CN111330567A - One-step solvothermal method for preparing rose-structured Bi2O3/BiVO4/GO nano composite photocatalytic material and application thereof - Google Patents
One-step solvothermal method for preparing rose-structured Bi2O3/BiVO4/GO nano composite photocatalytic material and application thereof Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 74
- 239000000463 material Substances 0.000 title claims abstract description 65
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 40
- 238000004729 solvothermal method Methods 0.000 title claims abstract description 35
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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- 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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/10—Photocatalysts
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Abstract
One-step solvothermal method for preparing rose-structured Bi2O3/BiVO4The GO nano composite photocatalytic material comprises the following components in percentage by weight: a certain molar amount of Bi (NO)3)3·5H2Dissolving O in glycerol; a certain molar weight of NaVO3·2H2Dissolving O in deionized water; mixing the above solutions; adding a certain mass fraction of Graphene Oxide (GO), and mixing the mixed solutionTransferring the mixture into an autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 8 hours; centrifugally separating, washing and drying to obtain Bi with rose structure2O3/BiVO4A GO nano composite photocatalytic material. The invention adopts a one-step solvothermal method, has simple and convenient preparation method, has the advantages of wide photoresponse range, narrow forbidden bandwidth and strong catalytic capability, has low cost, and effectively solves the problem of the existing BiVO4The problems that the electronic hole of the photocatalyst is difficult to separate and the photoresponse range is limited are solved, the preparation of a novel clean photocatalytic material is facilitated, and the sustainable development of resources is realized.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, and particularly relates to a method for preparing rose structure Bi by a one-step solvothermal method2O3/BiVO4A GO nano composite photocatalytic material and application thereof.
Background
Due to the shortage of energy and the increasing prominence of environmental problems, solar energy is widely used as an environment-friendly renewable energy source by researchers at home and abroadAttention is paid. Conventional photocatalyst TiO2Has high photocatalytic activity and stability, but the high band gap (3.2eV) enables the photocatalyst to be activated only by ultraviolet rays, and the development of the photocatalyst with visible light response is required. As TiO2Bismuth vanadate (BiVO) as ideal substitute4) The forbidden band width is narrow (2.4eV), but the recombination rate of photo-generated electrons and holes is high, so that the photodegradation efficiency is limited. Therefore, the problem of recombination of photogenerated electrons and holes is reduced, and BiVO is improved4The activity and efficiency of the visible light photocatalytic reaction have important significance in decomposing organic pollutants.
One of the means for improving the catalytic activity of the photocatalytic material is to increase the specific surface area of the material, so that research is carried out to prepare three-dimensional BiVO with one-dimensional materials, nano-sheet two-dimensional materials, hollow microsphere structures, layered structures or olive structures, wherein the one-dimensional materials, the nano-sheet two-dimensional materials, the hollow microsphere structures, the nano-sheet two-dimensional materials, the nano4Photocatalytic material and the like to effectively promote BiVO4And (4) photodegradability.
The performance and application of a single semiconductor material generally have great limitations and cannot meet various requirements of actual production. By recombination with other semiconductors, e.g. V2O5/BiVO4、Cu/BiVO4、CeO2/BiVO4The narrow bandgap material can sensitize the wide bandgap semiconductor to widen the photoresponse range; meanwhile, a built-in electric field is formed in the material after the semiconductor is compounded, so that the separation of a photon-generated carrier can be promoted, the photochemical performance of the compounded material is stable, and the photocatalytic effect can be obviously improved.
The carbon material has attracted extensive attention in the preparation of photocatalytic materials due to its large specific surface area, high chemical stability and excellent electrical conductivity. The photocatalyst of the loaded carbon material has stronger adsorption capacity, and simultaneously inhibits the recombination of photon-generated carriers, so that the catalytic capacity of the photocatalytic material is greatly improved; and the carbon material has better electronic conductivity, BiVO4The photo-generated electrons generated by the matrix can be rapidly transferred to the surface of the carbon material, so that the separation of the photo-generated electrons and the holes is promoted, and the capability of the photocatalytic material for producing hydrogen and oxygen by photolysis of water is improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing rose-structured Bi by a one-step solvothermal method2O3/BiVO4The one-step solvothermal method is simple to prepare and convenient to operate, and the Bi is constructed2O3/BiVO4the/GO composite structure provides more active sites, widens the photoresponse range, and can also promote the separation of photo-generated electron holes, greatly reduces the recombination rate and obviously improves the photocatalytic performance.
In order to achieve the purpose, the invention adopts the technical scheme that:
one-step solvothermal method for preparing rose-structured Bi2O3/BiVO4The method for preparing the/GO nano composite photocatalytic material comprises the following steps:
the method comprises the following steps:
a certain molar amount of Bi (NO)3)3·5 H2Dissolving O in glycerol to obtain a precursor solution A;
step two:
a certain molar weight of NaVO3·2 H2Dissolving O in deionized water to obtain a precursor solution B;
step three:
adding the solution A into the solution B and stirring vigorously to obtain a solution C;
step four:
adding a certain amount of Graphene Oxide (GO) into the solution C and stirring to obtain a solution D;
step five:
transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 8 hours to obtain a synthetic product E;
step six:
centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
step seven:
transferring the dried product F into a muffle furnace, calcining for 5 h at 300 ℃ in the air, and naturally cooling to room temperature to obtain the roseBi of rose structure2O3/BiVO4A GO nano composite photocatalytic material.
In the first step and the second step, Bi (NO)3)3·5 H2O and NaVO3·2 H2The molar ratio of O is 1: 1-5: 1.
And in the fourth step, the mass fraction range of the Graphene Oxide (GO) is 1-20%.
The temperature range of the solvent heat in the step five is 90-220 ℃.
And in the fifth step, the solvothermal reaction time is 3-24 hours.
And the calcining temperature range of the muffle furnace in the step seven is 300-550 ℃.
And in the seventh step, the calcining time of the muffle furnace is 2-10 h.
One-step solvothermal method for preparing rose-structured Bi2O3/BiVO4the/GO nano composite 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, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
The invention has the beneficial effects that:
preparing rose-structured Bi by adopting one-step solvothermal method2O3/BiVO4The preparation method of the/GO nano composite photocatalytic material is simple and convenient to operate. Bi in the composite material2O3And BiVO4A heterojunction is formed, a synergistic effect exists, and electron-hole pairs can be effectively separated; GO has the characteristics of large specific surface area and strong interlayer ion exchange capacity, and is compounded with GO to form a GO layer wrapped by Bi2O3/BiVO4The structure and the specific surface area of the material are increased, a large number of active sites are provided for the photocatalytic reaction, phase mass transfer and electron transfer are facilitated, photoproduction electrons can be rapidly captured and transferred, the recombination of the photoproduction electrons and holes is effectively prevented, and the BiVO is remarkably improved4The separation efficiency and electron mobility of the photon-generated carriers promote the catalytic reaction. The material has the advantages of low electron-hole recombination rate, small forbidden band width, wide spectral response range and high photocatalytic activity when being used as a photocatalytic material.
Drawings
FIG. 1 shows a one-step solvothermal method for preparing rose-structured Bi2O3/BiVO4SEM image of/GO nano composite photocatalytic material.
FIG. 2 shows a one-step solvothermal method for preparing rose-structured Bi2O3/BiVO4XRD images of the/GO nano composite 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 2
(1) 1.2 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 3
(1) 2.0 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 10% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 5
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml glycerol to obtain precursorA bulk solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 15% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 20% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 7
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 1% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 90 ℃ for 15 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained one-step solventThermal method for preparing Bi with rose structure2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 90 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 150 ℃ for 24 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to 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;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 220 ℃ for 3 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 12
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 15 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 13
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 400 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 14
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 5 hours at 550 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 15
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 1 h at 550 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 16
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 100 h in air at 300 ℃, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Example 17
(1) 0.4 mmol of Bi (NO)3)3·5 H2Dissolving O in 16 ml of glycerol to obtain a precursor solution A;
(2) adding 0.4 mmol of NaVO3·2 H2Dissolving O in 16 ml of deionized water to obtain a precursor solution B;
(3) adding the solution A into the solution B and stirring vigorously to obtain a solution C;
(4) adding Graphene Oxide (GO) with the mass fraction of 5% into the solution C and stirring to obtain a solution D;
(5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 180 ℃ for 9 hours to obtain a synthetic product E;
(6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
(7) transferring the dried product F into a muffle furnace, calcining for 1 h at 300 ℃ in the air, and naturally cooling to room temperature to obtain a target product;
the obtained Bi with rose structure is prepared by one-step solvothermal method2O3/BiVO4The method for testing the photocatalytic performance of the/GO nano composite photocatalytic material comprises the following steps:
the light source was a 300W Xe lamp to simulate sunlight. 50 ml of rhodamine B solution is measured, 20 ml of catalyst is added, and ultrasonic dispersion is carried out. Before illumination, the catalyst and the pollutants are adsorbed and stirred for 30 min in the dark to reach adsorption equilibrium. After turning on the lamp, 4 mL samples were taken from the reaction vessel at regular 20 min intervals. Separating the photocatalyst from the solution by using a 10000 r/min high-speed centrifuge for the sample taken out each time, taking the supernatant, measuring the absorbance of Rh B by using an ultraviolet-visible spectrophotometer, and judging the degradation efficiency of the catalyst to the pollutant solution according to the absorbance.
Referring to FIG. 1, FIG. 1 shows the rose structure Bi obtained in example 12O3/BiVO4SEM image of/GO nano composite photocatalytic material. Bi is clearly observed from the figure2O3In-situ growth on BiVO through solvothermal reaction4Surface of Bi form2O3/BiVO4Microspheres, layered GO tightly wrapped in Bi2O3/BiVO4The surfaces of the microspheres are tightly combined by Van der Waals acting force to form rosette Bi2O3/BiVO4A GO nano composite photocatalytic material.
Referring to FIG. 2, FIG. 2 shows the rose structure Bi obtained in example 12O3/BiVO4XRD images of the/GO nano composite photocatalytic material. It is evident from the figure that without GO, Bi (NO) is present3)3·5 H2O and NaVO3·2 H2O generates monoclinic phase BiVO through solvothermal reaction4When the addition amount of GO is 5%, Bi is generated in the reaction process due to the oxidation capability of GO2O3And BiVO4. From the results in the figure, it is evident that Bi is present in the sample2O3And BiVO4Characteristic peak of (A), indicating successful formation of Bi under the oxidation of GO2O3/BiVO4。
The above examples show that the rose-structured Bi prepared by the one-step solvothermal method provided by the invention2O3/BiVO4The preparation method of the/GO nano composite photocatalytic material is simple and easy to operate, and the prepared Bi with the rose structure is prepared by a one-step solvothermal method2O3/BiVO4the/GO nano composite photocatalytic material has the advantages of remarkably reduced recombination rate of photo-generated electrons and holes and enhanced light absorption capacity, has the advantages of high catalytic activity, high degradation rate and strong hydrolytic capability as a photocatalytic material, remarkably improves the photocatalytic performance of a bismuth-based material, and aims to solve the problem of carrier recombination and efficiently prepare BiVO4Provides a new idea.
The invention is based on morphology regulation, semiconductor compounding and the likeStarting from the aspect and solving the BiVO4The bandgap problem and the carrier recombination problem provide new ideas. Preparing the rose structure Bi by controlling the appearance2O3/BiVO4/GO nano composite material and BiVO prepared from same4The surface is rough and porous, so that the composite material is beneficial to adsorbing more electrons to carry out redox reaction, the specific surface area of the rose structure composite material is increased, a large number of active sites are provided for photocatalytic reaction, phase mass transfer and electron transmission are facilitated, and the recombination of photoproduction electrons and holes is effectively prevented; for compounding of the carbon material, the sample is compounded with GO, so that separation of photo-generated electrons and holes is promoted, and the photocatalytic performance is improved. By utilizing the characteristics of large specific surface area and strong interlayer ion exchange capacity of GO and being capable of rapidly capturing and transferring photo-generated electrons, BiVO is remarkably improved4The separation efficiency and electron mobility of the photon-generated carriers promote the catalytic reaction. The GO-loaded photocatalyst has stronger adsorption capacity, and simultaneously inhibits the recombination of photon-generated carriers, so that the catalytic capacity of the photocatalytic material is greatly improved; and GO has better electronic conductivity, BiVO4The photo-generated electrons generated by the substrate can be rapidly transferred to the GO surface, so that the separation of the photo-generated electrons and holes is promoted, and the capability of producing hydrogen and oxygen by photolysis of water of the photocatalytic material is improved. Preparation of rose-structured Bi2O3/BiVO4the/GO nano composite photocatalytic material solves the problem of BiVO4The electron-hole of the base photocatalytic material is easy to recombine, the carrier separation rate is low, and an effective method and a reliable way for realizing sustainable development are provided.
Claims (9)
1. Rose structure Bi prepared by one-step solvothermal method2O3/BiVO4the/GO nano composite photocatalytic material is characterized in that Bi is prepared in situ2O3/BiVO4And heterojunction, and the heterojunction and graphene oxide GO are compounded to form a rosette nano composite structure.
2. The material of claim 1, wherein the material has a rosette-like structure on a nanometer scale.
3. Rose structure Bi2O3/BiVO4The preparation method of the/GO nano composite photocatalytic material is characterized by comprising the following steps:
will be dispersed with Bi (NO)3)3·5 H2O、NaVO3·2 H2O, GO, and calcining the dispersion in a muffle furnace to obtain Bi with a rose structure2O3/BiVO4A GO nano composite photocatalytic material.
4. The method according to claim 3, wherein Bi (NO) is dispersed3)3·5 H2O、NaVO3·2 H2O, GO is obtained by a process comprising the steps of:
adding Bi (NO)3)3·5 H2Glycerol solution of O, and NaVO3·2 H2Mixing the water solution of O according to the molar ratio of the solute (1-5) to 1; adding GO into the mixed solution and uniformly dispersing.
5. The method of claim 3, wherein the mass fraction of GO after addition to the dispersion is in the range of 1% to 20%.
6. The method according to claim 3, wherein the solvothermal reaction temperature is 90-220 ℃ and the reaction time is 3-24 h.
7. The method according to claim 3, wherein the muffle furnace calcination temperature is 300-550 ℃, and the reaction time is 1-10 h.
8. The method according to any one of claims 3 to 7, characterized by comprising the specific steps of:
1) adding Bi (NO)3)3·5 H2Dissolving O in glycerol to obtain a precursor solution A;
2) NaVO (sodium VO)3·2 H2Dissolving O in deionized water to obtainTo a precursor solution B;
3) adding the solution A into the solution B and stirring vigorously to obtain a solution C; adding the solution A into the solution B and stirring vigorously to obtain a solution C; bi (NO)3)3·5 H2O and NaVO3·2 H2The molar ratio of O is 1: 1-5: 1;
4) adding GO into the solution C and stirring to obtain a solution D; the mass fraction range of GO is 1% -20%;
5) transferring the solution D into a high-pressure autoclave with a polytetrafluoroethylene lining, and keeping the temperature at 90-220 ℃ for 3-24 h to obtain a synthetic product E;
6) centrifuging and separating the solvent thermal synthesis product E at 10000 rpm, washing with deionized water and ethanol, and drying at 60 ℃ for 4 hours to obtain a product F;
7) transferring the dried product F into a muffle furnace, calcining for 1-10 h at 300-550 ℃ in air, and naturally cooling to room temperature to obtain Bi with a rose structure2O3/BiVO4A GO nano composite photocatalytic material.
9. Use of the material according to claim 1 or 2 for photocatalytic degradation of organic pollutants or photocatalytic oxygen production.
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Application publication date: 20200626 |