CN114405497A - Three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst and preparation method and application thereof - Google Patents
Three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst and preparation method and application thereof Download PDFInfo
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 7
- 229910052724 xenon Inorganic materials 0.000 claims description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
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- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 3
- 230000031700 light absorption Effects 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000003426 co-catalyst Substances 0.000 abstract description 2
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- 229940010552 ammonium molybdate Drugs 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
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Classifications
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- B01J35/50—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
Abstract
The invention discloses a three-dimensional flower-shaped Bi @ Sn3O4A Schottky junction visible light catalyst and a preparation method and application thereof belong to the technical field of catalysis. The preparation method comprises the following steps: three-dimensional flower-shaped Sn3O4Uniformly dispersing in an ethanol solution by ultrasonic, adding Bi nanospheres, magnetically stirring for 2 hours at room temperature, evaporating the solvent to dryness, cooling to room temperature, and collecting a sample to obtain a target product Bi @ Sn3O4. The invention provides three-dimensional flower-shaped Bi @ Sn3O4Catalytic synthesis of H within 150min without any carbon emissions or pollutants and any co-catalyst involvement2O2The yield reaches 112 mu mol/L. The method has the characteristics of simplicity, convenience, high efficiency, low cost and high visible light absorption degree, and can be applied to the fields of photocatalytic preparation of hydrogen peroxide, degradation of organic matters and the like.
Description
Technical Field
The invention relates to a three-dimensional flower-shaped Bi @ Sn with visible light response3O4Schottky junction visible light catalyst and method for preparing H through photocatalysis2O2The application of the aspect is mainly aimed at industrial large-scale production of H2O2Belonging to the field of high value-added chemical production.
Background
Hydrogen peroxide (H)2O2) Is a clean multifunctional oxidant, and the by-product is only water. It has been widely used in the chemical industry and environmental management fields such as pulp bleaching, organic synthesis, disinfection and water remediation. Recently, H2O2As alternative H2Also of great interest is the ideal fuel cell energy carrier. This is due to H2O2Has water solubility, and thus can be compared with H2More convenient and safe storage and transportation. However, the anthraquinone process as H2O2The most common methods of production are limited by their complex route, high cost and toxic by-products. In addition, by means of noble metal catalysts in H2And O2Synthesis of H in the Presence of2O2There is a potential explosive problem. Therefore, there is an urgent need to develop a method for producing H2O2The technology is safe, efficient, environment-friendly and low in cost. Photocatalytic H2O2The production method has wide prospect and can reduce O at ambient temperature and pressure2Without the need for expensive Pd catalysts or high pressure H2. Most importantly, this method does not utilize or generate any harmful chemicals or carbon dioxide.
Sn3O4As a thermodynamically stable intermediate composition with a band gap in the visible range (about 2.65eV), it has been reported as a potential optical drive photocatalyst. Has the characteristics of inherent visible light absorption, good band edge positions, oxygen-rich vacancies, low electrical resistance, non-toxicity and good photochemical stability in acidic/basic media. However, pure Sn3O4Has a limited visible light absorption range of (<550nm), high recombination rate of photogenerated electron and hole pairs, and poor stability, limit its applications. In order to improve the aspect of photocatalytic performance, designing and constructing a good valence band matching photocatalytic heterostructure is a very effective strategy.
Disclosure of Invention
One of the purposes of the invention is to provide a three-dimensional flower-shaped Bi @ Sn with visible light response and improved photogenerated electrons and photogenerated holes3O4A Schottky junction catalyst and a preparation method thereof.
The second purpose of the invention is to provide a method for utilizing three-dimensional flower-shaped Bi @ Sn3O4H prepared by Schottky junction catalyst photocatalysis2O2The method of (1).
In order to achieve the purpose, the invention adopts the technical scheme that: three-dimensional flower-shaped Bi @ Sn3O4The preparation method of the Schottky junction visible light catalyst comprises the following steps: three-dimensional flower-shaped Sn3O4Uniformly dispersing in an ethanol solution by ultrasonic, adding Bi nanospheres, magnetically stirring for 2 hours at room temperature, evaporating the solvent to dryness, cooling to room temperature, and collecting a sample to obtain a target product Bi @ Sn3O4。
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst, Sn in mass ratio3O4:Bi＝20:1。
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst, the Sn3O4The preparation method comprises the following steps: SnCl2·2H2Adding O and trisodium citrate dihydrate into deionized water, stirring until the O and the trisodium citrate dihydrate are completely dissolved, then slowly adding NaOH solution, carrying out hydrothermal reaction on the obtained mixture at 180 ℃ for 12h after stirring, cooling to room temperature after reaction, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain Sn3O4。
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst, SnCl in molar ratio2·2H2Trisodium citrate dihydrate 2: 5.
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4The concentration of the NaOH solution is 0.2 mol/L.
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4The preparation method of the Schottky junction visible light catalyst and the Bi nanosphere comprises the following steps: adding Bi (NO)3)3·5H2Dissolving O in HNO3And adding polyvinylpyrrolidone (PVP) into the solution, stirring until the PVP is dissolved, carrying out hydrothermal reaction on the obtained mixture at 160 ℃ for 12 hours, cooling to room temperature, washing with deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain the Bi nanosphere.
Preferably, the three-dimensional flower-shaped Bi @ Sn3O4Schottky junction visible light catalyst, Bi (NO) according to mass ratio3)3·5H2O:PVP＝91:150。
The invention provides three-dimensional flower-shaped Bi @ Sn3O4The application of the Schottky junction visible light catalyst in preparing hydrogen peroxide by photocatalysis.
Preferably, the method is as follows: three-dimensional flower-shaped Bi @ Sn3O4Adding Schottky junction visible light catalyst into deionized water and ethanol, performing ultrasonic treatment for 10min, adjusting pH to 3, and adding O2The suspension was passed through a magnetic stirrer and magnetically stirred in the dark for 30min, and then the reaction was carried out by irradiation with a light source.
Preferably, the light source adopts a 300W xenon lamp as the light source, and the lambda of the xenon lamp is more than or equal to 420 nm.
The invention has the beneficial effects that:
1. the invention passes through three-dimensional flower-shaped Sn3O4And the Bi nanospheres are compounded, so that the photoresponse range and the photocatalytic performance are further improved, the efficiency of capturing photons is improved, the recombination of electron hole pairs is inhibited, the utilization rate of transition of electrons from a valence band to a conduction band is improved, and the photocatalytic activity is improved.
2. With the process of the present invention, there is a high hydrogen peroxide (H) without any carbon emissions or pollutants and any co-catalyst involved2O2) Yield, within 150min, H2O2The yield reaches 112 mu mol/L, and the method is suitable for productionH2O2Provides a green synthetic route and sustainable technology.
3. The invention has the characteristics of simplicity, convenience, high efficiency, low cost and high visible light absorption, and the prepared three-dimensional flower-shaped Bi @ Sn3O4The Schottky junction visible light catalytic material has the characteristics of narrow band gap, large specific surface area and high catalytic activity, has good visible light absorption performance and stability, high photoinduced charge transfer efficiency and good effect of preparing hydrogen peroxide through photocatalysis, and can be applied to the fields of preparing hydrogen peroxide through photocatalysis, degrading organic matters and the like.
Drawings
FIG. 1 shows a three-dimensional flower-like pattern Bi @ Sn3O4SEM image of schottky junction visible light catalyst.
FIG. 2 shows Bi and Sn3O4And Bi @ Sn3O4XRD pattern of (a).
FIG. 3 is a graph of different gas environments vs. H2O2The resulting effect.
FIG. 4 is the different pH vs. H2O2The resulting effect.
FIG. 5 shows Sn under irradiation of visible light3O4And Bi @ Sn3O4Generation of H2O2The yield map of (a).
Detailed Description
Example 1 three-dimensional flower-like Sn3O4Preparation of Schottky junction visible light catalyst
(I) three-dimensional flower-like Sn3O4Preparation of
SnCl2·2H2O (0.9g, 4mmol) and trisodium citrate dihydrate (2.94g, 10mmol) were added to 10mL of deionized water, stirred until completely dissolved, then 10mL of 0.2mol/L NaOH solution was slowly added thereto, stirred for 30min, the resulting mixed solution was transferred to a 100mL stainless steel autoclave with a Teflon liner, maintained at 180 ℃ for 12h, cooled to room temperature, washed several times with deionized water and anhydrous ethanol, and dried at 60 ℃ to obtain Sn3O4。
Preparation of (II) Bi nanospheres
0.364g of Bi (NO)3)3·5H2O is dissolved in 10mL of 1mol/L HNO3To the solution, vigorously stirred for 30min, then 0.600g of polyvinylpyrrolidone (PVP) was added, and after dissolution with stirring, the resulting mixed solution was transferred to a 100mL stainless steel autoclave with Teflon lining and held at 160 ℃ for 12 h. After cooling to room temperature, washing with deionized water and absolute ethyl alcohol for several times, and drying at 60 ℃ to obtain the Bi nanospheres.
(III) three-dimensional flower-shaped Bi @ Sn3O4Preparation of
0.200g of three-dimensional flower-shaped Sn3O4Ultrasonically dispersing in 20mL of ethanol solution, adding 0.010g of Bi nanosphere, uniformly mixing the mixture for 2 hours at room temperature under the action of magnetic stirring, evaporating the solvent in a water bath at 80 ℃, and drying in an oven at 60 ℃ to obtain a target product Bi @ Sn3O4。
FIG. 1 shows a three-dimensional flower-like pattern Bi @ Sn3O4SEM image of schottky junction visible light catalyst. As can be seen from FIG. 1, Bi @ Sn3O4The composite material is Bi nanospheres embedded in three-dimensional Sn3O4In the micro-flower structure.
FIG. 2 shows Bi and Sn3O4And Bi @ Sn3O4XRD pattern of (a). The XRD spectrum of FIG. 2 shows that Bi @ Sn3O4The composite material consists of Bi and Sn3O4And (4) compounding.
Example 2 three-dimensional flower-like Bi @ Sn3O4Application of Schottky junction visible light catalyst in photocatalytic preparation of hydrogen peroxide
Gas atmosphere pair H2O2Influence of generation
The method comprises the following steps: weighing three-dimensional flower-shaped Bi @ Sn3O450mg of catalyst is added into a mixed solution containing 18mL of deionized water and 2mL of ethanol, and the mixture is subjected to ultrasonic treatment for 10min to obtain a suspension. Then using HClO4The pH of the suspension was adjusted to 3. Respectively adding N2Air and O2The suspension was passed through to allow continuous uniform bubbling through the solution. Then magnetically stirring in dark for 30min to reach the desired levelAnd (4) carrying out adsorption-desorption balance before injection. The mixture was irradiated with a 300W xenon lamp (. lamda. gtoreq.420 nm) as a light source to carry out the reaction. Extracting 1mL suspension from the reaction tank after reacting for 60min, adding 2mL of 0.1mol/L KI solution and 0.05mL of 0.01mol/L ammonium molybdate solution, measuring absorbance A (detection wavelength is 350nm) by UV-visible absorption spectrometry, and calculating H according to the established standard curve2O2The amount of production of (c).
As can be seen from FIG. 3, O was maintained for 60min2In atmosphere, Bi @ Sn3O4Photocatalytic preparation of H2O2The yield is the highest and is 92 mu mol/L; by replacing O by air2When H is present2O2Is reduced and adjusted to N2In the atmosphere, H2O2Is completely inhibited, which indicates that the oxygen reduction may be H2O2Is the only source of (a).
(II) pH vs. H2O2Influence of generation
The method comprises the following steps: weighing three-dimensional flower-shaped Bi @ Sn3O450mg of catalyst is added into a mixed solution containing 18mL of deionized water and 2mL of ethanol, and the mixture is subjected to ultrasonic treatment for 10min to obtain a suspension. Then using HClO4The pH values of the suspensions were adjusted to 2, 3 and 4, respectively. Then adding O2The suspension was passed through to allow continuous uniform bubbling through the solution. Magnetic stirring was then carried out in the dark for 30min to reach the adsorption-desorption equilibrium before irradiation. The mixture was irradiated with a 300W xenon lamp (. lamda. gtoreq.420 nm) as a light source to carry out the reaction. Extracting 1mL suspension from the reaction tank after reacting for 60min, adding 2mL of 0.1mol/L KI solution and 0.05mL of 0.01mol/L ammonium molybdate solution, measuring absorbance A (detection wavelength is 350nm) by UV-visible absorption spectrometry, and calculating H according to the established standard curve2O2The amount of production of (c).
As can be seen from FIG. 4, within 60min, Bi @ Sn3O4Photocatalytic preparation of H2O2The yield was highest at pH 3, 92 μmol/L. And at pH 2, H2O2The yield of (2) was 84. mu. mol/L, which is probably due to H produced2O2Is gradually oxidized to H by excess protons2O(H2O2+2H++2e-＝2H2O). When the pH is further increased to 4, H2O2The amount of the produced (C) is remarkably reduced. The above results indicate that pH 3 is photocatalytic H production2O2The optimum pH value of (1).
(III) different catalyst pairs H2O2Influence of generation
The method comprises the following steps: respectively weighing Sn3O4And Bi @ Sn3O450mg of each of the solutions was added to a mixed solution containing 18mL of deionized water and 2mL of ethanol, and the mixture was sonicated for 10 min. Then using HClO4The pH of the suspension was adjusted to 3. Mixing O with2The suspension was passed through to allow continuous uniform bubbling through the solution. Magnetic stirring was then carried out in the dark for 30min to reach the adsorption-desorption equilibrium before irradiation. The mixture was irradiated with a 300W xenon lamp (. lamda. gtoreq.420 nm) as a light source to carry out the reaction. During the reaction, 1mL of suspension was extracted from the reaction cell every 30min, 2mL of 0.1mol/L KI solution and 0.05mL of 0.01mol/L ammonium molybdate solution were added, the absorbance A (detection wavelength: 350nm) was measured by UV-visible absorption spectrometry, and H was calculated from the established standard curve2O2The amount of production of (c).
Adopts different photocatalysts to test the photocatalytic H production2O2Performance, results are shown in FIG. 5, Bi @ Sn3O4Photocatalytic production of H2O2The effect of (A) is better than that of a single-component photocatalyst. After reaction for 150min, Bi @ Sn3O4Photocatalytic preparation of H2O2The yield reaches the maximum value, about 112 mu mol/L, is Sn alone3O4Photocatalytic production of H2O22.4 times of the total weight of the powder.
Claims (10)
1. Three-dimensional flower-shaped Bi @ Sn3O4The Schottky junction visible light catalyst is characterized in that the three-dimensional flower-shaped Bi @ Sn3O4The preparation method of the Schottky junction visible light catalyst comprises the following steps: three-dimensional flower-shaped Sn3O4Ultrasonically dispersing in ethanol solution, adding Bi nanospheres, and magnetically stirring at room temperatureAfter 2h, evaporating the solvent to dryness, cooling to room temperature, and collecting a sample to obtain a target product Bi @ Sn3O4。
2. The three-dimensional flower-like Bi @ Sn of claim 13O4The Schottky junction visible light catalyst is characterized in that Sn is added according to the mass ratio3O4:Bi＝20:1。
3. The three-dimensional flower-like Bi @ Sn of claim 13O4The Schottky junction visible light catalyst is characterized in that the Sn is3O4The preparation method comprises the following steps: SnCl2·2H2Adding O and trisodium citrate dihydrate into deionized water, stirring until the O and the trisodium citrate dihydrate are completely dissolved, then slowly adding NaOH solution, carrying out hydrothermal reaction on the obtained mixture at 180 ℃ for 12h after stirring, cooling to room temperature after reaction, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 60 ℃ to obtain Sn3O4。
4. The three-dimensional flower-like Bi @ Sn of claim 33O4The Schottky junction visible light catalyst is characterized in that SnCl is added according to molar ratio2·2H2Trisodium citrate dihydrate 2: 5.
5. The three-dimensional flower-like Bi @ Sn of claim 33O4The Schottky junction visible light catalyst is characterized in that the concentration of the NaOH solution is 0.2 mol/L.
6. The three-dimensional flower-like Bi @ Sn of claim 13O4The Schottky junction visible light catalyst is characterized in that the preparation method of the Bi nanosphere comprises the following steps: adding Bi (NO)3)3·5H2Dissolving O in HNO3Adding polyvinylpyrrolidone (PVP) into the solution, stirring to dissolve, performing hydrothermal reaction at 160 deg.C for 12 hr, cooling to room temperature, and removingWashing the seed water with absolute ethyl alcohol, and drying at 60 ℃ to obtain the Bi nanosphere.
7. The three-dimensional flower-like Bi @ Sn of claim 63O4The Schottky junction visible light catalyst is characterized in that Bi (NO) is mixed by mass3)3·5H2O:PVP＝91:150。
8. A three-dimensional flower-like Bi @ Sn as claimed in any one of claims 1 to 73O4The application of the Schottky junction visible light catalyst in preparing hydrogen peroxide by photocatalysis.
9. Use according to claim 8, characterized in that the method is as follows: three-dimensional flower-shaped Bi @ Sn3O4Adding Schottky junction visible light catalyst into deionized water and ethanol, performing ultrasonic treatment for 10min, adjusting pH to 3, and adding O2The resulting suspension was passed through a magnetic stirrer and adsorbed by bubbling continuously and uniformly in the solution for 30min in the dark, and then the reaction was carried out by irradiation with a light source.
10. The application of claim 9, wherein the light source is a 300W xenon lamp, and the lambda of the xenon lamp is more than or equal to 420 nm.
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| CN103877966A (en) * | 2014-04-09 | 2014-06-25 | 扬州大学 | Preparation method of heterostructure photocatalyst |
| CN105396603A (en) * | 2015-12-08 | 2016-03-16 | 辽宁石油化工大学 | Bismuth oxychloride catalyst with visible light response core-shell structure and preparation method thereof |
| CN108043433A (en) * | 2017-12-11 | 2018-05-18 | 湖北大学 | One kind four aoxidizes three tin/silver orthophosphate composite material photocatalyst and preparation method thereof |
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