CN113546648B - Preparation method of ultrathin nano wafer-shaped BiOBr high-activity photocatalyst - Google Patents
Preparation method of ultrathin nano wafer-shaped BiOBr high-activity photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 68
- 230000000694 effects Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 56
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000012265 solid product Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000004108 freeze drying Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 239000002798 polar solvent Substances 0.000 claims abstract description 7
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 6
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 239000011787 zinc oxide Substances 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 description 1
- 238000012726 Water-in-Oil Emulsion Polymerization Methods 0.000 description 1
- KIJXJCBYANQZLF-UHFFFAOYSA-N [Ce].[C] Chemical compound [Ce].[C] KIJXJCBYANQZLF-UHFFFAOYSA-N 0.000 description 1
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- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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- 125000005843 halogen group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- 229910052740 iodine Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
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- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
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- 239000011733 molybdenum Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention relates to a preparation method of an ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst, which comprises the following steps: firstly, at room temperature, Bi is added3+Adding the mixture into ethylene glycol, fully dissolving the mixture by magnetic stirring, adding aniline and stirring again to obtain a uniform and transparent mixed solution; secondly, adding Br into the mixed solution slowly and dropwise‑Fully stirring the aqueous solution until the aqueous solution is uniformly dispersed to obtain a BiOBr precursor solution; thirdly, transferring the precursor solution to a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining for reaction, then cooling to room temperature, and separating to obtain an off-white solid product; and fourthly, washing the off-white solid product for several times by using a polar solvent, and freeze-drying to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst. The method has the advantages of simple process, easily available raw materials, low cost, green and environment-friendly whole preparation process, safety and reliability. The obtained photocatalyst has the advantages of multiple photocatalytic active sites, large specific surface area, greenness, no toxicity and the like.
Description
Technical Field
The invention relates to the field of material science and the technical field of industrial wastewater treatment, in particular to a preparation method of an ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst.
Background
The problem of water pollution is always a hot focus object for environmental protection, and with the rapid development of economic science in China, the discharge of organic wastewater seriously harms fresh water resources in China. The organic pollutants are various in types, properties and pollution sources. The rhodamine B (RhB) is a typical cationic dye with wide application, and is a pollutant of nitrogen-containing dye. The presence of RhB affects not only the aesthetics of the water environment, but also water resources and human health. For this reason, many researchers have used a series of methods to remove these dye contaminants, including physical (adsorption), biological oxidation, and chemical treatment methods. For example, the invention patent CN 111729650 a discloses a ferroferric oxide @ covalent organic framework adsorption material and application thereof in removing organic dyes in wastewater, although the material has a large specific surface area and strong adsorption performance, the adsorption can only transfer pollutants, secondary pollution is easily caused, the preparation cost is high, and the thorough separation between the prepared adsorbent and the adsorbate also has a certain problem. In the process of biological oxidation, the amount of the biological film increases along with the increase of load, and if the load is too high, the biological film is too thick and is easy to block in some fillers, and when the fillers are selected, the conditions are too complicated and harsh under the influence of various factors. The two methods can not effectively remove the dye pollutants, can also generate potential carcinogenic aromatic amine to seriously affect the human health, and can cause immeasurable secondary pollution to the environment. Although some chemical methods can achieve the purpose of degradation, more serious secondary pollution is easily formed.
Comparing and analyzing these treatments, it is clear that, although each type of treatment has its advantages, it also has some disadvantages. Moreover, energy shortage and environmental pollution seriously threaten future development of human society at present. Therefore, photocatalytic materials have come to be produced. The presence of photocatalytic materials makes full use of the natural source of solar energy while compensating for these deficiencies. The photocatalytic technology has been widely applied to the fields of environment harmless treatment, energy conversion and the like. For example, patent CN 112958093 a discloses a photocatalyst with oxygen defect of cobalt ferrite, and a preparation method and application thereof, but the photocatalytic material also has a problem of dissolution of cobalt ions, which causes secondary pollution to the environment. Therefore, besides potential toxicity, most photocatalytic materials have the problems of poor visible light absorption capacity (only ultraviolet light can be subjected to photodegradation, and the ultraviolet light only accounts for 4-5% of solar energy), wide band gap capacity, few active sites and the like, so that the application of the photocatalytic materials in the field of photocatalysis is further limited.
Therefore, the development of a novel photocatalyst with high activity, which can meet the actual production and living needs and can be used efficiently, sustainably and stably has become a urgent needThe problem to be solved. There are many prior art methods for the synthesis of semiconductor photocatalytic materials that have been used to adsorb and degrade organic contaminants. For example, patent CN 109395710 a discloses a method for preparing cerium-carbon co-doped zinc oxide, which improves the photocatalytic activity of ZnO, but the synthesis process requires calcination, and thus has high energy consumption and high cost. The composite photocatalytic material raises the heat tide of photocatalyst modification, and the composite material is prepared by compounding a material with excellent photodegradation performance and easy agglomeration with a proper carrier to achieve the purpose of reducing catalyst agglomeration, or compounding two semiconductor materials with common photocatalytic performance to improve the comprehensive performance, or compounding a composite material to increase the specific surface area, thereby increasing the active sites of the photocatalyst. Such as: the invention patent CN 112871179A discloses an Er-Fe2O3/BiVO4 photocatalyst for degrading rhodamine B and a preparation method thereof, wherein Er is doped into Fe-2O-3 to enlarge the light absorption range thereof, thereby achieving the purpose of improving the band gap energy of the material; however, the preparation process of the material is too complex, and the material needs to be calcined, so that the requirement of low cost and economic effect is not met. Wang et al (simple failure of CdS/UiO-66-NH)2heterojunction photocatalysts for efficient and stable photodegradation of pollution, Journal of Photochemistry &Photobiology A Chemistry 2019, 376: 80-87) prepares CdS/UiO-66-NH by a water bath deposition method2The heterojunction photocatalyst is used for removing tetracycline and methyl orange under visible light. However, none of these techniques has achieved the objective of improving the photocatalytic activity itself.
BiOBr belongs to a series of BiOX (X = F, Cl, Br, I) families, which crystallizes in a tetragonal layered structure, the Bi center of each layer being surrounded by four oxygen atoms with strong covalent bonds and four halogen atoms with weak inter-layer van der Waals interactions. BiOBr is a promising photocatalyst because it has good chemical stability, relatively appropriate band gap energy and excellent photoelectric separation efficiency, and has been used for nitrogen fixation and H production2Photo-reduction of CO2And wastewater treatment. It can be used as a good photocatalyst for treating organic dye wastewater andantibiotic wastewater can improve the environmental problem. However, the high recombination rate of the photogenerated carriers inhibits the photocatalytic activity of the BiOBr, and in order to improve the charge separation efficiency, typical methods such as doping, crystal face exposure, construction of Oxygen Vacancies (OV), surface modification, construction of heterojunction, and the like can be employed. For example: the invention patent CN 110813326A discloses a preparation method of a C-doped BiOBr microsphere photocatalyst, which can be used for degrading organic wastewater, the material not only achieves controllable design of morphology, but also has excellent photodegradation performance, and the material has the characteristics of simple preparation method and low raw material cost. Such as: the invention patent CN 112892608A discloses a composite material of water-stable photodegradation organic pollutants and a preparation method thereof, the composite material is prepared by compounding MOF-808 containing six-core Zr group and a semiconductor photocatalytic material BiOBr, and can be used for degrading organic pollutants such as rhodamine B, methyl orange and antibiotic ciprofloxacin, but the preparation cost of the MOF is high, certain metal ion leaching problem exists, and secondary pollution is easy to form. For example, the invention patent CN 111792700 a discloses the application of BiOBr or oxygen vacancy BiOBr in removing organic matters in algae and a removing method thereof, the invention modifies BiOBr by constructing oxygen vacancy, and researches the removal of organic algae, although the construction of oxygen vacancy improves the photocatalytic activity of BiOBr, in practical application, the practicability and recycling performance of BiOBr need to be considered comprehensively. The invention patent CN 112371140A discloses a coral-shaped MoS2Photocatalyst and MoS2The preparation method of the-BiOBr heterojunction composite photocatalytic material is to use MoS with more coral-shaped structures with exposed active sites2And a heterojunction is constructed between the photocatalyst and BiOBr to achieve the purpose of improving the photocatalytic activity of the photocatalyst, but secondary pollution caused by dissolution of molybdenum ions cannot be considered, and the importance of the recycling performance of the photocatalyst in practical application is ignored.
The research of the photocatalytic material is gradually developed from a common semiconductor material to the steps of reducing the agglomeration phenomenon of the semiconductor material by means of a carrier, constructing a heterojunction by doping metal and nonmetal thereof and the photocatalytic material with excellent performance, and inducing the specific crystal face of the semiconductor material to be exposed or inducing the semiconductor material to generate specific morphology by adopting natural macromolecules. However, the research results focus on improving the photocatalytic performance, neglect the improvement of the performance of the material and the concept of cycle stability, economic benefit and environmental protection without pollution which need to be considered in the practical application of the material, and do not solve the problem of actual pollution from the source.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst with simple process and low cost.
In order to solve the problems, the preparation method of the ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst comprises the following steps:
firstly, at room temperature, Bi is added3+Adding the mixture into ethylene glycol, fully dissolving the mixture through magnetic stirring, adding aniline, and stirring for 20-60 min to obtain a uniform and transparent mixed solution; the Bi3+The mass ratio of the ethylene glycol to the ethylene glycol is 1: 30-1: 60, adding a solvent to the mixture; the Bi3+The mass ratio of the aniline to the aniline is 1: 0.1-1: 2;
secondly, slowly dripping Br with the concentration of 0.01-0.05 g/mL into the mixed solution-Fully stirring the aqueous solution until the aqueous solution is uniformly dispersed to obtain a BiOBr precursor solution; the Bi3+With said Br-Br in aqueous solution-The mass ratio of (1): 1-3: 1; said ethylene glycol and said Br-The volume ratio of the aqueous solution is 1: 1-5: 1;
thirdly, transferring the precursor solution into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15-25 h at 150-200 ℃, cooling to room temperature, and separating to obtain an off-white solid product;
and fourthly, washing the off-white solid product for several times by using a polar solvent, and freeze-drying to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
The magnetic stirring condition in the step refers to that the rotating speed is 500-1000 rpm, and the time is 20-60 min.
The step includes middle Bi3+Refers to Bi (NO)3)3、Bi(NO3)3•5H2O or BiOCl.
The step of adding Br-The aqueous solution refers to an aqueous solution of KBr or NaBr.
The polar solvent in the step four is one or two mixed liquids of absolute ethyl alcohol, absolute methyl alcohol and distilled water.
And step four, washing times are 2-6, and the amount of the detergent is 5-20 mL each time.
The conditions of freeze drying in the step four are that the temperature is-20 to-55 ℃, and the freezing time is 10 to 24 hours.
Compared with the prior art, the invention has the following advantages:
1. the invention takes ethylene glycol and water as Bi respectively at normal temperature3+And Br-The solvent is used for preparing a BiOBr precursor solution by a water-in-oil emulsion polymerization method, and then the photocatalyst with high hydrothermal stability and excellent photodegradation stability is prepared by hydrothermal reaction.
2. By analyzing the shape of the ultrathin nanometer wafer BiOBr high-activity photocatalyst prepared by the invention, more surface active sites can be generated due to the fact that the ultrathin nanometer wafer shape has larger specific surface area, so that the photocatalyst can be fully contacted with a substrate to further exert the performances of synergistic high-efficiency degradation and good circulation stability, and the aims of regulating and improving the shape and the photocatalytic performance of the traditional BiOBr nanometer sheet are fulfilled.
3. The ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst obtained by the invention has excellent photodegradability when being used for photocatalytic degradation of cationic dyes, is recycled for 10 times, has almost no change in the photodegradability, and can be used for treatment of dye wastewater.
4. The method has the advantages of simple process, easily available raw materials, low cost, green and environment-friendly whole preparation process, safety and reliability. The obtained photocatalyst has the advantages of multiple photocatalytic active sites, large specific surface area, greenness, no toxicity and the like, and can be applied to photocatalytic degradation of cationic dyes (such as rhodamine B, malachite green, crystal violet and the like) and anionic dyes (such as bromocresol green and formazanBlue, etc.), antibiotics (such as tetracycline, ciprofloxacin, etc.), and heavy metal ions (Cr) can be reduced2O7 2-)。
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a Scanning Electron Microscope (SEM) image of the high activity photocatalyst of the BiOBr ultrathin nanosheet obtained in example 1 of the present invention and the conventional BiOBr nanosheet photocatalyst. Wherein: the left image is an SEM image of the conventional BiOBr, and the right image is an SEM image of the BiOBr ultrathin nano wafer.
Fig. 2 is an Element Distribution Scanning (EDS) diagram of the high-activity photocatalyst of the BiOBr ultrathin nano wafer obtained in example 1 of the present invention.
Fig. 3 is an X-ray powder diffraction (XRD) pattern of the high activity photocatalyst of the BiOBr ultra-thin nano-wafer obtained in example 1 of the present invention.
Fig. 4 is a graph of the degradation effect and the recycling performance of the high-activity photocatalyst of the BiOBr ultrathin nano wafer obtained in example 1 of the present invention on organic pollutants. The left graph is a degradation effect graph of the conventional BiOBr and the BiOBr ultrathin nano wafer, and the right graph is a recycling performance graph of the BiOBr ultrathin nano wafer.
Detailed Description
A preparation method of an ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst comprises the following steps:
firstly, at room temperature, Bi is added3+Adding the mixture into ethylene glycol, magnetically stirring the mixture for 20 to 60 minutes at the rotating speed of 500 to 1000 rpm to fully dissolve the mixture, then adding aniline and stirring the mixture for 20 to 60 minutes to obtain a uniform and transparent mixed solution.
Wherein: bi3+Refers to Bi (NO)3)3、Bi(NO3)3•5H2O or BiOCl.
Bi3+The mass ratio of the ethylene glycol to the ethylene glycol is 1: 30-1: 60, adding a solvent to the mixture; bi3+The mass ratio of the aniline to the aniline is 1: 0.1-1: 2.
secondly, slowly dripping Br with the concentration of 0.01-0.05 g/mL into the mixed solution-And fully stirring the aqueous solution until the aqueous solution is uniformly dispersed to obtain a precursor solution of BiOBr.
Wherein: br-The aqueous solution refers to an aqueous solution of KBr or NaBr.
Bi3+With Br-Br in aqueous solution-The mass ratio of (1): 1-3: 1; ethylene glycol and Br-The volume ratio of the aqueous solution is 1: 1-5: 1.
thirdly, transferring the precursor solution into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15-25 h at 150-200 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And fourthly, washing the off-white solid product with a polar solvent for 2-6 times with the use amount of 5-20 mL each time, and then carrying out freeze drying at-20 to-55 ℃ for 10-24 h to obtain the ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst.
Wherein: the polar solvent is one or two of absolute ethyl alcohol, absolute methyl alcohol and distilled water.
Embodiment 1 a method for preparing an ultra-thin nano disk-shaped high-activity BiOBr photocatalyst, comprising the following steps:
first, 0.500 g of Bi (NO) was stirred at room temperature and 600 rpm3)3Dissolving in 16.8 mL of ethylene glycol, stirring for 20 min to dissolve completely, adding 0.0265 g of aniline, and stirring for 20 min to obtain a uniform and transparent mixed solution.
And slowly dripping 16.8 mL of aqueous solution containing 0.341 g of NaBr solid into the mixed solution, and continuously stirring until the dispersion is uniform, so that water-in-oil emulsion can rapidly appear, and the precursor solution of the BiOBr is obtained.
Thirdly, transferring the precursor solution into a 50 mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15 h at 150 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And fourthly, washing the gray white solid product with 5.0 mL of absolute ethyl alcohol for 3 times, and carrying out freeze drying treatment at-40 ℃ for 10 hours to obtain the ultrathin nano wafer-shaped BiOBr high-activity photocatalyst.
The degradation rate of the catalyst to RhB can reach 100% within 120 min of illumination.
[ microcosmic morphology ]
The microscopic shape Scanning Electron Microscope (SEM) picture of the ultrathin nanometer wafer BiOBr high-activity photocatalyst prepared by the invention is shown in figure 1. As can be seen from the SEM photographs, the conventional BiOBr nanoplates (left panel) had a thickness of about 200 nm and a size of about 3 μm; the BiOBr ultrathin nano wafer prepared by the invention has the advantages of thinner thickness (about 50 nm), smaller size (about 0.6 mu m) and far smaller size than that of the conventional BiOBr nano sheet, which indicates that the BiOBr ultrathin nano wafer-shaped BiOBr prepared by the invention has larger specific surface area, is more favorable for full contact with a degradation substrate and further promotes the occurrence of a photocatalytic reaction. The BiOBr precursor is in a water-in-oil state and is wrapped in the BiOBr precursor in the presence of aniline, so that the growth of the BiOBr is controlled under the condition of not destroying the crystal form of the BiOBr precursor, and finally the BiOBr ultrathin nano wafer high-activity photocatalyst is formed under the hydrothermal reaction condition. In conclusion, the method proves that the BiOBr ultrathin nanometer wafer high-activity photocatalyst is successfully prepared.
[ EDS elemental analysis ]
The distribution of each element in the selected area of the prepared ultrathin nanometer wafer BiOBr high-activity photocatalyst is analyzed by EDS, and the result is shown in figure 2. It can be obviously seen that the high-activity photocatalyst of the BiOBr ultrathin nanometer wafer mainly contains Bi, Br, O, C and N elements, wherein C, N elements are derived from aniline. Moreover, the elements can be seen to be uniformly distributed in the selected area, which indicates that the elements in the photocatalyst are uniformly distributed, and also indicates that aniline plays a certain role in inducing the improvement of the traditional BiOBr morphology in the process.
[ X-ray diffraction (XRD) analysis ]
XRD analysis is carried out on the prepared ultrathin nanometer wafer BiOBr high-activity photocatalyst so as to determine the crystal structure, the crystallinity and other information of the BiOBr ultrathin nanometer wafer high-activity photocatalyst, and the result is shown in figure 3. As can be understood from the figure, the characteristic diffraction peaks of BiOBr appear at 2 θ = 8.1 °, 25.2 °, 31.7 °, 32.2 °, 39.4 °, 46.2 °, 56.7 °, 57.1 °, 67.4 °, and 76.7 °, corresponding to the (001), (101), (102), (110), (112), (200), (104), (212), (220), and (310) crystal planes of the BiOBr crystal, respectively. The characteristic diffraction peaks are all shown in the photocatalyst, and the BiOBr ultrathin nanometer wafer high-activity photocatalyst keeps the crystal form and the structure of BiOBr.
[ photodegradability ] of
The degradation performance of the ultrathin nanometer wafer BiOBr high-activity photocatalyst prepared by the invention is tested by taking organic dye rhodamine B (RhB) as a simulated degradation substrate. First, the degradation efficiency was tested at room temperature at an initial RhB concentration of 5 mg/L. The experimental result shows that the degradation rate of the BiOBr ultrathin nano wafer high-activity photocatalyst on RhB pollutants reaches 100% within 120 min of illumination, and the result is shown in figure 4 (left). The photocatalyst was further examined for cycle stability (fig. 4 (right)), and it was found that the degradation rate of the catalyst was not substantially changed after 10 cycles of bad use. The catalyst has excellent degradation performance on organic pollutants, high degradation efficiency and high recycling rate.
In addition, in the actual dye wastewater treatment, aiming at wastewater with different dye concentrations, a proper amount of photocatalyst can be considered to be added in the treatment process, and the purpose of thoroughly removing pollutants can be achieved. Further illustrates that the high-activity photocatalyst of the BiOBr ultrathin nanometer wafer has excellent catalytic degradation performance in the aspect of removing organic pollutants.
Embodiment 2 a method for preparing an ultra-thin nano disk-shaped high-activity BiOBr photocatalyst, comprising the following steps:
firstly, 1.891 g of Bi (NO) is stirred at room temperature and 800 rpm3)3•5H2Dissolving O in 50.0 mL of glycol, stirring for 30 min to fully dissolve the O, continuously adding 3.782 g of aniline, and stirring for 30 min to obtain a uniform and transparent mixed solution.
And slowly dripping 10.0 mL of water solution containing 0.608 g of KBr solid in the mixed solution, and continuously stirring until the water-in-oil emulsion is uniformly dispersed, so that the BiOBr precursor solution can be quickly obtained.
Thirdly, transferring the precursor solution into a 100 mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15 h at 180 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And (4) washing the off-white solid product with 10.0 mL of alcohol-water mixed solution (methanol: water =1: 1) for 5 times, and carrying out freeze drying treatment at-40 ℃ for 15 hours to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
The degradation rate of the catalyst to RhB can reach 100% within 120 min of illumination.
Embodiment 3 a method for preparing an ultra-thin nano disk-shaped high-activity BiOBr photocatalyst, comprising the following steps:
firstly, dissolving 0.229 g of BiOCl in 7.5 mL of ethylene glycol at room temperature under the stirring condition of 750 rpm, stirring for 25 min to fully dissolve the BiOCl, and then continuously adding 0.184 g of aniline and stirring for 25 min to obtain a uniform and transparent mixed solution.
And slowly dripping 3.0 mL of aqueous solution containing 0.137 g of KBr solid into the mixed solution, and continuously stirring until the dispersion is uniform, so that water-in-oil emulsion can rapidly appear, and the precursor solution of the BiOBr is obtained.
Thirdly, transferring the precursor solution into a 50 mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15 h at 150 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And (4) washing the off-white solid product with 8.0 mL of alcohol-water mixed solution (ethanol: water =2: 1) for 5 times, and carrying out freeze drying treatment at-45 ℃ for 12 hours to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
The degradation rate of the catalyst to RhB can reach 100% within 120 min of illumination.
Embodiment 4 a method for preparing an ultra-thin nano disk-shaped high-activity BiOBr photocatalyst, comprising the following steps:
first, 0.963 g of Bi (NO) was stirred at 750 rpm at room temperature3)3•5H2O is dispersed in 40.0 mL of ethylene glycol, stirred for 35 min, 0.415 g of aniline is added continuously, and stirred for 35 min to obtain a uniform and transparent mixed solution.
And slowly dropwise adding 10.0 mL of water solution containing 0.360 g of KBr solid into the mixed solution, and fully stirring until the solution is uniformly dispersed, thereby obtaining the precursor solution of BiOBr.
Thirdly, transferring the precursor solution into a 100 mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 18 h at 150 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And fourthly, washing the off-white solid product with 8.0 mL of water for 3 times, and carrying out freeze drying treatment at-48 ℃ for 12 hours to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
The degradation rate of the catalyst to RhB within 120 min of illumination reaches 100%.
Embodiment 5 a method for preparing an ultra-thin nano disk-shaped high-activity BiOBr photocatalyst, comprising the following steps:
first, 1.153 g of BiOCl was dispersed in 50 mL of ethylene glycol at room temperature under stirring at 750 rpm, and stirred for 35 min, 0.925 g of aniline was continuously added, and stirred for 35 min to obtain a uniform and transparent mixed solution.
And slowly dropwise adding 15.0 mL of aqueous solution containing 0.690 g of KBr solid into the mixed solution, and fully stirring until the solution is uniformly dispersed, thereby obtaining the precursor solution of BiOBr.
Thirdly, transferring the precursor solution into a 100 mL stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 14 h at 150 ℃, cooling to room temperature, and separating to obtain an off-white solid product.
And fourthly, washing the off-white solid product with 10.0 mL of water for 3 times, and carrying out freeze drying at-53 ℃ for 14 hours to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
The degradation rate of the catalyst to RhB within 120 min of illumination reaches 100%.
Claims (7)
1. A preparation method of an ultrathin nanometer disk-shaped BiOBr high-activity photocatalyst comprises the following steps:
firstly, at room temperature, Bi is added3+Adding the mixture into ethylene glycol, fully dissolving the mixture by magnetic stirring, adding aniline, stirring for 20-60 min,obtaining a uniform and transparent mixed solution; the Bi3+The mass ratio of the ethylene glycol to the ethylene glycol is 1: 30-1: 60, adding a solvent to the mixture; the Bi3+The mass ratio of the aniline to the aniline is 1: 0.1-1: 2;
secondly, slowly dripping Br with the concentration of 0.01-0.05 g/mL into the mixed solution-Fully stirring the aqueous solution until the aqueous solution is uniformly dispersed to obtain a BiOBr precursor solution; the Bi3+With said Br-Br in aqueous solution-The mass ratio of (1): 1-3: 1; said ethylene glycol and said Br-The volume ratio of the aqueous solution is 1: 1-5: 1;
thirdly, transferring the precursor solution into a stainless steel hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 15-25 h at 150-200 ℃, cooling to room temperature, and separating to obtain an off-white solid product;
and fourthly, washing the off-white solid product for several times by using a polar solvent, and freeze-drying to obtain the ultrathin nano disc-shaped BiOBr high-activity photocatalyst.
2. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: the magnetic stirring condition in the step refers to that the rotating speed is 500-1000 rpm, and the time is 20-60 min.
3. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: the step includes middle Bi3+Refers to Bi (NO)3)3、Bi(NO3)3•5H2O or BiOCl.
4. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: the step of adding Br-The aqueous solution refers to an aqueous solution of KBr or NaBr.
5. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: the polar solvent in the step four is one or two mixed liquids of absolute ethyl alcohol, absolute methyl alcohol and distilled water.
6. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: and step four, washing times are 2-6, and the amount of the detergent is 5-20 mL each time.
7. The preparation method of the ultrathin nano disk-shaped BiOBr high-activity photocatalyst as claimed in claim 1, characterized in that: the conditions of freeze drying in the step four are that the temperature is-20 to-55 ℃, and the freezing time is 10 to 24 hours.
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