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 PDFInfo
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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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- 239000000463 material Substances 0.000 title claims abstract description 67
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910001868 water Inorganic materials 0.000 claims abstract description 44
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001354 calcination Methods 0.000 claims abstract description 24
- 230000015556 catabolic process Effects 0.000 claims abstract description 23
- 238000006731 degradation reaction Methods 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 229910019501 NaVO3 Inorganic materials 0.000 claims abstract description 20
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 34
- 239000003344 environmental pollutant Substances 0.000 claims description 33
- 231100000719 pollutant Toxicity 0.000 claims description 33
- 230000001699 photocatalysis Effects 0.000 claims description 26
- 238000007146 photocatalysis Methods 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 241000218231 Moraceae Species 0.000 claims description 2
- 235000008708 Morus alba Nutrition 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Substances [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims 4
- 238000006722 reduction reaction Methods 0.000 claims 4
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 111
- 238000001035 drying Methods 0.000 abstract description 17
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 6
- 230000004044 response Effects 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 66
- 238000002835 absorbance Methods 0.000 description 34
- 238000010521 absorption reaction Methods 0.000 description 22
- 238000005286 illumination Methods 0.000 description 16
- 238000005259 measurement Methods 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- 239000006228 supernatant Substances 0.000 description 16
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 16
- 238000011056 performance test Methods 0.000 description 15
- 239000003643 water by type Substances 0.000 description 15
- 239000011668 ascorbic acid Substances 0.000 description 11
- 238000010586 diagram Methods 0.000 description 11
- 230000003595 spectral effect Effects 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000001177 diphosphate Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- YECIFGHRMFEPJK-UHFFFAOYSA-N lidocaine hydrochloride monohydrate Chemical compound O.[Cl-].CC[NH+](CC)CC(=O)NC1=C(C)C=CC=C1C YECIFGHRMFEPJK-UHFFFAOYSA-N 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000001394 sodium malate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts 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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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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
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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