LU503921B1 - Visible light photocatalyst for in-situ synthesis of hydrogen peroxide and preparation method and application thereof - Google Patents
Visible light photocatalyst for in-situ synthesis of hydrogen peroxide and preparation method and application thereof Download PDFInfo
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- LU503921B1 LU503921B1 LU503921A LU503921A LU503921B1 LU 503921 B1 LU503921 B1 LU 503921B1 LU 503921 A LU503921 A LU 503921A LU 503921 A LU503921 A LU 503921A LU 503921 B1 LU503921 B1 LU 503921B1
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- visible light
- hydrogen peroxide
- organic polymer
- covalent organic
- light photocatalyst
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 66
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 34
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 32
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920000620 organic polymer Polymers 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 239000013310 covalent-organic framework Substances 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000005470 impregnation Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 9
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 claims description 9
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 claims description 9
- 238000004659 sterilization and disinfection Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000010942 self-nucleation Methods 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 3
- 239000010931 gold Substances 0.000 description 28
- 230000008569 process Effects 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000009303 advanced oxidation process reaction Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 244000052616 bacterial pathogen Species 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 208000025721 COVID-19 Diseases 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 208000019331 Foodborne disease Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004904 UV filter Substances 0.000 description 1
- 208000034817 Waterborne disease Diseases 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- FFGPTBGBLSHEPO-UHFFFAOYSA-N carbamazepine Chemical compound C1=CC2=CC=CC=C2N(C(=O)N)C2=CC=CC=C21 FFGPTBGBLSHEPO-UHFFFAOYSA-N 0.000 description 1
- 229960000623 carbamazepine Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 1
- 229940006461 iodide ion Drugs 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012029 structural testing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
- B01J35/45—Nanoparticles
-
- 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
- B01J37/0201—Impregnation
-
- 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
- B01J37/16—Reducing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/027—Preparation from water
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0244—Nitrogen containing compounds with nitrogen contained as ring member in aromatic compounds or moieties, e.g. pyridine
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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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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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
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- Hydrology & Water Resources (AREA)
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The present invention discloses visible light photocatalyst for in-situ synthesis of hydrogen peroxide and preparation method and application thereof, which belongs to the technical field of photocatalytic material preparation; according to the invention, a wet impregnation method is adopted, and covalent organic polymer is impregnated with chloroauric acid, so that the chloroauric acid is uniformly distributed on an inner surface of the covalent organic polymer, thereby assisting the reduction of sodium borohydride to prepare Au nanoparticles to be loaded on the covalent organic polymer to synthesize Au-loaded covalent organic polymer (Au/COFs) visible light photocatalyst; the present photocatalyst can significantly improve the absorption capacity of visible light and has good visible light photoresponse and excellent photocatalytic performance, and can efficiently reduce oxygen to hydrogen peroxide in situ under visible light; the present photocatalyst can be applied in the field of sustainable development environment and clean production.
Description
DESCRIPTION LU503921
Visible light photocatalyst for in-situ synthesis of hydrogen peroxide and preparation method and application thereof
The present invention belongs to the technical field of photocatalytic material preparation, in particular to visible light photocatalyst for in-situ synthesis of hydrogen peroxide and preparation method and application thereof.
As the COVID-19 seriously endangers people's life, people pay more and more attention to the harm caused by microorganisms. Waterborne and foodborne diseases caused by pathogenic microorganisms have become worldwide problems. The main sources of these microorganisms are house lives, hospitals, agriculture and industrial production. Disinfection is an essential step in the water treatment industry to avoid the spread of pathogenic bacteria and associated diseases.
Although there are already many methods that can solve the problem of treatment of microorganisms in water, the traditional technologies are somewhat too complicated, inefficient and sometimes subject to influence by the environment, and even cause secondary pollution to the environment.
The in situ synthesis of hydrogen peroxide by photocatalysis and simultaneous advanced oxidation processes (AOPs) has become a research hotspot in the field of photocatalysis and environmental chemistry. Compared with the traditional anthraquinone process, this process does not use the more dangerous hydrogen (H») to participate in the reaction, but uses the abundant oxygen on the earth as the raw material and sunlight as the energy source to produce hydrogen peroxide. Semiconductors act as photocatalysts, and no pollution occurs throughout the process.
The limitation of high energy consumption of traditional photoelectric in situ synthesis of hydrogen peroxide is avoided.
And advanced oxidation processes (AOPs) are one of the most promising technologies in the treatment of industrial wastewater and water disinfection. Its main advantage is that with the participation of hydroxyl radicals (-OH), it can effectively remove stubborn components and pathogenic bacteria in water, and the whole process will not produce secondary waste. In general, the Fenton reaction utilizing the reaction of Fe** and hydrogen peroxide to generate hydroxyl radicals is the main method for water disinfection [equation (1)]. Ferrous iron reacts witiJ503921 hydrogen peroxide to generate hydroxyl radicals, 1 mol of ferric iron (Fe3+) and 1 mol of hydroxyl (OH). It is precisely because of the existence of hydroxyl radicals that the Fenton reaction has a strong oxidizing property. Therefore, the application of Fenton technology for water disinfection and degradation of pollutants has broad prospects.
Fe’ +H,0,—Fe’*+OH+ OH (1)
As an emerging porous material, COFs are a class of crystalline porous organic polymers with permanent porosity and highly ordered structures, which have high thermal stability, high surface area, extremely low density and better modifiability. They mainly consist of a series of light elements C, N, H, O, B, etc., and are connected by structural units such as covalent bonds. A polygonal topology is formed with a rich nitrogen-atom skeleton and a stable chemical structure.
It can provide more sites for oxygen adsorption and hydrogen peroxide generation reaction in situ, which is beneficial to the photocatalytic reaction, and is a novel organic photocatalytic material with potential development prospects.
According to literature and reports, a covalent organic polymer linked by imine bonds (He, S.,
Yin, B., Niu, H, Cai, Y., Targeted synthesis of visible-light-driven covalent organic framework photocatalyst via molecular design and precise construction. Applied Catalysis B: Environmental 2018, 239, 147-153.), is a photocatalyst with application potential, but the covalent organic polymer has a narrow photoresponse range and a high recombination rate of photogenerated carriers. These problems restrict its further application in the field of photocatalysis. The introduction of noble metals as co-catalysts can significantly improve the material's ability to absorb visible light while inhibiting the recombination of photogenerated carriers. Therefore, loading gold nanoparticles on covalent organic polymers can greatly improve their photocatalytic performance.
The invention with the publication number CN104397026A provides a water treatment potassium ferrate bactericide and its preparation method, but it does not solve the problem that the combination of potassium ferrate and electrons to form Fe(IV) and Fe(V) with strong oxidation ability is done at relatively low efficiency, the oxidation ability of potassium ferrate is not fully used, which is not suitable for industrial application, uses phosphorus trichloride in the production process simultaneously, causes further environmental pollution easily; publication number of CN104014352A discloses a multivariate controllable synthesis method of BIOCI photocatalyst , the catalyst can be used for photocatalytic degradation of pollutants in watdsJ503921 especially carbamazepine, but a large amount of reagents are used in the catalyst preparation process, and the preparation process is complicated, takes a long time, and increases environmental burden.
The present invention discloses a visible light photocatalyst for synthesis in-situ hydrogen peroxide and preparation method and application thereof. The present photocatalyst can significantly improve the absorption capacity of visible light and has good visible light photoresponse and excellent photocatalytic performance, and can efficiently reduce oxygen to hydrogen peroxide in situ under visible light; the present photocatalyst can be applied in the field of sustainable development environment and clean production. The advanced oxidation technology is used to sterilize water, and the preparation method is simple, the synthesis efficiency is high, which meets the needs of practical production, and has high practical value and good environmental significance.
Technical solutions of the present invention are as follows:
One of the objects of the present invention is to provide a preparation method of visible light photocatalyst for synthesis in-situ hydrogen peroxide, wherein a wet impregnation method is adopted, and covalent organic polymer is impregnated with chloroauric acid, so that the chloroauric acid is uniformly distributed on an inner surface of the covalent organic polymer, thereby assisting the reduction of sodium borohydride to prepare Au nanoparticles to be loaded on the covalent organic polymer to synthesize Au-loaded covalent organic polymer (Au/COFs) visible light photocatalyst.
Further, the preparation method is specifically as follows:
S1. under ambient temperature conditions, dissolving 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, and sonicating the mixed solution in an ultrasonic machine and introducing nitrogen, and then placing the mixed solution in an oven to react, and forming a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively,
and drying the same in a vacuum oven to obtain a covalent organic polymer; LU503921
S3. after placing the covalent organic polymer obtained in S2 in ultrapure water for ultrasonic treatment, adding chloroauric acid and stirring to mix well; and
S4. slowly adding sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60 min, then placing the same on an oil bath pan to continue stirring until the reaction is complete, after the reaction completed, naturally cooling to room temperature, then washing with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for Au-loaded covalent organic polymer.
Further, the volume ratio of mesitylene, 1,4-dioxane, and 3M acetic acid in the ternary solvent in
S1 is 5: 5: 1, respectively, and the amount of the ternary solvent added is 11 mL.
Further, the ultrasonic time of the mixed solution in the S1 is 10-20 min, and the time of introducing nitrogen 1s 10-20 min.
Further, the reaction temperature in the oven in S1 is 110-130°C, and the reaction time is 2- 4d.
Further, the drying temperature in S2 is 110-130°C, and the drying time is 8-12h.
Further, the volume of the sodium borohydride aqueous solution in S4 is 15-25uL, and the concentration is 0.2 -0.4g mL.
Further, the stirring temperature of S4 in an oil bath pan is 50-70°C, and the time is 2-4h.
The second object of the present invention is to provide a visible light photocatalyst for synthesis in-situ hydrogen peroxide.
The third object of the present invention is to provide an application of a visible light photocatalyst for synthesis in-situ hydrogen peroxide, wherein the Au-loaded covalent organic polymer is used as photocatalyst, and hydrogen peroxide is synthesized in-situ by visible light to reduce oxygen, combined with advanced oxidation technology for sterilization of water bodies.
Compared with the prior art, the beneficial effects of the present invention are that: 1. The present invention is the first to introduce Au nanoparticles into a novel covalent organic polymer, and develop a novel photocatalytic material loaded with noble metal elements as a cocatalyst, which significantly improves the absorption capacity of visible light and realizes fast response, good visible light photoresponse and photocatalytic performance. And the HO» production performance test was carried out under the premise of the same metal loading.
Compared with other metals, Au has the most outstanding loading performance, and H,O, production thereof can reach about 1932umol gh.
2. The visible light photocatalyst provided by the present invention can effectively utilize visiblé/503921 light to reduce oxygen to synthesize hydrogen peroxide in situ, take use of advanced oxidation processes to generate more hydroxyl radicals, which makes the Fenton reaction have strong oxidative properties, and effectively remove stubborn components and pathogenic bacteria, and no secondary waste will be produced in the whole process. 3. The present invention adopts the chemical reduction method and uses sodium borohydride as a reducing agent to prepare Au-loaded covalent organic polymer visible light photocatalyst
Au/COFs. Compared with other traditional methods such as photoreduction and high-temperature calcination, composite materials with high metal loading can be obtained in a short time by using sodium borohydride reduction. 4. The preparation method provided by the present invention overcomes the time-consuming and labor-intensive problems of traditional preparation methods. The preparation method is simple, simple to operate, controllable in process, easy to implement, does not require high temperature and high pressure preparation conditions, has fast synthesis rate and high efficiency, which meets the requirements of environmental friendliness.
Fig. 1 is a transmission electron microscope image of visible light photocatalyst according to embodiment 2 in the present invention;
Fig. 2 is a Fourier transform infrared spectrum of a covalent organic polymer and the visible light photocatalyst of the embodiment 2 in the present invention;
Fig. 3 is a diagram of in-situ synthesis of hydrogen peroxide between covalent organic polymer and visible light photocatalyst of the embodiment 2 in the present invention;
Fig. 4 is a diagram showing bactericidal effects of a covalent organic polymer and a visible light photocatalyst of the embodiment 2 in the present invention.
Hereinafter, the present invention will be further described in combination with the accompanying drawings and preferred embodiments, and the given embodiments are only for clarifying the present invention, not for limiting the scope of the present invention.
Materials, reagents, etc. used in the following examples, if not otherwise specified, can be obtained from commercial sources; LU503921
Quantitative experiments in the following examples are all set to repeat the experiment three times, and the results are averaged;
The experimental methods in the following examples, if no special instructions, are conventional methods:
Embodiment 1
The present embodiment provides a preparation method of visible light photocatalyst for synthesis in-situ hydrogen peroxide, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, the volume ratios of the three solvents are 5:5:1, and the total volume of the three is 11mL; and sonicating the mixed solution in an ultrasonic machine for 10min to disperse evenly, and nitrogen is introduced for 10min; and then placing the mixed solution in an oven of 100°C to react for 2d to form a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven at 110°C for 8h to obtain a covalent organic polymer;
S3. putting 100mg of covalent organic polymer in 150mL of ultrapure water and sonicate for 30min, then adding chloroauric acid with a content of 0.5mg Au into the aqueous solution and stirring for 30min to make the two fully contact;
S4. slowly adding 15uL of 0.2gmL”! sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to keep stirring at 50°C for 2h, until naturally cooling to room temperature, washing it with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for
Au-loaded covalent organic polymer.
The content of Au in the visible light photocatalyst prepared according to the method of embodiment 1 is 0.5mg.
Embodiment 2
The present embodiment provides a visible light photocatalyst for synthesis in-situ hydrogen peroxide, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4°,4”-(1,3,5-triazine-2,4,6-triyl)
triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solveht/503921 composed of mesitylene, 1,4-dioxane, and 3M acetic acid, the volume ratios of the three solvents are 5:5:1, and the total volume of the three is 11 mL; and sonicating the mixed solution in an ultrasonic machine for 15min to disperse evenly, and nitrogen is introduced for 15min; and then placing the mixed solution in an oven of 120°C to react for 3d to form a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven at 120°C for 10h to obtain a covalent organic polymer;
S3. putting 100mg of covalent organic polymer in 150mL of ultrapure water and sonicate for 30min, then adding chloroauric acid with a content of Img Au into the aqueous solution and stir for 30 min to make the two fully contact;
S4. slowly adding 20uL of 0.3gmL”! sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to keep stirring at 60°C for 3h, until it naturally cools to room temperature, washing it with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for
Au-loaded covalent organic polymer.
The content of Au in the visible light photocatalyst prepared according to the method of embodiment 2 is Img.
Embodiment 3
The present embodiment provides a preparation method of visible light photocatalyst for synthesis in-situ hydrogen peroxide, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4°,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, the volume ratios of the three solvents are 5:5:1, and the total volume of the three is 11mL; and sonicating the mixed solution in an ultrasonic machine for 15min to disperse evenly, and nitrogen is introduced for 15min; and then placing the mixed solution in an oven of 120°C to react for 4d to form a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven at 120°C for 10h to obtain a covalent organic polymer;
S3. putting 100mg of covalent organic polymer in 150mL of ultrapure water and sonicate for
30min, then adding chloroauric acid with a content of 1.5mg Au into the aqueous solution and/503921 stir for 30min to make the two fully contact;
S4. slowly adding 20uL of 0.3gmL”! sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to keep stirring at 60°C for 3h, until it naturally cools to room temperature, washing it with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for
Au-loaded covalent organic polymer.
The content of Au in the visible light photocatalyst prepared according to the method of embodiment 3 is 1.5mg.
Embodiment 4
The present embodiment provides a preparation method of visible light photocatalyst for synthesis in-situ hydrogen peroxide, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4°,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, the volume ratios of the three solvents are 5:5:1, and the total volume of the three is 11mL; and sonicating the mixed solution in an ultrasonic machine for 15min to disperse evenly, and nitrogen is introduced for 15min; and then placing the mixed solution in an oven of 120°C to react for 3d to form a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven at 120°C for 10h to obtain a covalent organic polymer;
S3. putting 100mg of covalent organic polymer in 150mL of ultrapure water and sonicate for 30min, then adding chloroauric acid with a content of 2mg Au into the aqueous solution and stir for 30min to make the two fully contact;
S4. slowly adding 20uL of 0.3gmL”! sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to keep stirring at 60°C for 3h, until it naturally cools to room temperature, washing it with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for
Au-loaded covalent organic polymer.
The content of Au in the visible light photocatalyst prepared according to the method of embodiment 4 is 2mg.
Embodiment 5 LU503921
The present embodiment provides a preparation method of visible light photocatalyst for synthesis in-situ hydrogen peroxide, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4°,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, the volume ratios of the three solvents are 5:5:1, and the total volume of the three is 11mL; and sonicating the mixed solution in an ultrasonic machine for 20min to disperse evenly, and nitrogen is introduced for 20min; and then placing the mixed solution in an oven of 130°C to react for 4d to form a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven at 130°C for 12h to obtain a covalent organic polymer;
S3. putting 100mg of covalent organic polymer in 150mL of ultrapure water and sonicate for 30min, then adding chloroauric acid with a content of 3mg Au into the aqueous solution and stir for 30min to make the two fully contact;
S4. slowly adding 25uL of 0.4gmL”! sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to keep stirring at 70°C for 4h, until it naturally cools to room temperature, washing it with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for
Au-loaded covalent organic polymer.
The content of Au in the visible light photocatalyst prepared according to the method of embodiment 5 is 3mg.
Performance Testing 1. Structural testing of visible light photocatalysts
Fig. 1 is a transmission electron microscope image of visible light photocatalyst of embodiment 2; it can be clearly seen from the figure that the Au nanoparticles are evenly loaded on the surface of the covalent organic polymer, and the particle size is about 2 nm;
Fig. 2 is a Fourier transform infrared spectrum of a covalent organic polymer and the visible light photocatalyst of the embodiment 2; it can be clearly seen from Fig. 2 that the covalent organic polymer has the same absorption characteristic peaks as the Au-loaded covalent organic polymer visible light photocatalyst in Embodiment 2, which indicates that the introduction of Au nanoparticles does not change the parent polymer structure of the covalent organic polymer. LU503921 2. Visible light photocatalyst synthesis hydrogen peroxide test
Fig. 3 1s an effect diagram of in-situ synthesis of hydrogen peroxide between covalent organic polymer and visible light photocatalyst of the embodiment 2; 10mg of photocatalyst is dissolved in 50mL of deionized water, shading and ultrasonication for 30min, and then the aqueous solution is stirred in the dark for 30min. It is placed under a 300W xenon lamp with a UV filter for irradiation, and the entire reaction temperature is controlled at about 25°C; within a fixed period of time, 3mL of the reaction solution is taken to detect the concentration of hydrogen peroxide. The method adopted is an iodine titration method; take 1ml of potassium hydrogen phthalate solution (0.1mol-L") and potassium iodide solution (0.4 mol-L!) and mix them with the reaction solution, and store them in the dark state for 30min; under the conditions, it will react with the iodide ion (I') in the solution to generate iodine triion (Is"), and the iodide triton will have a strong absorption peak at 350nm. The process is detected by UV-vis photometer; the content of hydrogen peroxide can be estimated by the intensity of the absorption peak at 350nm; it can be clearly seen from the experimental results that compared with the parent material, the performance of the visible light photocatalyst for in situ synthesis of hydrogen peroxide has been greatly improved. 3. Visible light photocatalyst sterilization test
Fig. 4 is a bactericidal effect diagram of a covalent organic polymer and a visible light photocatalyst of the embodiment 2; the bacterium adopted for sterilization is Escherichia coli, and before the experiment, Escherichia coli is first kept in 75mL of LB culture medium at a constant temperature of 37°C for culturing for 16h, ImL of bacterial liquid is taken out and centrifuged for Imin, and is washed twice with 0.9% sterile normal saline, and then the bacteria are cultured in normal saline; the concentration of bacterial liquid is 2x10” cfu-mL*. 10mg of photocatalyst is mixed with bacteria in a beaker for dark state adsorption for 30min, and then
Fe?” is added to activate the hydrogen peroxide to generate hydroxyl radicals when the light is turned on. The concentration of Fe?" was controlled at about 2.7mM; At time intervals, ImL of the reaction solution is diluted step by step, and the inactivation of bacteria is observed by plate counting method; from the experimental results, it can be seen that the sterilization effect of the visible light photocatalyst is significantly enhanced compared with that of the parent.
The above are only embodiments of the present invention, and do not limit the patent scope of the present invention.
Any equivalent structure or equivalent process conversion made by usih&}503921 the content of the description of the present invention, or directly or indirectly used in other related technical fields, shall all be included in the scope of protection of the present invention.
Claims (10)
1. À preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide, wherein a wet impregnation method is adopted, and covalent organic polymer is impregnated with chloroauric acid, so that the chloroauric acid is uniformly distributed on an inner surface of the covalent organic polymer, thereby assisting the reduction of sodium borohydride to prepare Au nanoparticles to be loaded on the covalent organic polymer to synthesize Au-loaded covalent organic polymer (Au/COFs) visible light photocatalyst.
2. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, specifically comprises the following steps:
S1. under normal temperature conditions, dissolving 4,4°,4”-(1,3,5-triazine-2,4,6-triyl) triphenylcarbaldehyde, 4,4’,4”-(1,3,5-triazine-2,4,6-triyl) triphenylamine in a ternary solvent composed of mesitylene, 1,4-dioxane, and 3M acetic acid, and sonicating the mixed solution in an ultrasonic machine and introducing nitrogen, and then placing the mixed solution in an oven to react, and forming a yellowish precipitate by self-nucleation, and naturally cooling to room temperature after the reaction;
S2. washing the precipitate in the reaction kettle with acetone and tetrahydrofuran respectively, and drying same in a vacuum oven to obtain a covalent organic polymer;
S3. after placing the covalent organic polymer obtained in S2 in ultrapure water for ultrasonication, adding chloroauric acid and stir to mix well; and
S4. slowly adding sodium borohydride aqueous solution to the solution described in S3 to stir vigorously for 60min, then placing same on an oil bath pan to continue to stirring until the reaction is complete, after the reaction completed, naturally cooling to room temperature, then washing with pure water and absolute ethyl alcohol, and then freeze-drying to obtain visible light photocatalyst for Au-loaded covalent organic polymer.
3. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, wherein the volume ratio of mesitylene, 1,4-dioxane, and 3M acetic acid in the ternary solvent in S1 is 5: 5: 1, respectively, and the amount of the ternary solvent added is 11 mL.
4. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, wherein the ultrasonic time of the mixed solution in the S1 is 10-20min, and the time of introducing nitrogen is 10-20min.
5. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogé/503921 peroxide according to claim 1, wherein the reaction temperature in the oven in S1 is 110-130°C, and the reaction time is 2- 4d.
6. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, wherein the drying temperature in S2 is 110-130°C, and the drying time is 8-12h.
7. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, wherein the volume of the sodium borohydride aqueous solution in S4 is 15-25 pL, and the concentration is 0.2 -0.4g mL".
8. The preparation method of visible light photocatalyst for in-situ synthesis of hydrogen peroxide according to claim 1, wherein the stirring temperature of S4 in an oil bath pan is 50-70°C, and the time is 2-4h.
9. A visible light photocatalyst for in-situ synthesis of hydrogen peroxide prepared according to any one of the method according to any one of claims 1 to 8.
10. An application of a visible light photocatalyst for in-situ synthesis of hydrogen peroxide, wherein the Au-loaded covalent organic polymer is used as photocatalyst, and hydrogen peroxide is synthesized in-situ by visible light to reduce oxygen, combined with advanced oxidation technology for sterilization of water bodies.
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