CN112516991B - Preparation method of bismuth oxide photocatalyst with two-dimensional structure - Google Patents
Preparation method of bismuth oxide photocatalyst with two-dimensional structure Download PDFInfo
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- CN112516991B CN112516991B CN202011546466.3A CN202011546466A CN112516991B CN 112516991 B CN112516991 B CN 112516991B CN 202011546466 A CN202011546466 A CN 202011546466A CN 112516991 B CN112516991 B CN 112516991B
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 40
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000004729 solvothermal method Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 10
- 229920000570 polyether Polymers 0.000 claims description 10
- 150000001735 carboxylic acids Chemical class 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 239000004698 Polyethylene Substances 0.000 claims 1
- 239000004743 Polypropylene Substances 0.000 claims 1
- -1 polyethylene Polymers 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- 229920000428 triblock copolymer Polymers 0.000 claims 1
- 239000002135 nanosheet Substances 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 10
- 229940043267 rhodamine b Drugs 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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Classifications
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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
-
- B01J35/39—
-
- 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
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention belongs to the field of novel catalysts, and discloses bismuth oxide (Bi) with a two-dimensional structure 2 O 3 ) A preparation method of the photocatalyst. Which comprises the following steps: (1) preparing an ethanol/ethylene glycol solution of P123; (2) Adding bismuth nitrate until the bismuth nitrate is completely dissolved, adding a certain amount of oxalic acid to adjust the pH value, and magnetically stirring; (3) And carrying out solvothermal reaction, washing, centrifuging and drying to obtain the bismuth oxide photocatalyst with the two-dimensional structure. The preparation method is simple and convenient, the cost is low, and the product has high purity, uniform appearance, good dispersibility and stable performance. The bismuth oxide nanosheet with the two-dimensional structure, which is prepared by the method, has the advantages of high solar energy utilization rate, high quantum efficiency and high photocatalytic activity, and can be applied to catalyzing degradation of organic pollutants in the field of environment.
Description
Technical Field
The invention relates to the field of novel catalysts, in particular to a preparation method of a bismuth oxide photocatalyst with a two-dimensional structure.
Background
The adoption of semiconductor photocatalysis technology for treating environmental pollution is increasingly gaining attention. Theoretically, as long as the energy of the excitation light is larger than the energy value of the band gap of the semiconductor, photogenerated electrons and holes can be generated, and the semiconductor can be possibly used as a photocatalytic material. However, due to the factors such as material cost, chemical stability and photo-corrosion resistance, the efficient and practical semiconductor photocatalytic material needs to be studied intensively. Common anatase phase TiO 2 Photocatalysts have been studied more and more extensively, but with a wider band gap (E g =3.2 eV) can only absorb ultraviolet light, and has low solar energy utilization rate, low light quantum efficiency and low catalytic activity. Therefore, there is a need to develop a visible-light-driven photocatalyst having high performance. The bismuth compound has good photogenerated carrier separation capacity and visible light response performance, and compared with the traditional block nano material, the two-dimensional semiconductor nano sheet can effectively improve the electron transfer efficiency and the surface energy and ensure effective light absorptionThe adsorption of target reactants is absorbed, the generation of interface catalytic reaction is promoted, and photo-generated charges can be rapidly transferred from the interior of the material to the surface, so that the high separation efficiency of bulk phase charges is ensured. At present, relevant reports of a preparation method of a bismuth oxide photocatalyst based on a two-dimensional structure are rarely seen.
Disclosure of Invention
The invention aims to provide a controllable preparation method of a bismuth oxide nanosheet photocatalyst with a two-dimensional structure, in order to research and develop a novel high-performance visible light bismuth oxide photocatalyst.
In order to realize the purpose of the invention, the technical scheme is as follows:
the preparation method of the bismuth oxide photocatalyst with the two-dimensional structure comprises the following steps:
(1) Weighing polyether, placing the polyether in an absolute ethyl alcohol-ethylene glycol mixed solvent, and magnetically stirring to obtain a uniform polyether alcoholic solution;
(2) Adding carboxylic acid into the polyether alcoholic solution obtained in the step (1), and magnetically stirring to dissolve the carboxylic acid;
(3) Adding a bismuth-containing compound into the solution obtained in the step (2), and carrying out ultrasonic treatment and stirring until the bismuth-containing compound is completely dissolved;
(4) And (4) transferring the solution obtained in the step (3) into a reaction kettle, carrying out solvothermal reaction, washing reaction products with deionized water and ethanol respectively, centrifuging and drying to obtain the bismuth oxide nanosheet photocatalyst.
In the step (1), the polyether is selected from PEO-PPO-PEO (p 123) (Ma = 5800) nonionic surfactant, and the addition amount is 0.3 to 0.5g.
In the step (1), the volume ratio of the absolute ethyl alcohol to the ethylene glycol is (2) - (1).
The carboxylic acid in the step (2) is selected from one of oxalic acid and glacial acetic acid.
Adding carboxylic acid to adjust the pH of the solution = 4~5 in step (2).
In the step (3), the bismuth-containing compound is Bi (NO) 3 ) 3 ·5H 2 O, the adding amount is 2 mmol, ultrasonic dispersion is carried out for 0.5 h, and stirring is carried out for 1h.
The solvent thermal reaction conditions in the step (4) are as follows: transferring the 80 ml solution into a 100 ml reaction kettle, and keeping the temperature at 160-180 ℃ for 8-12 h.
The centrifugation conditions in the step (4) are as follows: the centrifugation speed is 4000 rpm, the centrifugation time is 5 min, and deionized water and absolute ethyl alcohol are respectively adopted for washing 3 times. The drying conditions were: the temperature is 60 ℃ and the time is 24h.
The invention has the following principle or innovation points:
the invention provides a preparation method of a novel bismuth oxide photocatalyst with a two-dimensional structure. Bismuth nitrate is used as a precursor, ethylene glycol/ethanol mixed solution is used as a reaction medium, carboxylic acid is used for adjusting the pH value of the solution, preferably triblock compound is used as a morphology control agent of a bismuth oxide semiconductor, and a solvothermal method is adopted to prepare the efficient bismuth oxide photocatalyst with a two-dimensional sheet structure. According to the invention, the thickness of the two-dimensional bismuth oxide nanosheet is regulated and controlled by controlling the synthesis conditions (template agent, pH and solvent), and compared with other existing preparation methods of bismuth oxide, the method has more remarkable visible light catalytic activity and chemical stability, and is suitable for large-scale application in the field of photocatalysis; the photocatalyst has the advantages of easily available raw materials, low preparation cost and simple and convenient preparation method, and solves the technical problems of high synthesis cost, complicated steps and inconvenience for mass synthesis in the prior art.
The invention has the advantages that: the nano-sheet bismuth oxide photocatalyst is prepared by a template method, the preparation method is simple and convenient, the cost is low, the purity reaches more than 99.8 percent, the appearance is uniform, the dispersibility is good, and the performance is stable. The bismuth oxide with the two-dimensional structure prepared by the invention is flaky, has high solar energy utilization rate, high quantum efficiency and high photocatalytic activity, and can be applied to the degradation of catalytic organic pollutants in the environmental field.
Drawings
FIG. 1 is a Scanning Electron Micrograph (SEM) (a) and a Transmission Electron Micrograph (TEM) (b) of a bismuth oxide material prepared according to the present invention.
Fig. 2 is an X-ray electron diffraction (XRD) pattern of the bismuth oxide material prepared in accordance with the present invention.
FIG. 3 shows Bi 2 O 3 Atomic force microscope and nanosheet of sampleThickness profile, wherein, a, b- -Bi 2 O 3 (Solvothermal + p 123), c, d- -Bi 2 O 3 (solvothermal).
FIG. 4 is a graph showing that the bismuth oxide material prepared by the invention is used as a photocatalyst to catalyze degradation of rhodamine B.
FIG. 5 is a graph showing the degradation curve of rhodamine B catalyzed by the bismuth oxide and carbon nitride composite material prepared by the invention.
Detailed Description
To better illustrate the invention, the examples are as follows:
example 1
Under the condition of stirring, 0.5g of P123 is added into a mixed solution of 80 mL glycol and absolute ethyl alcohol (the volume ratio of the two is 2:1), the mixed solution is stirred and dissolved, then 2 mmol of bismuth nitrate pentahydrate is added, the mixed solution is stirred, the pH value of the solution is adjusted to 4-5 by oxalic acid, and the mixed solution is obtained after 1 hour of stirring. The mixed solution was transferred to an autoclave and kept at 160 ℃ for 8 hours for solvothermal reaction. After the reaction is finished, cooling to room temperature, centrifuging to obtain a precipitate, washing with distilled water, and drying 24h at 60 ℃ to obtain the bismuth oxide nano material with the purity of 99.8%. From the electron microscope topography (fig. 1) of the material, it can be seen that the bismuth oxide is in the form of nano-platelets.
Example 2
Under the stirring condition, 0.3g of EO20PO70EO20 (Ma = 5800) is added into a mixed solution of 80 mL ethylene glycol and absolute ethyl alcohol (the volume ratio of the two is 4:1), the mixed solution is stirred and dissolved, 2 mmol of bismuth nitrate pentahydrate is added, the mixed solution is stirred and is used for adjusting the pH value of the solution to 4-5 (glacial acetic acid), the mixed solution is stirred for 1h, the mixed solution is transferred into an autoclave, 10 h is kept under the condition of 160 ℃ for carrying out solvothermal reaction, after the reaction is finished, the mixed solution is cooled to room temperature, precipitates are centrifugally taken, the precipitates are washed by distilled water, 24h is dried under the condition of 60 ℃ to obtain 99.8% of bismuth oxide nano materials, the bismuth oxide nano materials are in a nano-sheet shape, the bismuth oxide is in a nano-sheet shape, the material is in a pure beta-phase, and the bismuth oxide prepared by an Atomic Force Microscope (AFM) analysis result (3) of the material, and the two nano-sheet thickness can be obtained by the method.
Application example 1
In the photocatalytic degradation experiment, the absorption spectrum of rhodamine B (RhB) in a solution is measured by using an ultraviolet-visible spectrophotometer. And measuring the change of the concentration of rhodamine B in the solution by using the change of the absorbance. DrawingC/C 0 With respect to timetCurve of (1), whereinC 0 Is the initial concentration of RhB and,Cfor a period of time after light irradiationtMeasured RhB concentration values after.
The specific experimental steps are as follows: 0.025g of the bismuth oxide photocatalyst prepared according to the present invention was weighed. Adding 50 mL with concentration of 1 × 10 -5 And (3) in mg/L RhB solution, stirring for 30 min in the dark, then reacting under visible light, sampling at 20 min intervals, centrifuging, and taking supernatant to detect by a spectrophotometer. As can be seen from fig. 4, the photocatalytic activity of the material is significantly greater than that of common commercial bismuth oxide. When the light reaction is carried out for 120 minutes, the bismuth oxide nano-sheets can catalyze and degrade over 70% of RhB, while the common commercial bismuth oxide can catalyze and degrade only about 15%. The research results show that the thickness of the bismuth oxide nanosheet has obvious positive correlation with the photocatalytic activity thereof, and the photocatalytic activity of the two-dimensional bismuth oxide nanomaterial prepared by the method is superior to that of bismuth oxide before modification. The carbon nitride/bismuth oxide composite photocatalyst formed by compounding the bismuth oxide nanosheets and the carbon nitride prepared by the method disclosed by the invention is excellent in degradation performance, and the degradation rate of RhB reaches more than 95% in 40 minutes under the irradiation of visible light, as shown in figure 5.
Claims (2)
1. A preparation method of a bismuth oxide photocatalyst with a two-dimensional structure is characterized by comprising the following steps:
(1) Weighing polyether, placing the polyether in an absolute ethyl alcohol-ethylene glycol mixed solvent, and magnetically stirring to obtain an alcoholic solution of the polyether;
(2) Adding carboxylic acid into the polyether alcoholic solution obtained in the step (1), and magnetically stirring to dissolve the carboxylic acid;
(3) Adding a bismuth-containing compound into the solution obtained in the step (2), and carrying out ultrasonic treatment and stirring until the bismuth-containing compound is completely dissolved;
(4) Transferring the solution obtained in the step (3) into a reaction kettle, carrying out solvothermal reaction, washing reaction products with deionized water and ethanol respectively, centrifuging and drying to obtain a bismuth oxide photocatalyst;
the bismuth-containing compound is Bi (NO) 3 ) 3 ·5H 2 O；
The carboxylic acid is selected from one of oxalic acid and glacial acetic acid;
the polyether is selected from: polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymers (PEO-PPO-PEO);
the volume ratio of the absolute ethyl alcohol to the ethylene glycol in the step (1) is 2 to 1;
adding carboxylic acid to adjust the pH of the solution = 4~5 in step (2).
2. The method for preparing a bismuth oxide photocatalyst with a two-dimensional structure according to claim 1, wherein the solvothermal reaction conditions in the step (4) are as follows: and transferring the 80 ml solution into a 100 ml reaction kettle, wherein the reaction temperature is 160-180 ℃, and the constant temperature time is 8-12 h.
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| CN103466702A (en) * | 2013-09-27 | 2013-12-25 | 武汉工程大学 | Method for preparing porous bismuth oxide nano-material without template |
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