CN111151238B - Bismuth vanadate heterojunction BiVO4/Bi25VO40Material, preparation method and application thereof - Google Patents
Bismuth vanadate heterojunction BiVO4/Bi25VO40Material, preparation method and application thereof Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 59
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 59
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000012670 alkaline solution Substances 0.000 claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 27
- 239000003513 alkali Substances 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 22
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 18
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012265 solid product Substances 0.000 claims abstract description 17
- 239000003929 acidic solution Substances 0.000 claims abstract description 13
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 20
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium superoxide Chemical compound [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002957 persistent organic pollutant Substances 0.000 claims description 6
- 239000011941 photocatalyst Substances 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 6
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 6
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 6
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003599 detergent Substances 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 3
- 229940049676 bismuth hydroxide Drugs 0.000 claims description 3
- 229910001451 bismuth ion Inorganic materials 0.000 claims description 3
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 3
- TZSXPYWRDWEXHG-UHFFFAOYSA-K bismuth;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Bi+3] TZSXPYWRDWEXHG-UHFFFAOYSA-K 0.000 claims description 3
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 3
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 3
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 claims description 3
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 14
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000004098 Tetracycline Substances 0.000 description 13
- 229960002180 tetracycline Drugs 0.000 description 13
- 229930101283 tetracycline Natural products 0.000 description 13
- 235000019364 tetracycline Nutrition 0.000 description 13
- 150000003522 tetracyclines Chemical class 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 12
- 238000000967 suction filtration Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 229940088710 antibiotic agent Drugs 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000003637 basic solution Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 241000202807 Glycyrrhiza Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910016001 MoSe Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000035755 proliferation Effects 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
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
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- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The invention provides a bismuth vanadate heterojunction BiVO4/Bi25VO40A preparation method of a material belongs to the technical field of catalysis. The preparation method comprises the following steps: (1) dissolving a vanadium source and a bismuth source in an acidic solution, adding an alkaline solution, and carrying out a precipitation reaction; (2) carrying out hydrothermal reaction on a system obtained by the precipitation reaction, and separating to obtain a solid product; (3) dispersing the solid product in an alkaline solution, carrying out alkali treatment, and separating to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material. The invention can realize bismuth vanadate heterojunction BiVO by adopting two steps of hydrothermal reaction-alkali treatment4/Bi25VO40The material is synthesized in situ, the method is simple, and the prepared material has excellent photocatalytic degradation performance.
Description
Technical Field
The invention relates to the technical field of catalysis, in particular to a bismuth vanadate heterojunction BiVO4/Bi25VO40A material and a preparation method and application thereof.
Background
Antibiotics are an effective drug for the treatment of human diseases and bacterial infections in animals. With the development of medicine, the use amount and the production amount of antibiotics are larger and larger, and the ecological environment is seriously polluted by the overuse and abuse of the antibiotics. Antibiotics generally cannot be decomposed by conventional wastewater treatment methods due to inhibition of bacterial proliferation. Therefore, there is an urgent need to find an effective strategy for removing antibiotics from water bodies. The photocatalytic oxidation method is an effective method for degrading organic pollutants, and can convert macromolecular organic pollutants into low-toxicity organic micromolecules, carbon dioxide and water at normal temperature and normal pressure by directly utilizing sunlight through a semiconductor photocatalyst without adding an oxidant.
Bismuth vanadate is a visible light catalytic material, has the characteristics of good chemical stability, high sunlight utilization rate, no toxicity and the like, and draws wide attention. Wherein the monoclinic BiVO4Is the most studied bismuth vanadate material, has a narrow band gap (about 2.4eV) and strong visible light absorption capacity, but the monoclinic BiVO is greatly limited by the low electron-hole separation efficiency4The photocatalytic application of (1).
The construction of the heterojunction material based on bismuth vanadate can obviously improve the photocatalytic activity of the heterojunction material. For example: peng et al (Chemical Engineering Journal,2014,236,430-437) synthesized C-Bi by first hydrothermal method followed by calcination at 600 deg.C2WO6/BiVO4The result of the heterojunction shows that the catalyst has excellent performance in the photocatalytic reaction for degrading rhodamine B. Luo et al (Journal of colloid and Interface Science,2018,532,456-463) synthesized peanut-like MoSe by a two-step hydrothermal method2/BiVO4The heterojunction catalyst shows obviously improved photocatalytic performance in the reaction of degrading the glycyrrhiza phosphine. However, current reports are limited to the construction of heterojunctions between bismuth vanadate and another semiconductor using a multi-step, complex approach.
Disclosure of Invention
The invention aims to provide a bismuth vanadate heterojunction BiVO4/Bi25VO40The invention adopts two steps of simple hydrothermal reaction-alkali treatment to realize bismuth vanadate heterojunction BiVO4/Bi25VO40And (3) in-situ synthesis of the material.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a bismuth vanadate heterojunction BiVO4/Bi25VO40The preparation method of the material comprises the following steps:
(1) dissolving a vanadium source and a bismuth source in an acidic solution, adding an alkaline solution, and carrying out a precipitation reaction;
(2) carrying out hydrothermal reaction on a system obtained by the precipitation reaction, and separating to obtain a solid product;
(3) dispersing the solid product in an alkaline solution, carrying out alkali treatment, and separating to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
Preferably, in the step (1),
the bismuth source is one or more of bismuth chloride, bismuth nitrate, bismuth sulfate, bismuth trioxide and bismuth hydroxide;
the vanadium source is one or more of vanadium trichloride, ammonium vanadate, sodium vanadate, ammonium metavanadate and sodium metavanadate;
the mass ratio of bismuth ions in the bismuth source to vanadium ions in the vanadium source is (0.1-10): 1.
preferably, in the step (1),
the concentration of the acidic solution and the concentration of the alkaline solution are 0.1-5 mol/L independently;
the solvent of the acidic solution and the solvent of the alkaline solution are one or more of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide independently;
the solute of the acid solution is one or more of hydrochloric acid, nitric acid, sulfuric acid and acetic acid;
the solute of the alkaline solution is one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide.
Preferably, in the step (1), the temperature of the precipitation reaction is room temperature, and the time is 0.5-10 h.
Preferably, in the step (2), the temperature of the hydrothermal reaction is 100-250 ℃ and the time is 1-24 h.
Preferably, in the step (3), the temperature of the alkali treatment is 25-150 ℃, and the heat preservation time is 0.3-12 h.
Preferably, in the step (3),
the solvent of the alkaline solution is one or more of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the solute is one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide; the concentration of the alkaline solution is 0.1-5 mol/L.
Preferably, in the steps (2) and (3), after separation, the obtained solid is washed and dried; the washing detergent is two or three of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the drying temperature is 40-100 ℃, and the heat preservation time is 6-24 h.
The invention provides bismuth vanadate heterojunction BiVO prepared by the preparation method in the scheme4/Bi25VO40A material.
The invention provides a bismuth vanadate heterojunction BiVO adopting the scheme4/Bi25VO40The material is used as a photocatalyst in the application of photocatalytic degradation of organic pollutants.
The invention provides a bismuth vanadate heterojunction BiVO4/Bi25VO40The preparation method of the material comprises the following steps: (1) dissolving a vanadium source and a bismuth source in an acidic solution, adding an alkaline solution, and carrying out a precipitation reaction; (2) carrying out hydrothermal reaction on a system obtained by the precipitation reaction, and separating to obtain a solid product; (3) dispersing the solid product in an alkaline solution, carrying out alkali treatment, and separating to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material. The invention can realize bismuth vanadate heterojunction BiVO by adopting two steps of hydrothermal reaction-alkali treatment4/Bi25VO40The in-situ synthesis of the material has the advantages of simple method, no need of a template, mild conditions, no need of high temperature and high pressure, simple and easy operation and high efficiency.
BiVO is formed by adopting the method of the invention4/Bi25VO40The heterojunction is favorable for the effective separation and conduction of electron-hole pairs, so that the prepared bismuth vanadate heterojunction BiVO4/Bi25VO40The material has excellent photocatalytic degradation performance.
The results of the examples show that the invention is appliedBismuth vanadate heterojunction BiVO prepared by Ming method4/Bi25VO40The material is applied to photocatalytic degradation of organic pollutant tetracycline under visible light, and after 1h of adsorption and 2h of visible light photocatalytic degradation under a dark state, the tetracycline removal efficiency can reach over 72 percent.
Drawings
FIG. 1 is a scanning electron micrograph of a material prepared in example 1;
FIG. 2 is an XRD pattern of the materials obtained in examples 1 to 3;
FIG. 3 is a graph showing the effect of the material prepared in examples 1 to 3 when applied to photocatalytic degradation of tetracycline.
Detailed Description
The invention provides a bismuth vanadate heterojunction BiVO4/Bi25VO40The preparation method of the material comprises the following steps:
(1) dissolving a vanadium source and a bismuth source in an acidic solution, adding an alkaline solution, and carrying out a precipitation reaction;
(2) carrying out hydrothermal reaction on a system obtained by the precipitation reaction, and separating to obtain a solid product;
(3) dispersing the solid product in an alkaline solution, carrying out alkali treatment, and separating to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material;
in the present invention, the starting materials used are all commercially available products well known in the art, unless otherwise specified.
The vanadium source and the bismuth source are dissolved in an acidic solution, and an alkaline solution is added to carry out precipitation reaction.
In the present invention, the vanadium source is preferably one or more of vanadium trichloride, ammonium vanadate, sodium vanadate, ammonium metavanadate and sodium metavanadate, and more preferably ammonium metavanadate. When the vanadium source comprises a plurality of substances, the distribution proportion of the vanadium source to the substances is not specially required, and the vanadium source can be prepared in any proportion. In the present invention, the bismuth source is preferably one or more of bismuth chloride, bismuth nitrate, bismuth sulfate, bismuth trioxide and bismuth hydroxide, and more preferably bismuth nitrate. When the bismuth source comprises a plurality of substances, the invention has no special requirements on the distribution ratio of the substances and can be used in any ratio. The vanadium source and the bismuth source may be the corresponding hydrates. In the present invention, the ratio of the amounts of the bismuth ion in the bismuth source to the vanadium ion in the vanadium source is preferably (0.1 to 10): 1, more preferably (1 to 8): 1, most preferably 1: 1.
in the present invention, the solvent of the acidic solution and the basic solution is independently preferably one or more of water, ethanol, diethyl ether, acetone, and N, N-dimethylformamide, and more preferably water. The solute of the acid solution is preferably one or more of hydrochloric acid, nitric acid, sulfuric acid and acetic acid; the solute of the alkaline solution is preferably one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide. In the invention, the concentration of the acidic solution and the concentration of the alkaline solution are independently preferably 0.1-5 mol/L, and more preferably 1-4 mol/L.
The method has no special requirement on the dosage of the acidic solution, and can be used for completely dissolving the vanadium source and the bismuth source. In the present invention, the amount of the alkaline solution is preferably such that the pH of the system is 0.5 to 6, and more preferably 0.8 to 4.
In the invention, the temperature of the precipitation reaction is preferably room temperature, and the time of the precipitation reaction is preferably 0.5-10 h, more preferably 1-8 h, and most preferably 2-6 h. In the present invention, the precipitation reaction is preferably carried out under stirring conditions, and the stirring conditions are not particularly limited in the present invention, and may be those well known in the art.
In the precipitation reaction process, the bismuth source and the vanadium source are dissolved and then react to generate amorphous tetragonal phase BiVO4。
After the precipitation reaction is finished, the method does not need any post-treatment, directly carries out hydrothermal reaction on a system obtained by the precipitation reaction, and obtains a solid product after separation.
In the invention, the temperature of the hydrothermal reaction is preferably 100-250 ℃, more preferably 130-220 ℃, and most preferably 160-200 ℃; the time is preferably 1 to 24 hours, more preferably 5 to 20 hours, and most preferably 10 to 15 hours. In the present invention, the hydrothermal reaction is preferably carried out in a hydrothermal reaction vessel. According to the invention, the temperature is preferably raised from room temperature to the temperature of the hydrothermal reaction, and the heating rate is preferably 0.2-10 ℃/min, and more preferably 3-7 ℃/min.
In the hydrothermal reaction process, amorphous tetragonal phase BiVO4Converted into monoclinic phase BiVO with high crystallinity4。
After the hydrothermal reaction, the invention separates the product system of the hydrothermal reaction. The hydrothermal reaction product system is preferably cooled to room temperature and then separated. The invention has no special requirements on the separation mode, and particularly can be suction filtration. After separation, the invention preferably also comprises washing and drying the solid material obtained after separation to obtain a solid product (high-crystallinity monoclinic phase BiVO)4). The washing detergent is preferably two or three of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the drying temperature is preferably 40-100 ℃, and the heat preservation time is preferably 6-24 h. In the present invention, the solid product is a yellow powdery solid.
After a solid product is obtained, the solid product is dispersed in an alkaline solution for alkali treatment and separated to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
In the present invention, the solvent of the basic solution is preferably one or more of water, ethanol, diethyl ether, acetone, and N, N-dimethylformamide, and more preferably water; the solute is preferably one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide, and is more preferably sodium hydroxide; the concentration of the alkaline solution is preferably 0.1-5 mol/L, more preferably 0.5-4 mol/L, and most preferably 1-3 mol/L. The invention has no special requirement on the dosage of the alkaline solution, and the solid product can be completely immersed. The dispersion mode of the solid product is not particularly required by the invention, and the dispersion mode which is well known in the field can be adopted.
In the invention, the temperature of the alkali treatment is preferably 25-150 ℃, more preferably 40-120 ℃, and most preferably 50-90 ℃; the heat preservation time is preferably 0.3-12 h, more preferably 0.5-10 h, and most preferably 1-6 h. In the present invention, the alkali treatment is preferably performed under stirring. In the invention, the temperature is preferably raised from room temperature to the temperature for alkali treatment, and the heating rate is preferably 0.2-10 ℃/min, and more preferably 3-7 ℃/min. In the present invention, the heating means of the alkali treatment is preferably water bath, oil bath or rotary oven hydrothermal.
In the alkali treatment process, part of BiVO4Conversion to Bi25VO40Finally obtaining bismuth vanadate heterojunction BiVO4/Bi25VO40. Bismuth vanadate heterojunction BiVO4/Bi25VO40BiVO with single material4And Bi25VO40Is more beneficial to the effective separation and conduction of electron-hole pairs, thereby having more excellent photocatalytic performance.
After the alkali treatment is finished, the system is separated to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material. The present invention preferably cools the system to room temperature before separation. The present invention has no special requirement on the separation mode, and the separation mode known in the field can be adopted, such as suction filtration.
After separation, the invention preferably also comprises washing and drying the solid obtained by separation; the washing detergent is preferably two or three of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the drying temperature is preferably 40-100 ℃, and the heat preservation time is preferably 6-24 h.
The invention provides bismuth vanadate heterojunction BiVO prepared by the preparation method in the scheme4/Bi25VO40A material. In the invention, the bismuth vanadate heterojunction BiVO4/Bi25VO40The material comprises BiVO4And Bi25VO40(ii) a Bismuth vanadate heterojunction BiVO4/Bi25VO40The material is preferably in powder form. The bismuth vanadate heterojunction BiVO is prepared by the method4/Bi25VO40BiVO in material4And Bi25VO40The content of (b) is not particularly limited and is determined according to the preparation method. In the invention, the BiVO4Is prismatic, said Bi25VO40Is cubic block.
The invention provides a bismuth vanadate heterojunction BiVO adopting the scheme4/Bi25VO40The material is used as a photocatalyst in the application of photocatalytic degradation of organic pollutants. In the present invention, the organic contaminant is preferably tetracycline. The invention has no special requirements for the mode of application, and can be applied by the mode of application well known in the field.
The bismuth vanadate heterojunction BiVO provided by the invention is combined with the embodiment4/Bi25VO40The materials, methods of preparation and uses thereof are described in detail, but they are not to be construed as limiting the scope of the invention.
Example 1
(1) Respectively weighing 10mmol of bismuth nitrate pentahydrate and 10mmol of ammonium metavanadate in 60mL of 2mol/L nitric acid solution, converting into yellow transparent solution under magnetic stirring, adding a certain volume of ammonia water to adjust the pH value of the solution to 1, and continuously stirring for 2 hours to obtain yellow precipitate.
(2) And transferring the system obtained by the precipitation reaction into a hydrothermal reaction kettle, heating the hydrothermal reaction kettle to 200 ℃ in an oven, and carrying out hydrothermal reaction for 10 hours at 200 ℃. And cooling the reaction kettle to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 24 hours to obtain yellow powder solid.
(3) The yellow powder solid obtained in the above step was dispersed in 60mL of 2mol/L sodium hydroxide solution, and the solution was heated to 60 ℃ by means of an oil bath under magnetic stirring and kept at 60 ℃ for 3 hours for alkali treatment. After the reaction is finished, cooling to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 24 hours to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
Bismuth vanadate heterojunction BiVO prepared in the example4/Bi25VO40The material was analyzed by scanning electron microscopy, and the results are shown in FIG. 1Bi having cubic block shape after hydrothermal reaction-alkali treatment25VO40BiVO appeared and combined with prism4Close contact shows that BiVO is synthesized4/Bi25VO40A heterojunction.
Example 2
(1) Respectively weighing 3mmol of bismuth nitrate pentahydrate and 3mmol of ammonium metavanadate in 60mL of 2mol/L nitric acid solution, converting into yellow transparent solution under magnetic stirring, adding a certain volume of ammonia water to adjust the pH value of the solution to 0.5, and continuously stirring for 2 hours to obtain yellow precipitate.
(2) And transferring the system obtained by the precipitation reaction into a hydrothermal reaction kettle, heating the hydrothermal reaction kettle to 200 ℃ in an oven, and carrying out hydrothermal reaction for 10 hours at 200 ℃. And cooling the reaction kettle to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 12 hours to obtain yellow powder solid.
(3) The yellow powder solid obtained in the above step is dispersed in 60mL of 1.5mol/L sodium hydroxide solution, the solution is heated to 50 ℃ by means of water bath under magnetic stirring, and is kept at 50 ℃ for 5h for alkali treatment. After the reaction is finished, cooling to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 12 hours to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
Example 3
(1) Respectively weighing 5mmol of bismuth nitrate pentahydrate and 5mmol of ammonium metavanadate in 60mL of 2mol/L nitric acid solution, converting into yellow transparent solution under magnetic stirring, adding a certain volume of ammonia water to adjust the pH value of the solution to 0.8, and continuously stirring for 2 hours to obtain yellow precipitate.
(2) And transferring the system obtained by the precipitation reaction into a hydrothermal reaction kettle, heating the hydrothermal reaction kettle to 200 ℃ in an oven, and carrying out hydrothermal reaction for 10 hours at 200 ℃. And cooling the reaction kettle to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 18h to obtain yellow powder solid.
(3) The yellow powder solid obtained in the above step is dispersed in 60mL of 1mol/L sodium hydroxide solution,the solution was warmed to 80 ℃ by means of an oil bath with magnetic stirring and kept at 80 ℃ for 1h for the alkali treatment. After the reaction is finished, cooling to room temperature, carrying out suction filtration and washing on the obtained solid, and finally transferring the solid into an oven to keep the temperature at 60 ℃ for 18h to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
Bismuth vanadate heterojunction BiVO prepared in examples 1 to 34/Bi25VO40The X-ray powder diffraction analysis showed that the diffraction peak in the graph was BiVO as shown in FIG. 24(PDF #14-0688) and Bi25VO40(PDF #46-0419), and no impurity peaks appeared, reflecting the good crystallinity and high purity of the sample.
Application example 1
100mg of BiVO obtained in example 1 were weighed out in a photoreactor4/Bi25VO40A sample is taken as a photocatalyst to be dispersed in 100mL of 30mg/L tetracycline solution, the tetracycline is adsorbed on the photocatalyst for 1h under the dark condition to achieve adsorption-desorption balance, and 4mL of liquid is taken out every 30min during the adsorption-desorption balance, and then the ultraviolet visible absorption spectrum test is carried out after the catalyst is separated. Then, the photo-reactor is irradiated under visible light with the wavelength of more than 420 nm for carrying out the photocatalytic reaction for 2h, 4mL of liquid is taken out every 20min for centrifugation, and the ultraviolet visible absorption spectrum test is carried out after the catalyst is separated. FIG. 3 shows bismuth vanadate heterojunction BiVO4/Bi25VO40The material has photocatalytic degradation performance on tetracycline under visible light. As can be seen from FIG. 3, BiVO4/Bi25VO40The material shows excellent photocatalytic performance, the concentration of the tetracycline is reduced to 96% of the initial concentration after 1h of adsorption, and the removal efficiency of the tetracycline can reach over 66% after 2h of visible light photocatalytic degradation. Illustrating the BiVO formed4/Bi25VO40The heterojunction is beneficial to the effective separation and conduction of electron-hole pairs, and shows higher photocatalytic activity.
Application example 2
The same procedure as in application example 1 was followed except that the material obtained in example 1 was changed to BiVO obtained in example 24/Bi25VO40Sample, results show that BiVO prepared in example 24/Bi25VO40The material shows excellent photocatalytic performance, the concentration of the tetracycline is reduced to 95% of the initial concentration after 1h of adsorption, and the tetracycline removal efficiency can reach more than 67% after 2h of visible light photocatalytic degradation. Illustrating the BiVO formed4/Bi25VO40The heterojunction is beneficial to the effective separation and conduction of electron-hole pairs, and shows higher photocatalytic activity.
Application example 3
The same procedure as in application example 1 was followed except that the material obtained in example 1 was changed to BiVO obtained in example 34/Bi25VO40Sample, results show that BiVO prepared in example 34/Bi25VO40The material shows excellent photocatalytic performance, the concentration of the tetracycline is reduced to 95% of the initial concentration after 1h of adsorption, and the tetracycline removal efficiency can reach over 72% after 2h of visible light photocatalytic degradation. Illustrating the BiVO formed4/Bi25VO40The heterojunction is beneficial to the effective separation and conduction of electron-hole pairs, and shows higher photocatalytic activity.
From the above embodiments, the invention provides a bismuth vanadate heterojunction BiVO4/Bi25VO40The preparation method adopts two-step synthesis of hydrothermal reaction-alkali treatment, does not need a template, has mild conditions, does not need high temperature and high pressure, is simple and easy to operate, and has high efficiency. In addition, BiVO is formed4/Bi25VO40The heterojunction is beneficial to the effective separation and conduction of electron-hole pairs, and the obtained material has excellent photocatalytic performance and can be applied to photocatalytic reaction.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Bismuth vanadate heterojunction BiVO4/Bi25VO40The preparation method of the material is characterized by comprising the following steps:
(1) dissolving a vanadium source and a bismuth source in an acidic solution, adding an alkaline solution, and carrying out a precipitation reaction;
(2) carrying out hydrothermal reaction on a system obtained by the precipitation reaction, and separating to obtain a solid product;
(3) dispersing the solid product in an alkaline solution, carrying out alkali treatment, and separating to obtain bismuth vanadate heterojunction BiVO4/Bi25VO40A material.
2. The production method according to claim 1, wherein, in the step (1),
the bismuth source is one or more of bismuth chloride, bismuth nitrate, bismuth sulfate, bismuth trioxide and bismuth hydroxide;
the vanadium source is one or more of vanadium trichloride, ammonium vanadate, sodium vanadate, ammonium metavanadate and sodium metavanadate;
the mass ratio of bismuth ions in the bismuth source to vanadium ions in the vanadium source is (0.1-10): 1.
3. the production method according to claim 1, wherein, in the step (1),
the concentration of the acidic solution and the concentration of the alkaline solution are 0.1-5 mol/L independently;
the solvent of the acidic solution and the solvent of the alkaline solution are one or more of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide independently;
the solute of the acid solution is one or more of hydrochloric acid, nitric acid, sulfuric acid and acetic acid;
the solute of the alkaline solution is one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide.
4. The preparation method according to claim 1, wherein in the step (1), the temperature of the precipitation reaction is room temperature, and the time is 0.5-10 h.
5. The preparation method according to claim 1, wherein in the step (2), the temperature of the hydrothermal reaction is 100 to 250 ℃ and the time is 1 to 24 hours.
6. The preparation method according to claim 1, wherein in the step (3), the temperature of the alkali treatment is 25-150 ℃ and the holding time is 0.3-12 h.
7. The production method according to claim 1 or 6, wherein, in the step (3),
the solvent of the alkaline solution is one or more of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the solute is one or more of ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, sodium peroxide, potassium oxide and potassium peroxide; the concentration of the alkaline solution is 0.1-5 mol/L.
8. The preparation method according to claim 1, wherein in steps (2) and (3), after separation, the obtained solid is washed and dried; the washing detergent is two or three of water, ethanol, diethyl ether, acetone and N, N-dimethylformamide; the drying temperature is 40-100 ℃, and the heat preservation time is 6-24 h.
9. Bismuth vanadate heterojunction BiVO prepared by the preparation method of any one of claims 1 to 84/Bi25VO40A material.
10. Bismuth vanadate heterojunction BiVO according to claim 94/Bi25VO40The material is used as a photocatalyst in the application of photocatalytic degradation of organic pollutants.
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