CN109985618A - A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications - Google Patents

A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications Download PDF

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CN109985618A
CN109985618A CN201910383915.8A CN201910383915A CN109985618A CN 109985618 A CN109985618 A CN 109985618A CN 201910383915 A CN201910383915 A CN 201910383915A CN 109985618 A CN109985618 A CN 109985618A
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bivo
ovs
solution
catalysis material
occupies
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CN109985618B (en
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杨艳玲
毕雅欣
叶晓慧
锁国权
孙瑜
邹鑫鑫
和茹梅
冯雷
侯小江
陈志刚
陈华军
张荔
朱建锋
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20Vanadium, niobium or tantalum
    • B01J23/22Vanadium
    • B01J35/39
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

Abstract

A kind of H for preparing occupies BiVO4The method and its application of-OVs catalysis material, preparation method include: by the Bi (NO of certain molar weight3)3·5 H2O is dissolved in glycerol;By certain molar weight NaVO3·2 H2O dissolves in deionized water;Mix previous solu;Mixed liquor is transferred in the autoclave of polytetrafluoroethyllining lining, 180 DEG C of holding 8h;Solvent-thermal process product is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of drying 4h;By clean solvent thermal reaction product in Muffle furnace 300 DEG C of calcining 5h;Calcined product is in Ar/H2The 10h that anneals at a temperature of 350 DEG C in atmosphere obtains H and occupies BiVO4- OVs catalysis material.The present invention has the advantage that optical response range is wide, catalytic activity is high, degradation rate is fast, hydrolysis ability is strong, can make effective use of solar energy.

Description

A kind of H occupies BiVO4The catalysis material of-OVs, preparation method and applications
Technical field
The present invention relates to catalysis material technical field, in particular to a kind of BiVO for preparing H and occupying oxygen-containing vacancy4 (BiVO4- OVs) catalysis material method and its application.
Background technique
As environmental pollution and energy shortage problem gradually aggravate, photocatalysis technology is defeated as energy by sunlight because of it Enter, there is clean and environmental protection, the advantages such as low in cost, energy is huge, photolysis water hydrogen and in terms of influence it is huge Greatly, the extensive concern of scientists is caused, there is good development prospect.However, photocatalysis technology is still limited by two Influence factor, i.e. spectral response range are narrow low with quantum efficiency, therefore, how to widen spectral absorption, improve solar energy utilization ratio, Inhibit the quick compound of photo-generate electron-hole, becomes the core and key of current research.
Pucherite (BiVO4) forbidden bandwidth be 2.3-2.4eV, valence band location is sufficiently high, it can be achieved that hole is to organic The degradation of object.Conduction band positions are conducive to the reduction of light induced electron, can decompose water and degradation of contaminant under visible light, edge is very Close to H2Evolution current potential has many advantages, such as that take-off potential is low, density of photocurrent is high, it is considered to be most promising optical electro-chemistry (PEC) one of water decomposition optical anode material.But since the diffusion length of carrier is short, light induced electron and hole are easy compound, make PhotoelectrocatalytiPerformance Performance reduces, and becomes limitation BiVO4An important factor for extensive use.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of H for preparing to occupy BiVO4-OVs The method and its application of catalysis material, H occupy BiVO4- OVs catalysis material band gap reduces, and light absorption improves, light absorption range It is broadening, there is excellent photocatalysis performance.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of H for preparing occupies BiVO4The method of-OVs catalysis material, comprising the following steps:
Step 1:
By the Bi (NO of certain molar weight3)3·5 H2O, which is dissolved in glycerol, obtains precursor solution A;
Step 2:
By certain molar weight NaVO3·2 H2O dissolution obtains precursor solution B in deionized water;
Step 3:
Solution B is added in solution A and is vigorously stirred, solution C is obtained;
Step 4:
Solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
Step 5:
Solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, after 60 DEG C of 4 h of drying Obtain product E;
Step 6:
Product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
Step 7:
Product F is in Ar/H210 h that anneal at a temperature of 350 DEG C in atmosphere obtain H and occupy BiVO4- OVs catalysis material.
The temperature range of solvent heat is 120 DEG C~200 DEG C in the step 4.
The reaction time range of solvent heat is 6~12 h in the step 4.
Calcination temperature range is 250 DEG C~450 DEG C in the step 6.
The calcination time range is the h of 5 h~24.
Annealing region is 300 DEG C~400 DEG C in the step 7.
Annealing time range is the h of 5h~12 in the step 7.
Ar/H in the step 72Proportional region is 95 %:30 of %:5 %~70 %.
H occupies BiVO4- OVs catalysis material is applied to photocatalysis technology, such as contaminant degradation, photodegradation water.With The Xe lamp of 300 W is light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml rhodamine B (Rh B) solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Beneficial effects of the present invention:
Using solvent heat-post annealed method, prepares H and occupy BiVO4- OVs catalysis material.Lacking oxygen in the composite material Near infrared light can be absorbed, increase active site and oxygen molecule is converted to active material participation redox reaction;? BiVO4Conduction band below formed defect state, make its forbidden bandwidth reduce, improve catalyst light abstraction width;Meanwhile as photoproduction Electronics trap center can efficiently separate electron-hole pair under the excitation of long wavelength and transfer them to catalyst surface, suppression Compound, the raising photocatalysis efficiency of light induced electron processed and hole.In BiVO4H is introduced in-OVs2, made by the H valence band for occupying the vacancy O For defect level or shallow donor's energy level, band gap width is reduced, and light abstraction width increases, and absorbance significantly improves.As photocatalysis Material has the advantage that separation of charge rate is high, light abstraction width is wide, photocatalytic activity is high, degradation rate is fast, hydrolysis ability is strong.
Detailed description of the invention
Fig. 1 is that H occupies BiVO4- OVs catalysis material preparation process schematic diagram;
Fig. 2 is that H occupies BiVO4The XRD diagram picture of-OVs catalysis material;
Fig. 3 is that H occupies BiVO4The SEM image of-OVs catalysis material;
Fig. 4 is that H occupies BiVO4The Raman spectral image of-OVs catalysis material;
Fig. 5 is that H occupies BiVO4The UV, visible light near infrared absorption image of-OVs catalysis material.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 120 DEG C of 6 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 2
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material, is denoted as OVH-BiVO4, photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 3
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 10 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and occupy BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 4
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 200 DEG C of 12 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 5
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 250 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 6
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 7
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 350 DEG C of 10 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 8
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 450 DEG C of 12 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 9
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 300 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 5 h that anneal under atmosphere obtain H and occupy BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 10
(1) by 2.0 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:95%:5%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 11
(1) by 1.2mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 400 DEG C in atmosphere, Ar/H2(Vol:90%:10%) 12 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 12
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
(7) product F is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:80%:20%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Gained H occupies BiVO4- OVs catalysis material photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 13
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
Products therefrom E is calcined without Muffle furnace, not in Ar/H2It anneals under reducing atmosphere, is denoted as OV'-BiVO4, photocatalysis Performance test methods are as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 14
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E 300 DEG C of 5 h of calcining in Muffle furnace obtain product F;
Products therefrom F is not in Ar/H2It anneals under reducing atmosphere, is denoted as OV-BiVO4, photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Embodiment 15
(1) by 0.4 mmol Bi (NO3)3·5 H2O is dissolved in 16 ml glycerol and obtains precursor solution A;
(2) by 0.4 mmol NaVO3·2 H2O is dissolved in 16 ml deionized waters and obtains precursor solution B;
(3) solution B is added in solution A and be vigorously stirred, obtain solution C;
(4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, obtains synthetic product D after 180 DEG C of 8 h of holding;
(5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing, 60 DEG C of 4 h of drying After obtain product E;
(6) product E is in Ar/H2At 350 DEG C in atmosphere, Ar/H2(Vol:80%:20%) 10 h that anneal under atmosphere obtain H and account for According to BiVO4- OVs catalysis material.
Products therefrom E is calcined without Muffle furnace, is denoted as OVH'-BiVO4, photocatalysis performance test method is as follows:
Using the Xe lamp of 300 W as light source, with the edge filter simulated solar irradiation less than 800 nm wavelength.Measure 50 ml Luo Dan Bright B solution is added 20 ml catalyst and carries out ultrasonic disperse.Before illumination, 30 min of absorption stirring make catalyst in the dark Reach adsorption equilibrium with pollutant.After turning on light, 4 mL samples are taken from reaction vessel every fixing 20 min.The sample taken out every time Product are separated photochemical catalyst with solution with the supercentrifuge of 10000 r/min, take supernatant liquor, with UV-vis spectroscopy light The absorbance of degree meter measurement Rh B, judges catalyst to the degradation efficiency of pollutant solution according to absorbance.
Referring to fig. 2, Fig. 2 is that H occupies BiVO4The XRD diagram picture of-OVs catalysis material.In figure: whether a. passes through Muffle furnace The BiVO for not adding H of calcining4XRD diagram picture, i.e. the XRD diagram picture of embodiment 13 and the made sample of embodiment 14;B. whether pass through Cross Muffle furnace calcining plus H BiVO4XRD diagram picture, i.e. the XRD diagram picture of embodiment 15 and the made sample of embodiment 2: c. is not By Muffle furnace calcining plus before and after H BiVO4XRD diagram picture, i.e. the XRD diagram of embodiment 15 and the made sample of embodiment 13 Picture: d. is by Muffle furnace calcining plus before and after H the BiVO containing Lacking oxygen4XRD diagram picture, i.e. embodiment 2 and embodiment The XRD diagram picture of 14 made samples.
Referring to Fig. 3, Fig. 3 is that H occupies BiVO4The SEM image of-OVs catalysis material, i.e. OV obtained by embodiment 2H- BiVO4The SEM image of catalysis material;Can obviously observe that sample topography is obvious and size uniformity, radius size 500~ 600nm or so, is in mulberries shape structure, and rough surface provides more reactivity sites for light-catalyzed reaction, is conducive to photoproduction The capture of electronics.
Referring to fig. 4, Fig. 4 is that H occupies BiVO4The Raman spectral image of-OVs catalysis material, i.e. embodiment 2, embodiment 13, embodiment 14, H occupies BiVO obtained by embodiment 154The Raman spectral image of-OVs catalysis material;It can be observed to exist The OV-BiVO of Lacking oxygen4Compare BiVO4Peak position is consistent, and peak value reduces, the presence of provable Lacking oxygen.Meanwhile H occupies BiVO4- OVs, that is, OVH-BiVO4Compared to OV-BiVO4Peak value is substantially reduced, and illustrates that H partially or completely occupies Lacking oxygen.Pass through Raman light The presence of provable Lacking oxygen is composed, also provable H can partially or completely occupy Lacking oxygen.
Referring to Fig. 5, Fig. 5 is that H occupies BiVO4The UV, visible light near infrared absorption image of-OVs catalysis material, that is, implement Example 2, embodiment 13, embodiment 14, H occupies BiVO obtained by embodiment 154The UV, visible light near-infrared of-OVs catalysis material Absorption image;By BiVO can be observed in figure4There is obvious absorption within 500 nm visible lights;OV-BiVO4Compared to BiVO4Out Existing Red Shift Phenomena, it is seen that light abstraction width increases, it was demonstrated that Lacking oxygen is conducive to expand optical response range;Calcined without Muffle furnace, By H2The OV of annealingH'-BiVO4There is absorption in the full spectral region of 200~2500 nm, and absorptivity reaches 0.4 or more;Through Cross Muffle furnace calcining, by H2The OV of annealingH-BiVO4In the full spectral region absorptivity of 200~2500 nm up to 0.9 or more, have There are broader light abstraction width and stronger light absorpting ability, photocatalytic activity significantly improves.
A kind of H for preparing provided by the invention occupies BiVO as can be seen from the above embodiments4- OVs photocatalyst material system Preparation Method step is simple, and the H of preparation occupies BiVO4- OVs photocatalyst material optical response range increases, carrier separation rate mentions Height has the advantage that catalytic activity is high, degradation rate is fast, hydrolysis ability is strong as catalysis material, is the efficient benefit of solar energy With offer new approaches.
H occupies BiVO4- OVs technology is to solve BiVO4Band gap issues and Carrier recombination problem provide opportunity, it is coarse Porous BiVO4Help to adsorb more polyelectron progress redox reaction, after introducing Lacking oxygen defect, Lacking oxygen absorbs close red Outer light, increases light absorption range, and active site increases.H generates new defect level or shallow donor's energy level, band gap after occupying the vacancy O Width is reduced, and light abstraction width increases, and absorbance has larger improvement, and photocatalytic activity significantly improves.Preparation H occupies BiVO4- OVs catalysis material is to solve that catalysis material greater band gap, optical response range is narrow, electron-hole is easily compound efficacious prescriptions Method and reliable approach.

Claims (10)

1. a kind of H occupies BiVO4The catalysis material of-OVs, which is characterized in that hydrogen moiety fully takes up oxygen-containing vacancy BiVO4Lacking oxygen in structure.
2. a kind of H according to claim 1 occupies BiVO4The catalysis material of-OVs, which is characterized in that there is nanoscale Mulberries shape pattern.
3. a kind of H occupies BiVO4The preparation method of the catalysis material of-OVs, which comprises the following steps:
By the BiVO of oxygen-containing vacancy4Reduction reaction is carried out under hydrogen reduction atmosphere, is obtained a kind of H and is occupied BiVO4The photocatalysis of-OVs Material.
4. a kind of H according to claim 3 occupies BiVO4The preparation method of the catalysis material of-OVs, which is characterized in that The hydrogen reduction atmosphere is Ar:H2Volume ratio is the Ar/H of 95 %:30 of %:5 %~70 %2Mixed atmosphere.
5. a kind of H according to claim 3 occupies BiVO4The preparation method of the catalysis material of-OVs, which is characterized in that The reduction reaction temperature is 300 ~ 400 DEG C.
6. a kind of H according to claim 3 occupies BiVO4The preparation method of the catalysis material of-OVs, which is characterized in that The BiVO of the oxygen-containing vacancy4It is obtained by method comprising the following steps: by BiVO4In 250 DEG C~450 DEG C calcining 5h~for 24 hours, Obtain the BiVO of oxygen-containing vacancy4
7. a kind of H according to claim 6 occupies BiVO4The preparation method of the catalysis material of-OVs, which is characterized in that The BiVO4It is obtained by method comprising the following steps: Bi (NO will be dispersed with3)3·5 H2And NaVO O,3·2 H2The dispersion of O Body obtains BiVO in 120 DEG C~200 DEG C progress solvent thermal reactions4
8. a kind of H according to claim 7 occupies BiVO4The preparation method of the catalysis material of-OVs, which is characterized in that Bi(NO3)3·5 H2O and NaVO3·2 H2O molar ratio is 1:1~5:1.
9. occupying BiVO according to a kind of described in any item H of claim 3 ~ 84The preparation method of the catalysis material of-OVs, it is special Sign is that specific steps include:
1) by Bi (NO3)3·5 H2O, which is dissolved in glycerol, obtains precursor solution A;
2) by NaVO3·2 H2O dissolution obtains precursor solution B in deionized water;
3) solution B is added in solution A and be vigorously stirred, obtain solution C;Bi(NO3)3·5 H2O and NaVO3·2 H2O molar ratio For 1:1~5:1;The volume ratio of solution A and solution B is 1:1~5:1;
4) solution C is transferred in the autoclave of polytetrafluoroethyllining lining, and synthesis is obtained after 120 DEG C~200 DEG C 6~12h of holding and is produced Object D;
5) solvent-thermal process product D is centrifugated by 10000 rpm, deionized water and ethanol washing are produced after dry Object E;
6) product E 250 DEG C~450 DEG C calcining 5h~obtain product F for 24 hours in Muffle furnace;
7) product F is in Ar/H2The h of 5 h~12 that anneals at a temperature of 300 DEG C~400 DEG C in atmosphere obtains H and occupies BiVO4-OVs Catalysis material;The Ar/H2Volume ratio is 95 %:30 of %:5 %~70 %.
10. a kind of H of any of claims 1 or 2 occupies BiVO4The catalysis material of-OVs is for photocatalytic pollutant degradation Using.
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CN115608352B (en) * 2022-09-23 2024-04-05 山东大学 BiVO with spatial oxygen vacancy distribution 4 Photocatalytic material and preparation method and application thereof

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