A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications |
| CN110860283A (en) * | 2019-12-04 | 2020-03-06 | 南通大学 | Preparation method for synthesizing carbon fiber-bismuth vanadate photocatalytic material by hydrothermal method |
| CN111186858A (en) * | 2019-11-26 | 2020-05-22 | 湖南三丰钒业有限公司 | Preparation method of vanadium bismuth red and application of vanadium bismuth red as pigment |
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| CN103170353B (en) * | 2013-04-17 | 2015-05-13 | 东华大学 | Preparation method of heterogeneous visible photocatalyst |
| CN103170353A (en) * | 2013-04-17 | 2013-06-26 | 东华大学 | Preparation method of heterogeneous visible photocatalyst |
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