CN111330568A - BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4Flexible easily-recycled photocatalytic material, preparation method and application thereof - Google Patents
BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4Flexible easily-recycled photocatalytic material, preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 77
- 239000004744 fabric Substances 0.000 title claims abstract description 70
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 54
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 50
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims description 5
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 238000007146 photocatalysis Methods 0.000 claims abstract description 19
- 229910019501 NaVO3 Inorganic materials 0.000 claims abstract description 17
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000004729 solvothermal method Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 239000003344 environmental pollutant Substances 0.000 claims description 27
- 231100000719 pollutant Toxicity 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 26
- 239000002243 precursor Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 14
- -1 polytetrafluoroethylene Polymers 0.000 claims description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000003786 synthesis reaction Methods 0.000 claims description 13
- 229910001868 water Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 97
- 239000003054 catalyst Substances 0.000 description 40
- 238000002835 absorbance Methods 0.000 description 24
- 230000015556 catabolic process Effects 0.000 description 16
- 238000006731 degradation reaction Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000005286 illumination Methods 0.000 description 12
- 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 12
- 229940043267 rhodamine b Drugs 0.000 description 12
- 238000001179 sorption measurement Methods 0.000 description 12
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 238000000926 separation method Methods 0.000 description 7
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 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 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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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
-
- B01J35/40—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4Flexible easily-recycled photocatalytic material: with Bi (NO)3)3·5 H2O and NaVO3·2 H2O is taken as a raw material, carbon cloth with a certain size is added, and the mixture undergoes a solvothermal reaction at 180 ℃ for 8 hours to obtain carbon cloth-loaded BiVO4Powder of at Ar/H2Annealing for 10 h at 350 ℃ in the atmosphere, and reducing the alloy in situ into BiVO modified by Bi loaded with non-noble metal on carbon cloth4The photocatalysis material is flexible and easy to recycle. The invention takes the carbon cloth as the substrate and shows excellent performanceDifferent conductivity, flexibility, bendability, high carrier diffusion rate, wide photoresponse range, recyclability and low cost, and utilizes SPR effect of non-noble metal Bi and BiVO4Improving BiVO by synergistic effect of4The defect that the photoproduction electrons and the holes are easy to compound is overcome, the problem that the powder photocatalyst is difficult to recover can be effectively solved, and the sustainable development of resources is realized.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a BiVO modified by Bi for preparing carbon cloth supported in-situ growth non-noble metal4A method for flexible easy-recycling photocatalytic material and application thereof.
Background
Semiconductor photocatalysis is a high-efficiency utilization technology of clean energy, has application in the aspects of hydrogen production by photolysis of water, carbon dioxide conversion, air purification, water degradation treatment and the like, and is expected to solve the problems of energy shortage and environmental pollution in the world. Because of the rich bismuth yield in China, the bismuth group photocatalyst has higher photocatalytic efficiency, so the method causesHas attracted extensive attention from researchers. Bismuth vanadate (BiVO)4) The forbidden band width of the material is 2.3-2.4eV, the material can decompose water and degrade pollutants under visible light, and the material has the characteristics of wide photoresponse range, low carbon, environmental protection and no toxicity. However, the photodegradation efficiency is limited because the photo-generated electrons and holes are easily recombined and the quantum efficiency is low. Accordingly, BiVO with high photogenerated carrier separation efficiency, wide range of visible light response and low cost is developed4Matrix composites remain of great interest and challenge.
The performance and application of a single semiconductor material generally have great limitations and cannot meet various requirements of actual production. By loading metals or metal oxides, e.g. V, on their surfaces2O5/BiVO4、Cu/BiVO4、CeO2/BiVO4And the like, a built-in electric field is formed in the material to promote the separation of photon-generated carriers, thereby improving the photocatalytic activity.
Recently, noble metal photocatalysts have become the focus of current research, such as Au/TiO2、TiO2/Ag-Ag2S and the like, the plasma resonance (SPR) effect of the noble metal is utilized, the carrier transmission rate of the noble metal can be improved, the photon-generated electron-hole recombination is inhibited, and the purpose of better conversion from light energy to chemical energy is achieved.
Although these measures are effective in improving photocatalytic activity, noble metals are a major factor limiting the development thereof due to their high cost. Meanwhile, the nano composite powder is difficult to recover in the application process of photocatalytic water treatment, which causes secondary pollution and limits the practical application of the nano composite powder. Therefore, how to ensure the stability of the photocatalyst, reduce the cost of the catalyst, and reduce the difficulty in recovery is a problem to be solved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing carbon cloth loaded in-situ growth non-noble metal Bi modified BiVO4Method for preparing flexible easily-recycled photocatalytic material and application thereof, and carbon cloth loaded Bi/BiVO4The photocatalytic material uses simple and easily available carbon cloth as a substrate, shows excellent conductivity, flexibility and bendability, and can be bent for a long timeThe material can be folded or repeatedly bent without worrying about material damage, can be cut according to different use environments, has the advantages of high carrier diffusion rate, wide photoresponse range, recyclability, good cycle performance and low cost, and utilizes the SPR effect of non-noble metal Bi and BiVO4Improving BiVO by synergistic effect of4The method has the advantages of wide photoresponse range, recyclability, good cycle performance and low cost, and can realize sustainable development and cyclic utilization of resources.
In order to achieve the purpose, the invention adopts the technical scheme that:
BiVO modified by Bi for preparing carbon cloth loaded in-situ growth non-noble metal4A method for flexible easy recovery of photocatalytic material, comprising the steps of: a certain molar amount of Bi (NO)3)3·5 H2Dissolving O in glycerol; a certain molar weight of NaVO3·2 H2Dissolving O in deionized water; mixing the solution, transferring the mixed solution into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size, and keeping the temperature at 180 ℃ for 8 hours; washing with water and alcohol, and drying at 60 ℃ for 4 h to obtain carbon cloth loaded BiVO4And (3) powder. At Ar/H2Annealing for 10 h at 350 ℃ in the atmosphere, and reducing the alloy in situ into carbon cloth loaded Bi/BiVO4Obtaining carbon cloth loaded in-situ growth non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
The method comprises the following steps:
0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
step two:
adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
step three:
washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
step four:
product E at Ar/H2Annealing at 350 ℃ for 10 h in the atmosphere of (95%:5%) to obtain carbon cloth-supported in-situ-grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
And in the second step, the temperature range of the solvent is 120-200 ℃.
And in the second step, the solvothermal reaction time is 6-12 h.
Ar/H in the fourth step2The proportion range is 95%:5% -70%: 30 percent.
The annealing temperature range in the fourth step is 300-400 ℃.
The annealing time range in the fourth step is 5-12 h.
BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4The flexible easily-recycled photocatalytic material is applied to photocatalytic technologies, such as pollutant degradation, photolysis water and the like. A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
The invention has the beneficial effects that:
the invention takes the carbon cloth as the substrate, has excellent conductivity, accelerates the carrier transmission, is beneficial to improving the carrier separation efficiency and can improve BiVO4The photo-generated electrons and the holes are easy to recombine, and the photo-generated electrons and the holes also have flexibility and bendability, do not need to worry about material damage even if being folded for a long time or repeatedly bent, and have the advantages of high charge separation rate, wide light absorption range, high photocatalytic activity, high degradation rate and strong hydrolysis capacity.
In addition, in practical application, the problem of recovering and reusing the photocatalyst must be solved, so the photocatalyst should be fixed on some substrates, and the carbon cloth is used as the substrate to facilitate the recovery of the photocatalyst, thereby solving the current situation that the powdery catalyst is difficult to recover.
The noble metal nanoparticles can effectively transfer electrons and inhibit the recombination of photogenerated electrons and holes, and meanwhile, the Surface Plasmon Resonance (SPR) effect of the noble metal nanoparticles is beneficial to absorbing visible light, so that the photocatalysis effect is obviously improved. The non-noble metal Bi has the similar properties with noble metals, becomes an effective substitute of noble metals, and reduces the use cost. By using SPR effect of non-noble metal Bi and BiVO4The synergistic effect can effectively improve BiVO4Carrier separation rate, expanded photoresponse range and enhanced photocatalytic activity.
Drawings
FIG. 1 shows BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4SEM image of flexible easily-recycled photocatalytic material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 10 h in 95%:5% atmosphere to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 2
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 120 ℃ for 12 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 10 h in 95%:5% atmosphere to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 3
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 160 ℃ for 10 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 10 h in 95%:5% atmosphere to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 4
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 200 ℃ for 6 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 10 h in 95%:5% atmosphere to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 5
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2(85%:15%) annealing at 350 deg.C for 10 h to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 6
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing for 10 h at 350 ℃ in the atmosphere of (70%:30%) to obtain carbon cloth-supported in-situ-grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 7
(1) Adding 0.4 mmol of Bi(NO3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 300 ℃ for 10 h in the atmosphere of (95%:5%) to obtain carbon cloth-supported in-situ grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 8
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 400 ℃ for 10 h in the atmosphere of (95%:5%) to obtain carbon cloth-supported in-situ grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 9
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing for 5h at 350 ℃ in the atmosphere of (95%:5%) to obtain carbon cloth-supported in-situ grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 10
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 8 h in 95%:5% atmosphere to obtain carbon cloth supported in-situ grown non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Example 11
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
(3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
(4) product E at Ar/H2Annealing at 350 deg.C for 12h in 95%:5%) atmosphere to obtain carbon cloth-supported in-situ grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
BiVO modified by Bi of non-noble metal supported by obtained carbon cloth and grown in situ4The method for testing the photocatalytic performance of the flexible easily-recycled photocatalytic material comprises the following steps:
A300W Xe lamp was used as a light source, and a cut-off filter with a wavelength of less than 800 nm was used to simulate sunlight. 50 ml of rhodamine B (Rh B) solution is measured and added with the catalyst. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30min in the dark to reach adsorption equilibrium. After turning on the lamp, taking 4 mL samples from the reaction vessel every 20 min, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst on the pollutant solution according to the absorbance.
Referring to FIG. 1, FIG. 1 shows BiVO modified by carbon cloth loaded in-situ growth non-noble metal Bi4SEM picture of flexible easily-recycled photocatalytic material, i.e. sample made in example 1. The in-situ growth and modification of Bi in BiVO can be obviously observed from the figure4The particle size of the surface is about 500-600 nm, and the surface is uniformly attached to the surface of the carbon cloth, thereby being beneficial to improving the photocatalytic performance.
The above embodiment shows that the BiVO modified by the non-noble metal Bi loaded and grown in situ for preparing the carbon cloth provided by the invention4The preparation method of the flexible easily-recycled photocatalytic material is simple in steps, and the prepared carbon cloth loaded in-situ grown non-noble metal Bi modified BiVO4The flexible easily-recycled photocatalytic material has enlarged photoresponse range and improved carrier separation rate and can be used as lightThe catalytic material has the advantages of high catalytic activity, high degradation rate and strong hydrolysis capability, and provides a new idea for efficient utilization of solar energy.
Bi/BiVO loaded by taking carbon cloth as substrate4To solve BiVO4The bandgap problem and the carrier recombination problem provide opportunities, spherical BiVO4Is beneficial to adsorbing more electrons to carry out redox reaction, and Bi grows in situ and is modified in BiVO4On the surface, charge is effectively separated by utilizing the SPR effect of Bi having noble-like metals. In addition, Bi and BiVO are utilized4The synergistic effect of the two components promotes the charge separation efficiency and enhances the light absorption range. The carbon cloth is used as a substrate, the carbon cloth has excellent conductivity, flexibility and bendability, is cheap and easy to obtain, has a simple preparation method, can be cut at will according to actual use conditions, is convenient for recycling of the photocatalyst, and solves the problem that the existing powdery catalyst is difficult to recycle. BiVO modified by Bi for preparing carbon cloth supported in-situ growth non-noble metal4The flexible easily-recycled photocatalytic material is an effective method and a reliable way for solving the problems that an electron-hole of the photocatalytic material is easy to compound, a powdered catalyst is difficult to recycle and sustainable development is realized.
Claims (6)
1. Carbon cloth loaded in-situ growth non-noble metal Bi modified BiVO4The preparation method of the flexible easily-recycled photocatalytic material is characterized by comprising the following steps of:
with Bi (NO)3)3·5 H2O and NaVO3·2 H2Adding carbon cloth with a certain size into O serving as a raw material, and carrying out solvothermal reaction for a certain time to obtain carbon cloth loaded BiVO4Powder; at Ar/H2Annealing for a certain time at a certain temperature in the atmosphere to obtain the carbon cloth-loaded in-situ-grown non-noble metal Bi-modified BiVO4The photocatalysis material is flexible and easy to recycle.
2. The method of claim 1, wherein the carbon cloth supports BiVO4The powder is obtained by a process comprising the steps of: adding a certain size of carbon cloth with Bi (NO) dispersed therein3)3And NaVO3At 120, inCarrying out solvothermal reaction at the temperature of 200 ℃ to obtain the carbon cloth loaded BiVO for 6-12 h4And (3) powder.
3. The method of claim 1, wherein the carbon cloth supports Bi/BiVO4The powder is obtained by a process comprising the steps of: loading carbon cloth with BiVO4Powder in Ar/H2Annealing for 5 to 12 hours at the temperature of between 300 and 400 ℃ in the atmosphere to obtain the carbon cloth loaded Bi/BiVO4。
4. The method of claim 1, comprising the steps of:
1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A; adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
2) adding the solution A into the solution B and stirring vigorously to obtain a solution C; transferring the solution C into a high-pressure autoclave with a polytetrafluoroethylene lining, adding carbon cloth with a certain size as a flexible substrate, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product D;
3) washing the solvent thermal synthesis product D with deionized water and ethanol, and drying at 60 ℃ for 4 h to obtain a product E;
4) the product E is Ar/H with the proportion ranging from (95-70)% to (5-30)%2Annealing for 5-12 h at the temperature of 300-400 ℃ in the atmosphere to obtain carbon cloth-loaded in-situ growth non-noble metal Bi modified BiVO4The photocatalysis material is flexible and easy to recycle.
5. BiVO modified by carbon cloth supported in-situ growth non-noble metal Bi obtained by the method of any one of claims 1 to 44The photocatalysis material is flexible and easy to recycle.
6. Use of the material of claim 5 for photocatalytic degradation of pollutants or photocatalytic oxygen production.
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