CN112973743A - BC/Bi4O5Br2Preparation method of composite photocatalytic material - Google Patents
BC/Bi4O5Br2Preparation method of composite photocatalytic material Download PDFInfo
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- CN112973743A CN112973743A CN202110248026.8A CN202110248026A CN112973743A CN 112973743 A CN112973743 A CN 112973743A CN 202110248026 A CN202110248026 A CN 202110248026A CN 112973743 A CN112973743 A CN 112973743A
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- composite photocatalytic
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 16
- 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 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract 2
- 239000002244 precipitate Substances 0.000 claims description 15
- 238000003760 magnetic stirring Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 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 abstract description 7
- 229940043267 rhodamine b Drugs 0.000 abstract description 7
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 abstract description 6
- 229960004989 tetracycline hydrochloride Drugs 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000031700 light absorption Effects 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229910052724 xenon Inorganic materials 0.000 abstract description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007810 chemical reaction solvent Substances 0.000 abstract 1
- 238000011056 performance test Methods 0.000 abstract 1
- 238000003911 water pollution Methods 0.000 abstract 1
- 229910052797 bismuth Inorganic materials 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 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 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
Classifications
-
- 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
-
- B01J35/39—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
-
- 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
- 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
- C02F2101/36—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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention provides BC/Bi4O5Br2The preparation method of the composite photocatalytic material comprises the steps of preparing BC/Bi by using bismuth nitrate pentahydrate, BC and potassium bromide as raw materials and ethylene glycol as a reaction solvent through a simple and easily-operated room-temperature precipitation method4O5Br2Composite photocatalytic materialAnd (5) feeding. Using xenon lamp as light source, passing light of low wavelength (lambda) through filter<420nm) filtering off, and p-BC/Bi4O5Br2And carrying out a photocatalytic performance test on the composite photocatalytic material. Degradation of rhodamine B and tetracycline hydrochloride is carried out, and degradation rates of rhodamine B and tetracycline hydrochloride are used for representing BC/Bi4O5Br2The photocatalytic performance of the composite photocatalytic material. The material has the advantages of high chemical stability, large specific surface area, unique electronic structure, strong light absorption capacity and the like, so that the material has wide application prospect in the aspect of water pollution treatment.
Description
Technical Field
The invention belongs to the field of preparation of photocatalytic materials, and particularly relates to BC/Bi4O5Br2A preparation method of a composite photocatalytic material.
Background
In sewage treatment, photocatalytic oxidation is a novel advanced oxidation technology, is developed on the basis of photochemical oxidation, has strong oxidation capability and no secondary pollution, can be carried out at normal temperature and normal pressure, and has the characteristics of environmental protection, energy conservation and the like.
Bismuth-based semiconductors are a unique new class of photocatalytic materials that have been developed in recent years. Due to the special structure of Bi atoms, the compound can easily form a layered structure, and a bismuth-based compound with visible light response capability is generated. Wherein Bi is in the bismuth-rich halide material4O5Br2The organic light-emitting diode has attracted attention due to high chemical stability, large specific surface area, unique electronic structure and high light absorption capacity, and researches show that the organic light-emitting diode has excellent performance in the degradation aspect of organic matters.
Biochar (BC) is a carbon material that has been extensively studied in recent years and is produced by carbonizing wood, straw, grass, fallen leaves or other agricultural waste by pyrolysis under low oxygen and relatively low temperature conditions. It not only has a large number of pore channel structures and larger specific surface area, but also has good adsorption property when being compounded with the catalystThe conductivity, combined with the catalyst, can be used as an electron acceptor to conduct electrons in time so as to improve the separation efficiency of electron-hole pairs. Therefore, it is considered that Bi4O5Br2The high-efficiency photocatalyst can be prepared by compounding with a ZSM-5 zeolite molecular sieve.
Disclosure of Invention
The invention aims to provide BC/Bi4O5Br2A preparation method of a composite photocatalytic material is used for solving the environmental problem.
The method comprises the following specific steps:
(1) dissolving bismuth nitrate pentahydrate in ethylene glycol, adding BC under stirring, performing ultrasonic treatment, performing magnetic stirring, and adding potassium bromide to perform magnetic stirring until the potassium bromide is dissolved;
(2) sequentially and slowly adding ultrapure water and ammonia monohydrate into the solution obtained in the step (1), and magnetically stirring;
(3) filtering the reaction solution obtained in the step (2), collecting precipitate, and washing the precipitate;
(4) drying the precipitate obtained in the step (3), and grinding to obtain BC/Bi4O5Br2A composite photocatalytic material.
Preferably, the magnetic stirring time in the step (1) is 30min, and the ultrasonic time is 30 min.
Preferably, the magnetic stirring time of the step (2) is 6 h.
Preferably, the oven drying time is 12 h.
Preferably, the ratio of activated carbon BC: bi4O5Br2The mass fraction ratio is 0.75: 100. 1.5: 100. 5: 100, calculating.
Preparation of BC/Bi as described above4O5Br2The composite photocatalytic material can be used in the field of sewage treatment. The material is a composite of active carbon and a bismuth oxyhalide semiconductor, the existence of the active carbon improves the adsorption performance of the catalyst, and the active carbon is used as an electron acceptor to conduct electrons in time and improve the separation efficiency of electron-hole pairs. The composite photocatalytic material has strong oxidizing ability, no secondary pollution, can be carried out at normal temperature and normal pressure, has the characteristics of economy, environmental protection, energy conservation and the like, and is used for solving the problems of low cost and high costProvides a way to solve the environmental problem.
The method has the advantages that:
(1) the BC/Bi is prepared by a simple ultrasonic-assisted room temperature in-situ precipitation method4O5Br2The composite photocatalytic material is simple and easy to operate;
(2) prepared BC/Bi4O5Br2The composite photocatalytic material has the performance of effectively degrading rhodamine B (RhB) and tetracycline hydrochloride (TC) under visible light;
(3) prepared BC/Bi4O5Br2The composite photocatalytic material has better circulation stability, and the problem that the photocatalytic efficiency of the material is greatly reduced after primary photocatalysis is avoided;
(4) the application is simple, and only the prepared BC/Bi is needed4O5Br2The composite photocatalytic material powder is put into RhB or TC with a certain concentration, and degradation of RhB or TC can be carried out under visible light.
Drawings
FIG. 1: BC/Bi4O5Br2C/C of composite photocatalytic material for degrading RhB0Graph (a) and kinetic fit graph (b);
FIG. 2: BC/Bi4O5Br2C/C of composite photocatalytic material for degrading TC0Graph (a) and removal rate graph (b);
FIG. 3: BC/Bi4O5Br2SEM picture of the composite photocatalytic material;
FIG. 4: BC/Bi4O5Br2XRD spectrogram of the composite photocatalytic material;
FIG. 5: BC/Bi4O5Br2Nitrogen adsorption-desorption isotherms of the composite photocatalytic material;
FIG. 6: BC/Bi4O5Br2XPS full spectrum of the composite photocatalytic material;
FIG. 7: BC/Bi4O5Br2An ultraviolet-visible diffuse reflection spectrogram (a) and a forbidden band width chart (b) of the composite photocatalytic material;
FIG. 8:BC/Bi4O5Br2a Raman spectrogram of the composite photocatalytic material;
FIG. 9: BC/Bi4O5Br2PL profile of the composite photocatalytic material;
FIG. 10: BC/Bi4O5Br2A photocurrent response graph of the composite photocatalytic material;
FIG. 11: BC/Bi4O5Br2EIS diagram of composite photocatalytic material.
Detailed Description
The present invention is further described in detail with reference to the following specific examples 1-5, which are intended to be illustrative, but not limiting, of the invention.
Example 1:
BC/Bi was prepared as follows4O5Br2The composite photocatalytic material is as follows:
(1) dissolving 2.425g of bismuth nitrate pentahydrate in 20mL of ethylene glycol, adding 0.0182g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate pentahydrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 0.75 BC/BOB.
Example 2:
(1) dissolving 2.425g of pentahydrate bismuth nitrate in 20mL of ethylene glycol, adding 0.0364g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, and then adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 1.5 BC/BOB.
Example 3:
(1) dissolving 2.425g of pentahydrate bismuth nitrate in 20mL of ethylene glycol, adding 0.1213g of BC under stirring, carrying out ultrasonic treatment for 30min, then carrying out magnetic stirring for 30min, and then adding 0.595g of potassium bromide, and carrying out magnetic stirring for 30min until the bismuth nitrate is dissolved;
(2) slowly adding 8mL of ultrapure water and 2mL of ammonia monohydrate into the solution obtained in the step (1) in sequence, and magnetically stirring for 6 h;
(3) carrying out vacuum filtration on the reaction liquid obtained in the step (2), collecting precipitates, and sequentially washing the precipitates for 3 times by using ultrapure water and absolute ethyl alcohol in turn;
(4) drying the precipitate obtained in the step (3) in an oven at 60 ℃ for 12h, and grinding to obtain BC/Bi4O5Br2The composite photocatalytic material is marked as 5 BC/BOB.
Under the irradiation of a xenon lamp, light below 420nm is filtered by using a filter plate, and the photocatalytic performance of the material is characterized by using the degradation efficiency of RhB and BPA.
Doping of BC increases Bi4O5Br2The specific surface area of the photocatalytic material enhances the adsorption performance of the catalyst, and the BC is used as an electron acceptor to conduct electrons in time, so that the separation efficiency of electron-hole pairs is improved. Cause BC/Bi4O5Br2The composite photocatalytic material shows better photocatalytic activity in a visible light area, so that organic pollutants can be efficiently degraded.
Claims (7)
1. BC/Bi4O5Br2The preparation method of the composite photocatalytic material is characterized by comprising the following specific steps:
(1) dissolving bismuth nitrate pentahydrate in ethylene glycol, adding BC under stirring, performing ultrasonic treatment, performing magnetic stirring, and adding potassium bromide to perform magnetic stirring until the potassium bromide is dissolved;
(2) sequentially and slowly adding ultrapure water and ammonia monohydrate into the solution obtained in the step (1), and magnetically stirring;
(3) filtering the reaction solution obtained in the step (2), collecting precipitate, and washing the precipitate;
(4) drying the precipitate obtained in the step (3), and grinding to obtain BC/Bi4O5Br2A composite photocatalytic material.
2. The method of claim 1, wherein: the magnetic stirring time in the step (1) is 30min, and the ultrasonic time is 30 min.
3. The method of claim 1, wherein: the magnetic stirring time in the step (2) is 6 h.
4. The method of claim 1, wherein: the drying time of the oven is 12 h.
5. The method of claim 1, wherein: the added raw materials comprise activated carbon BC: bi4O5Br2The mass fraction ratio is 0.75: 100. 1.5: 100. 5: 100, calculating.
6. BC/Bi obtained by the method of claim 14O5Br2A composite photocatalytic material.
7. BC/Bi obtained by the method of claim 14O5Br2The composite photocatalytic material is applied to the field of sewage treatment.
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Cited By (1)
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CN115634702A (en) * | 2021-07-20 | 2023-01-24 | 南昌航空大学 | Bismuth oxycarbonate/biochar composite photocatalyst and preparation method and application thereof |
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