CN107497459B - Bi2Sn2O7/Bi24O31Br10Preparation method of composite visible light catalyst - Google Patents
Bi2Sn2O7/Bi24O31Br10Preparation method of composite visible light catalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims description 16
- 238000000034 method Methods 0.000 title abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 41
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 21
- 229910001868 water Inorganic materials 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 16
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
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- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
-
- B01J35/39—
Abstract
The invention discloses a Bi2Sn2O7/Bi24O31Br10The preparation method of the composite visible-light-driven photocatalyst comprises Bi2Sn2O7Nanoparticles and irregular nanoplatelets of Bi24O31Br10. The invention uses a hydrothermal method and a calcination method, namely Bi is utilized2Sn2O7And Bi24O31Br10Preparation of Bi by mixing precursors2Sn2O7/Bi24O31Br10A composite photocatalyst is provided. The composite photocatalyst can increase Bi24O31Br10The active sites on the surface can also promote the separation rate of carriers at the material interface. The invention has the advantages that: the method is simple, high in stability and strong in repeatability.
Description
Technical Field
The invention relates to a preparation method of a composite visible light catalyst, in particular to Bi2Sn2O7/Bi24O31Br10A preparation method of a composite visible light catalyst.
Background
The social development is followed by increasingly serious environmental pollution problems, particularly water pollution problems, and the water pollution problem is solved at all times. At present, the main reasons causing the water pollution problem are endless discharge of industrial wastewater, abuse of antibiotics and the like, and the pollutants in the water are difficult to be biodegraded or chemically degraded. In order to find a way to degrade these contaminants, researchers have conducted extensive researchHowever, the appearance of the photocatalyst indicates a new direction for solving the problem of water pollution. At present, the principle of a photocatalyst is that after a semiconductor material is irradiated with light, electrons are excited from a ground state to a conduction band, electrons in the conduction band and holes in a valence band participate in the generation of an active material, and the generated active material directly oxidizes and decomposes an organic substance. The main factors influencing the photocatalytic efficiency are the forbidden bandwidth of the semiconductor material and the recombination degree of electrons and holes. Therefore, researchers have made a number of modifications and developed a wide variety of photocatalysts. TiO is the most studied at present2Wide band gap semiconductors such as ZnO, which have a large forbidden band width and can only absorb ultraviolet light, have limited practical applications.
In recent years, bismuth-based oxide semiconductors have been favored by researchers as a novel, non-toxic, green photocatalyst. Although the special electronic structure and the relatively dispersed valence band structure of the bismuth-based material determine that most bismuth-based materials can absorb visible light, the material needs to be modified because the recombination rate of photogenerated electrons and hole pairs in the material is relatively high, and the construction of the composite material is one of the common methods for improving the photocatalytic efficiency.
Disclosure of Invention
The invention aims to provide Bi with simple method, high stability and strong repeatability2Sn2O7/Bi24O31Br10A preparation method of a composite visible light catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
bi2Sn2O7/Bi24O31Br10The preparation method of the composite visible light catalyst comprises the following steps:
1）Bi2Sn2O7the preparation of (1):
adding 0.5-2 mmol of Bi (NO)3)3Dissolving in 10-30 mL of nitric acid solution with the volume ratio of 1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain a clear solution A;
adding 0.5-2 mmol of Na2Sn2O3Dissolving in 20-50 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2The pH value of the O solution is 9-12, and a mixture D is obtained; transferring the mixture D into a 50mL polytetrafluoroethylene inner container, keeping the temperature at 180 ℃ for 24 hours, cooling to room temperature, respectively cleaning 3 times with 50-100 mL deionized water and 50-100 mL absolute ethyl alcohol, and drying at 70-90 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution:
adding 2-4 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 20-80 mL of glycol solution, and stirring for 1h at room temperature to obtain a solution E;
dissolving 2-4 mmol of KBr in 20-50 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 70-90 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10The preparation of (1):
adding 0.01 to 0.2g of Bi2Sn2O7Dispersing in 50-100 mL of ethanol-water solution with the volume ratio of 10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; dropwise adding the solution G into the mixture H to obtain a mixture I, after centrifugal separation, respectively cleaning 3 times with ultrapure water and absolute ethyl alcohol, and drying at 70-90 ℃ for 2 hours to obtain powder J; transferring the powder J into a muffle furnace, heating to 400-700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10And compounding the visible light catalyst.
Preferably, in Bi2Sn2O7In the preparation of (1), the drying temperature is 80 ℃.
Preferably, in Bi24O31Br10In the preparation of the precursor solution, a water bath is usedThe temperature of (a) is 80 ℃.
Preferably, in Bi2Sn2O7/Bi24O31Br10In the preparation of (1), the drying temperature is 80 ℃.
Bi of the present invention2Sn2O7/Bi24O31Br10The composite visible light catalyst is prepared by mixing Bi24O31Br10The precursor solution is dripped into the Bi dispersed solution2Sn2O7Ethanol-water solution of nano-particles, then centrifuging, washing and annealing to enable Bi2Sn2O7Nanoparticles attached to the sheet Bi24O31Br10On the surface, thereby forming a composite material, and improving the performance.
In a photocatalytic reaction system, factors such as defects in materials cause lower photocatalytic efficiency of single-component materials, so that the two materials with matched energy bands are constructed into a composite material, the recombination rate of photon-generated carriers can be reduced, and the method is a common method for improving the photocatalytic efficiency at present. Although Bi2Sn2O7Visible light can be absorbed, but the recombination rate of electrons and hole pairs formed by the material under the excitation of light is high, so that the photocatalytic efficiency is greatly influenced. And Bi24O31Br10As a two-dimensional material, the material also has response to visible light, and the recombination rate of photo-generated electrons and holes formed by light excitation is higher. Therefore, the nanoparticles can be compounded with the two-dimensional material, and the photocatalytic efficiency of the material can be improved by constructing the composite material. The invention firstly prepares Bi24O31Br10Precursor solution and Bi2Sn2O7Mixing the particles, annealing Bi in the composite material24O31Br10Phase formation to finally form the band structure cross-dislocation type Bi2Sn2O7/Bi24O31Br10And compounding the visible light catalyst. The Bi24O31Br10The precursor solution is Bi24O31Br10Clear solution before precipitation of precursorAnd (4) liquid. The cross dislocation type energy band structure is Bi2Sn2O7Both the valence band and the conduction band of (A) are higher or lower than Bi24O31Br10I.e. a mutually dislocated heterojunction structure. By adding Bi2Sn2O7Fine particles dispersed in the flake Bi24O31Br10On the surface, a potential difference is formed at the interface of the two materials, so that photogenerated carriers move to achieve effective separation, finally, different active substances are respectively formed on the surfaces of the two materials, the active substances can directly degrade pollutants in water, and the photogenerated electrons and hole pairs formed in the composite material can be effectively separated while the two materials can absorb visible light.
The invention adopts chemical methods to prepare Bi2Sn2O7/Bi24O31Br10The composite visible light catalyst has the advantages of simple method, high stability and strong repeatability.
Drawings
FIG. 1 shows Bi prepared according to the present invention2Sn2O7/Bi24O31Br10Scanning electron micrograph (c).
FIG. 2 is Bi2Sn2O7/Bi24O31Br10Transmission diagram of composite visible light catalyst.
FIG. 3 is Bi2Sn2O7-Bi24O31Br10Scanning electron micrographs of mechanical blends.
Detailed Description
Example 1:
1）Bi2Sn2O7preparation of
Adding 1.5 mmol of Bi (NO)3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 1.5 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring solution B toObtaining emulsion C in the solution A; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation of
0.03g of Bi2Sn2O7Dispersing in 50mL of ethanol-water solution with v/v =10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; dropwise adding the solution G into the mixture H to obtain a mixture I, after centrifugal separation, respectively washing with ultrapure water and absolute ethyl alcohol for 3 times, and drying at 80 ℃ for 2 hours to obtain powder J; transferring the powder J into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10A composite material.
The Bi produced can be seen from FIGS. 1 and 22Sn2O7/Bi24O31Br10The composite visible light catalyst consists of Bi2Sn2O7The nano particles are uniformly adhered to the sheet Bi24O31Br10On the surface.
Comparative example 1
1）Bi2Sn2O7Preparation of
1.5 mmol ofBi(NO3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 1.5 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G; dropwise adding the solution into an ethanol-water solution with the volume ratio of 50mL and v/v =10:1, after centrifugal separation, respectively washing the solution with ultrapure water and absolute ethanol for 3 times, and drying the solution at 80 ℃ for 2 hours to obtain powder H; transferring the powder H into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2H to obtain Bi24O31Br10Powder;
3）Bi2Sn2O7/Bi24O31Br10preparation of
1.0g of Bi2Sn2O7And 1.0g of Bi24O31Br10Dispersing the powder in 20 mL of absolute ethyl alcohol, performing ultrasonic treatment for 0.5h, stirring for 3h, and drying the solvent at 70 ℃ to obtain Bi2Sn2O7-Bi24O31Br10Mixing the photocatalyst.
SEM photograph of comparative example 1In FIG. 3, SEM pictures of example 1, i.e., FIGS. 1 and 2, are compared, and it can be seen that Bi obtained by mechanical blending2Sn2O7-Bi24O31Br10Bi in mixed photocatalyst24O31Br10Quilt Bi2Sn2O7And (4) coating.
Example 2:
1）Bi2Sn2O7preparation of
Adding 1.0 mmol of Bi (NO)3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 1.0 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation of
0.01g of Bi2Sn2O7Dispersing in 50mL of ethanol-water solution with v/v =10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; adding solution G dropwise into mixture H to obtain mixture I, and centrifugingAfter separation, respectively cleaning the obtained product by using ultrapure water and absolute ethyl alcohol for 3 times, and drying the obtained product at 80 ℃ for 2 hours to obtain powder J; transferring the powder J into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10A composite material.
Example 3:
1）Bi2Sn2O7preparation of
2.0 mmol of Bi (NO)3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 2.0 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation of
0.05g of Bi2Sn2O7Dispersing in 50mL of ethanol-water solution with v/v =10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; adding solution G dropwise into mixture H to obtain mixture I, and centrifugingAfter separation, respectively cleaning the obtained product by using ultrapure water and absolute ethyl alcohol for 3 times, and drying the obtained product at 80 ℃ for 2 hours to obtain powder J; transferring the powder J into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10A composite material.
Example 4:
1）Bi2Sn2O7preparation of
3.0 mmol of Bi (NO)3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 3.0 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation of
0.1g of Bi2Sn2O7Dispersing in 50mL of ethanol-water solution with v/v =10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; adding solution G dropwise into mixture H to obtain mixture I, and centrifugingThen, respectively cleaning the obtained product by using ultrapure water and absolute ethyl alcohol for 3 times, and drying the obtained product for 2 hours at 80 ℃ to obtain powder J; transferring the powder J into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10A composite material.
Example 5:
1）Bi2Sn2O7preparation of
3.0 mmol of Bi (NO)3)3Dissolving in 10 mL nitric acid solution with v/v =1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain clear solution A;
adding 3.0 mmol of Na2Sn2O3Dissolving in 10 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2O till the pH value is 12 to obtain a mixture D; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for three times, and drying at 80 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution
3.8 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 50mL of glycol solution, and stirring the mixture for 1 hour at room temperature to obtain a solution E;
dissolving 3.8 mmol of KBr in 20 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; and heating the mixture G in a water bath at 80 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G.
3）Bi2Sn2O7/Bi24O31Br10Preparation of
0.15g of Bi2Sn2O7Dispersing in 50mL of ethanol-water solution with v/v =10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; dropwise adding the solution G into the mixture H to obtain a mixture I, and centrifuging the mixture IRespectively cleaning with ultrapure water and absolute ethyl alcohol for 3 times, and drying at 80 ℃ for 2h to obtain powder J; transferring the powder J into a muffle furnace, heating to 700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10A composite material.
Claims (4)
1. Bi2Sn2O7/Bi24O31Br10The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
1）Bi2Sn2O7the preparation of (1):
adding 0.5-2 mmol of Bi (NO)3)3Dissolving in 10-30 mL of nitric acid solution with the volume ratio of 1:10, performing ultrasonic treatment for 10min, and stirring for 20min to obtain a clear solution A;
adding 0.5-2 mmol of Na2Sn2O3Dissolving in 20-50 mL of deionized water to obtain a solution B;
transferring the solution B into the solution A to obtain emulsion C; adding NH dropwise to emulsion C3•H2The pH value of the O solution is 9-12, and a mixture D is obtained; transferring the mixture D into a 50mL polytetrafluoroethylene liner, keeping the temperature at 180 ℃ for 24h, cooling to room temperature, respectively washing with deionized water and absolute ethyl alcohol for 3 times, and drying at 70-90 ℃ to obtain Bi2Sn2O7A yellow powder;
2）Bi24O31Br10preparation of precursor solution:
adding 2-4 mmol of Bi (NO)3)3Ultrasonically dissolving the mixture in 20-80 mL of glycol solution, and stirring for 1h at room temperature to obtain a solution E;
dissolving 2-4 mmol of KBr in 20-50 mL of ethylene glycol, and stirring for 1h to obtain a solution F;
adding the solution F into the solution E, and stirring for 1h to obtain a mixture G; heating the mixture G in a water bath at 70-90 ℃ for 4.5h, and stirring at room temperature for 0.5h to room temperature to obtain a clear solution G;
3）Bi2Sn2O7/Bi24O31Br10the preparation of (1):
adding 0.01 to 0.2g of Bi2Sn2O7Dispersing in 50-100 mL of ethanol-water solution with the volume ratio of 10:1, and performing ultrasonic treatment for 0.5H to obtain a mixture H; dropwise adding the solution G into the mixture H to obtain a mixture I, after centrifugal separation, respectively cleaning 3 times with ultrapure water and absolute ethyl alcohol, and drying at 70-90 ℃ for 2 hours to obtain powder J; transferring the powder J into a muffle furnace, heating to 400-700 ℃ at a heating rate of 5 ℃ per min, and keeping for 2h to obtain Bi2Sn2O7/Bi24O31Br10And compounding the visible light catalyst.
2. The Bi of claim 12Sn2O7/Bi24O31Br10The preparation method of the composite visible light catalyst is characterized in that Bi is added2Sn2O7In the preparation of (1), the drying temperature is 80 ℃.
3. The Bi of claim 12Sn2O7/Bi24O31Br10The preparation method of the composite visible light catalyst is characterized in that Bi is added24O31Br10In the preparation of the precursor solution, the temperature of the water bath is 80 ℃.
4. The Bi of claim 12Sn2O7/Bi24O31Br10The preparation method of the composite visible light catalyst is characterized in that Bi is added2Sn2O7/Bi24O31Br10In the preparation of (1), the drying temperature is 80 ℃.
Priority Applications (1)
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| CN106925304A (en) * | 2017-04-19 | 2017-07-07 | 宁德师范学院 | Bi24O31Br10/ ZnO composite visible light catalysts and preparation method thereof |
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