CN112473651A - Graphene aerogel with photocatalytic activity and preparation method thereof - Google Patents
Graphene aerogel with photocatalytic activity and preparation method thereof Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000004964 aerogel Substances 0.000 title claims abstract description 53
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 27
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910020350 Na2WO4 Inorganic materials 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
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- 238000002791 soaking Methods 0.000 claims description 7
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 9
- 238000005215 recombination Methods 0.000 abstract description 4
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- 238000000926 separation method Methods 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 21
- 229960000907 methylthioninium chloride Drugs 0.000 description 21
- 239000000463 material Substances 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
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- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
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- 230000008859 change Effects 0.000 description 2
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- 230000007423 decrease Effects 0.000 description 2
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- 238000005286 illumination Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- UMPSXRYVXUPCOS-UHFFFAOYSA-N 2,3-dichlorophenol Chemical compound OC1=CC=CC(Cl)=C1Cl UMPSXRYVXUPCOS-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229910002115 bismuth titanate Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-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
- 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- 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
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- 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
- B01J37/32—Freeze drying, i.e. lyophilisation
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the field of graphene preparation and application, and particularly relates to a graphene aerogel with photocatalytic activity and a preparation method thereofPreparing a method; the composite material is prepared from graphene with a three-dimensional porous structure and Bi loaded on the surface of the graphene2WO6Micron particle composition; wherein, Bi2WO6The diameter of the micron particles is 3-5 μm. The preparation method comprises the following steps: first Bi (NO)3)3Uniformly mixing the solution with the graphene oxide solution, and further mixing the solution with Na2WO4Mixing and carrying out hydrothermal reaction to prepare the bismuth tungstate-graphene composite material. The bismuth tungstate-graphene composite material has the advantages of large specific surface area, band gap reaching 2.96eV, strong absorption on visible light, capability of effectively improving the separation of photon-generated carriers and reducing the recombination rate of the carriers, and more excellent photocatalytic performance compared with a single phase. Moreover, the method is novel, uniform in particles, low in equipment operation requirement, simple in process and easy to control process conditions.
Description
Technical Field
The invention belongs to the field of graphene preparation and application, and particularly relates to a graphene aerogel with photocatalytic activity and a preparation method thereof.
Background
Energy shortage and environmental pollution are urgent problems to be solved for realizing social sustainable development. Among various pollution treatment technologies, the visible light catalysis technology can directly utilize visible light to degrade and even mineralize pollutants, and has good application prospects in the aspects of environmental protection and new energy development. Among them, bismuth-based visible light photocatalysts have attracted great interest to researchers due to their unique electronic structures and excellent visible light absorption capabilities. Common bismuth-based photocatalysts include bismuth oxide, bismuth titanate, bismuth vanadate, bismuth molybdate, bismuth tungstate, bismuth ferrite and the like. Wherein bismuth tungstate (Bi)2WO6) As an excellent n-type semiconductor functional material, the material has narrow band gap energy, can absorb visible light, has stable photochemical property and is environment-friendly, and is widely used in the field of environmental catalysis.
In Bi2WO6During the research process of the material, researchers find that single Bi2WO6The nano material has narrow spectral response range (<450nm), too fast of the recombination speed of the photo-generated electron and hole, and the like, thereby carrying out a great deal of Bi-based2WO6And (5) research of materials. Researches show that the visible light catalysis performance of the semiconductor can be improved by compounding the graphene and the semiconductor photocatalysis material. If the photocatalytic performance is greatly improved after the bismuth ferrite and the graphene are compounded, the graphite is shownThe recombination of the alkene can improve the recombination effect between the photo-generated electrons and the holes of the raw materials, so that the photo-generated electrons and the holes can be better separated. In addition, the large specific surface area of the graphene improves the adsorption performance, and the visible light catalytic performance of the material can be further improved.
Therefore, the bismuth ferrite-graphene composite aerogel is prepared by combining the respective advantages of bismuth tungstate and graphene materials and utilizing a simple and easily-controlled one-step hydrothermal method. The aerogel is used for visible light catalytic degradation of methylene blue, can obtain good catalytic degradation effect, and has important significance for development of visible light catalytic technology.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the technical problem, a graphene aerogel with photocatalytic activity is provided.
The technical scheme of the invention is as follows: the graphene aerogel with photocatalytic activity is characterized in that the mass fraction of bismuth tungstate in the graphene aerogel is 70-95%, and the mass fraction of graphene is 5-30%.
The graphene aerogel is prepared by the following steps:
(1) adding Bi (NO)3)3Dissolving in glycol, and performing ultrasonic treatment;
(2) dispersing graphene oxide in deionized water by adopting ultrasonic treatment;
(3) adding the solution prepared in the step (1) into the solution prepared in the step (2), and stirring and mixing;
(4) adding Na into the solution prepared in the step (3)2WO4Continuously stirring and mixing, and transferring to a reaction kettle for hydrothermal reaction;
(5) and (5) soaking and cleaning the product obtained in the step (4) by using deionized water, and freeze-drying to obtain the graphene aerogel.
In step (1), Bi (NO)3)3The concentration is 0.001-0.2M, and the ultrasonic treatment time is 10-30 min;
in the step (2), the concentration of the graphene oxide solution is 1-20 g/L, and the ultrasonic treatment time is 30-60 min;
the stirring time in the step (3) is 15-30 min;
bi (NO) in step (4)3)3With Na2WO4The molar ratio of (1) to (2), continuously stirring and mixing for 15-30 min, and carrying out hydrothermal reaction in a reaction kettle at 180-200 ℃ for 24 h;
soaking and cleaning for 2-3 days in the step (5), and freeze-drying for 60-72 hours at-30 ℃.
The graphene aerogel prepared by the preparation method is used for treating pollutants in the environment.
The beneficial effects of the invention are as follows: the invention provides a preparation method for synthesizing bismuth tungstate-graphene composite aerogel, which can synthesize graphene aerogel with photocatalytic activity in one step and simultaneously complete reduction of graphene oxide and compounding of bismuth tungstate-graphene. The obtained aerogel is used for visible light catalytic degradation of methylene blue and dichlorophenol, and has excellent catalytic activity.
Drawings
Fig. 1 is an X-ray diffraction pattern (XRD) of bismuth tungstate-graphene composite aerogel having different graphene contents according to examples 1, 2, and 3 of the present invention from comparative example 1. (a is comparative example 1 Bi)2WO6(ii) a b is example 1Bi2WO6-10% graphene aerogel; c is example 2Bi2WO6-20% graphene aerogel; d is example 3Bi2WO6-30% graphene aerogel)
FIG. 2 shows Bi in example 2 of the present invention2WO6-visible light catalysis effect diagram of 20% graphene on methylene blue.
Fig. 3 is a comparison of the visible light catalytic effects of the bismuth tungstate-graphene composite aerogel with different graphene contents in examples 1, 2 and 3 of the present invention and comparative example 1 on methylene blue.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1: bi2WO6Preparation of-10% graphene aerogel
(1) 0.5mmol of Bi (NO)3)3Dissolving in 20ml ethylene glycol, and performing ultrasonic treatment for 10 min;
(2) dispersing graphene oxide in deionized water to prepare 20mL of solution with the concentration of 1g/L, and carrying out ultrasonic treatment for 40 min;
(3) adding the solution prepared in the step (1) into the solution prepared in the step (2), and stirring and mixing for 15 min;
(4) adding 0.25mmol of Na into (3)2WO4Continuously stirring and mixing for 15min, transferring to a reaction kettle for hydrothermal reaction under the conditions of 180 ℃ and 24 h;
(5) and (5) soaking and cleaning the product obtained in the step (4) by using deionized water for 3 days, and freeze-drying at-30 ℃ for 72 hours to obtain the graphene aerogel.
(6) The prepared bismuth tungstate-graphene aerogel is used as a photocatalyst, and methylene blue can be degraded by visible light catalysis. The initial concentration of methylene blue was 40mg/L, the aerogel loading was 0.5g/L, and the temperature was 25 ℃.
As can be seen from the XRD test result in FIG. 1b, Bi is contained in the bismuth tungstate-graphene aerogel prepared by the one-step hydrothermal method2WO6. The characteristic peak of the graphene oxide completely disappears, which indicates that the graphene oxide is completely reduced in the hydrothermal process, and the material is Bi2WO6-10% graphene aerogel.
Adding Bi2WO6The-10% graphene aerogel has a good effect when used for catalyzing methylene blue by visible light. As can be seen from FIG. 2, the concentration of methylene blue continuously decreases with the increase of illumination time, and the removal efficiency of methylene blue is 65% after 3h of photocatalysis.
Comparative example 1: single phaseBi2WO6Preparation of
Compared with the example 1, the single-phase bismuth tungstate material is prepared by other steps like the example 1 without adding graphene oxide in the preparation process. From the XRD test result in FIG. 1a, it is known that the prepared bismuth tungstate is Bi2WO6。
As can be seen from FIG. 2, Bi is a single phase2WO6The photocatalytic activity of the catalyst is relatively weak, and the removal efficiency of methylene blue is 31 percent after 3 hours of photocatalysis.
Example 2: bi2WO6Preparation of-20% graphene aerogel
(1) 0.5mmol of Bi (NO)3)3Dissolving in 20ml ethylene glycol, and performing ultrasonic treatment for 10 min;
(2) dispersing graphene oxide in deionized water to prepare 10mL of solution with the concentration of 5g/L, and carrying out ultrasonic treatment for 40 min;
(3) adding the solution prepared in the step (1) into the solution prepared in the step (2), and stirring and mixing for 15 min;
(4) adding 0.25mmol of Na into (3)2WO4Continuously stirring and mixing for 15min, transferring to a reaction kettle for hydrothermal reaction under the conditions of 180 ℃ and 24 h;
(5) and (5) soaking and cleaning the product obtained in the step (4) by using deionized water for 3 days, and freeze-drying at-30 ℃ for 72 hours to obtain the graphene aerogel.
(6) The prepared bismuth tungstate-graphene aerogel is used as a photocatalyst, and methylene blue can be degraded by visible light catalysis. The initial concentration of methylene blue was 40mg/L, the aerogel loading was 0.5g/L, and the temperature was 25 ℃.
As can be seen from the XRD test result in FIG. 1c, Bi is contained in the bismuth tungstate-graphene aerogel prepared by the one-step hydrothermal method2WO6Consistent with the results of example 1. Therefore, the crystal structure of bismuth ferrite in the aerogel cannot be influenced by the change of the addition amount of the graphene.
Adding Bi2WO6-20% graphene aerogel for visible light catalyzed methylene blue degradation. As can be seen from FIG. 2, the concentration of methylene blue continuously decreases with the increase of illumination time, and the removal efficiency of methylene blue is 73% after 3h of photocatalysis. Can be used forThe increase of the content of graphene in the composite aerogel is beneficial to the degradation of methylene blue.
Example 3: bi2WO6Preparation of-30% graphene aerogel
(1) 0.5mmol of Bi (NO)3)3Dissolving in 20ml ethylene glycol, and performing ultrasonic treatment for 10 min;
(2) dispersing graphene oxide in deionized water to prepare 5mL of solution with the concentration of 17g/L, and carrying out ultrasonic treatment for 40 min;
(3) adding the solution prepared in the step (1) into the solution prepared in the step (2), and stirring and mixing for 15 min;
(4) adding 0.25mmol of Na into (3)2WO4Continuously stirring and mixing for 15min, transferring to a reaction kettle for hydrothermal reaction under the conditions of 180 ℃ and 24 h;
(5) and (5) soaking and cleaning the product obtained in the step (4) by using deionized water for 3 days, and freeze-drying at-30 ℃ for 72 hours to obtain the graphene aerogel.
(6) The prepared bismuth tungstate-graphene aerogel is used as a photocatalyst, and methylene blue can be degraded by visible light catalysis. The initial concentration of methylene blue was 40mg/L, the aerogel loading was 0.5g/L, and the temperature was 25 ℃.
As can be seen from the XRD test result in FIG. 1b, Bi is contained in the bismuth tungstate-graphene aerogel prepared by the one-step hydrothermal method2WO6Consistent with the results of example 1. Therefore, the crystal structure of bismuth ferrite in the aerogel cannot be influenced by the change of the addition amount of the graphene.
Adding Bi2WO6-30% graphene aerogel for visible light catalyzed methylene blue degradation. As can be seen from fig. 3, the removal efficiency of methylene blue after 3 hours of photocatalysis was 97%, which was higher than that of examples 1 and 2. Therefore, the further increase of the graphene content in the composite aerogel is still beneficial to the degradation of methylene blue.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The graphene aerogel with photocatalytic activity is characterized in that the mass fraction of bismuth tungstate in the graphene aerogel is 70-95%, and the mass fraction of graphene is 5-30%.
2. The method for preparing graphene aerogel having photocatalytic activity according to claim 1, comprising the steps of:
(1) adding Bi (NO)3)3Dissolving in glycol, and performing ultrasonic treatment;
(2) dispersing graphene oxide in deionized water by adopting ultrasonic treatment;
(3) adding the solution prepared in the step (1) into the solution prepared in the step (2), and stirring and mixing;
(4) adding Na into the solution prepared in the step (3)2WO4Continuously stirring and mixing, and transferring to a reaction kettle for hydrothermal reaction;
(5) and (5) soaking and cleaning the product obtained in the step (4) by using deionized water, and freeze-drying to obtain the graphene aerogel.
3. The method for preparing graphene aerogel having photocatalytic activity according to claim 1, wherein Bi (NO) is used in step (1)3)3The concentration is 0.001-0.2M, and the ultrasonic treatment time is 10-30 min.
4. The preparation method of the graphene aerogel with photocatalytic activity according to claim 1, wherein the concentration of the graphene oxide solution in the step (2) is 1-20 g/L, and the ultrasonic treatment time is 30-60 min.
5. The preparation method of the graphene aerogel with photocatalytic activity according to claim 1, wherein the stirring time in the step (3) is 15-30 min.
6. The method for preparing graphene aerogel having photocatalytic activity according to claim 1, wherein Bi (NO) is used in step (4)3)3With Na2WO4The molar ratio of (1) to (2), continuously stirring and mixing for 15-30 min, and carrying out hydrothermal reaction in a reaction kettle at 180-200 ℃ for 24 h.
7. The method for preparing graphene aerogel with photocatalytic activity according to claim 1, wherein the soaking and cleaning in step (5) is performed for 2 to 3 days.
8. The preparation method of the graphene aerogel with photocatalytic activity according to claim 1, wherein the freeze drying in the step (5) is performed for 60-72 hours at-30 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626634A (en) * | 2012-03-30 | 2012-08-08 | 南京理工大学 | Bismuth ferrite-graphene compounding magnetism visible light catalyst, as well as preparation method and application of same |
| CN106512987A (en) * | 2016-11-24 | 2017-03-22 | 河南师范大学 | Ismuth tungstate/graphene aerogel compound visible-light-induced photocatalyst and preparation method thereof |
| CN108579727A (en) * | 2018-01-11 | 2018-09-28 | 湘潭大学 | A kind of graphene quantum dot-bismuth tungstate composite photocatalyst and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626634A (en) * | 2012-03-30 | 2012-08-08 | 南京理工大学 | Bismuth ferrite-graphene compounding magnetism visible light catalyst, as well as preparation method and application of same |
| CN106512987A (en) * | 2016-11-24 | 2017-03-22 | 河南师范大学 | Ismuth tungstate/graphene aerogel compound visible-light-induced photocatalyst and preparation method thereof |
| CN108579727A (en) * | 2018-01-11 | 2018-09-28 | 湘潭大学 | A kind of graphene quantum dot-bismuth tungstate composite photocatalyst and preparation method thereof |
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Application publication date: 20210312 |