CN116870920A - Preparation method and application of cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst - Google Patents
Preparation method and application of cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst Download PDFInfo
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- CN116870920A CN116870920A CN202311150334.2A CN202311150334A CN116870920A CN 116870920 A CN116870920 A CN 116870920A CN 202311150334 A CN202311150334 A CN 202311150334A CN 116870920 A CN116870920 A CN 116870920A
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- photocatalyst
- vanadium
- cuprous oxide
- vanadium pentoxide
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 57
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 title claims abstract description 22
- 229960000282 metronidazole Drugs 0.000 claims abstract description 32
- VAOCPAMSLUNLGC-UHFFFAOYSA-N metronidazole Chemical compound CC1=NC=C([N+]([O-])=O)N1CCO VAOCPAMSLUNLGC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011259 mixed solution Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 15
- 230000000593 degrading effect Effects 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims abstract description 4
- 239000010949 copper Substances 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 23
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 10
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 9
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 9
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 8
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 8
- 239000008103 glucose Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 abstract description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 4
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 4
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 4
- 229940112669 cuprous oxide Drugs 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical class O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
-
- 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
- C02F2101/38—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 discloses a preparation method and application of a cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, which relate to the technical field of photocatalyst preparation and specifically comprise the following steps: s1: preparation of Cu 2 O; s2: preparing a cuprous oxide-vanadium dioxide/vanadium pentoxide composite material: cu is taken out 2 Dispersing O in deionized waterAdding vanadium pentoxide, isopropanol and benzyl alcohol, stirring vigorously to obtain a mixed solution B, transferring the mixed solution B into a hydrothermal reaction kettle for constant-temperature reaction, cooling to room temperature after the reaction is finished, washing with deionized water and absolute ethyl alcohol for 3 times, drying, and grinding to obtain the cuprous oxide-vanadium dioxide/vanadium heptaoxide photocatalyst. The photocatalyst has stable performance, good effect on degrading metronidazole, high light source utilization rate, low price of all raw materials, no pollution, simple preparation and low energy consumption, has good application prospect in solving the environmental pollution, energy crisis and photocatalysis application field, and can be produced in a large scale.
Description
Technical Field
The invention relates to the technical field of photocatalyst preparation, in particular to a preparation method and application of a cuprous oxide-vanadium dioxide/vanadium heptaoxide photocatalyst.
Background
Along with the development of scientific technology, the usage amount of antibiotics in agriculture and medicine is gradually increased, so that the content of metronidazole in the ecological environment is also gradually increased, and the situation of general exceeding standard exists. The problem of environmental metronidazole pollution treatment is a worldwide problem, and the traditional technology such as adsorption, biological treatment, semi-permeable membranes and the like is difficult to completely degrade the metronidazole in the ecological environment, and has the advantages of high cost, slow reaction, easy secondary pollution, incapability of completely eliminating pollutants and the like.
The photocatalysis technology using the semiconductor and the derivative material thereof as media is a sustainable, pollution-free, economical and effective means, and can utilize clean and sustainable solar energy to treat toxic substances such as waste water, waste gas and the like in the environment, thereby improving the environmental cleanliness and effectively solving the environmental problems facing the human society. The vanadium-based catalyst has the advantages of low cost, good biocompatibility, easy acquisition, easy synthesis, good electrical and optical properties and the like, but the problems of complex preparation process, low light source utilization rate, limited catalytic properties and the like are generally existed.
Based on the above, the photocatalyst which is simple to prepare, excellent in catalytic performance and high in light source utilization rate is provided, and the technical problem to be solved by the person in the field is needed.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method and application of a cuprous oxide-vanadium dioxide/vanadium heptaoxide photocatalyst.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
as shown in fig. 1, the invention provides a preparation method of an ultrathin sheet cuprous oxide-vanadium dioxide/vanadium heptaoxide photocatalyst, which specifically comprises the following steps:
s1: preparation of Cu 2 O: weighing anhydrous copper sulfate, potassium sodium tartrate and sodium hydroxide in a beaker, adding deionized water, stirring for 10min, and obtaining a mixed solution A after the solution is blue-black; transferring the mixed solution A into a beaker containing glucose, continuously stirring, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparing a cuprous oxide-vanadium dioxide/vanadium pentoxide composite material: taking a certain amount of Cu prepared in the step S1 2 Dispersing O in deionized water, adding vanadium pentoxide, isopropanol and benzyl alcohol, vigorously stirring to obtain a mixed solution B, transferring the mixed solution B into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out constant-temperature reaction in an electric blast drying box, cooling to room temperature after the reaction is finished, washing with deionized water and absolute ethyl alcohol for 3 times, drying, and grinding to obtain the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst.
Further, in the step S1, the mass ratio of the copper sulfate pentahydrate, the potassium sodium tartrate, the sodium hydroxide to the glucose is 1.2:1.2:1:1.
Further, in the step S1, the volume of deionized water is 200mL.
Further, in the step S2, the volume of deionized water is 36mL, the mass of vanadium pentoxide is 1.82g, the volume of isopropanol is 12.5mL, and the volume of benzyl alcohol is 1.5mL; the volume of polytetrafluoroethylene was 100mL.
Further, in the step S2, cu 2 The mass of O is one of 0.1274g, 0.2867g, 0.4915g and 0.7646 g.
Further, in the step S2, the stirring speed is 1100rpm, the isothermal reaction temperature is 180 ℃, the isothermal reaction time is 48 hours, the drying temperature is 80 ℃, and the drying time is 12 hours.
The invention also provides application of the cuprous oxide-vanadium dioxide/vanadium heptaoxide photocatalyst, and the photocatalyst is used for catalyzing and degrading metronidazole under visible light.
Further, the mass ratio of the photocatalyst to the metronidazole is 6:1.
Compared with the prior art, the invention has the beneficial effects that:
the method of the invention uses a one-step hydrothermal method to prepare cuprous oxide and VO 2 /V 3 O 7 The combination utilizes cuprous oxide to promote the transmission of photo-generated charge, accelerates the rapid separation of photo-generated electrons and holes, further promotes the conversion of persulfate to sulfate free radicals, and simultaneously ensures that the catalyst has good recoverability due to the mutual conversion of metals with different valence states. The photocatalyst composite material prepared by the method has stable performance, good effect on degrading metronidazole, high light source utilization rate, low price of all used raw materials, no pollution, simple preparation and low energy consumption, has good application prospect in solving environmental pollution, energy crisis and photocatalysis application fields, and can be produced in a large scale.
Drawings
FIG. 1 is a Cu of the present invention 2 O-VO 2 /V 3 O 7 Scanning electron microscope images of the samples;
FIG. 2 is a graph showing the effect of different catalysts of the present invention on photocatalytic metronidazole degradation under visible light.
Detailed Description
The present invention will be described in further detail with reference to examples in order to make the objects and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The instruments, reagents, materials, etc. used in the following examples are conventional instruments, reagents, materials, etc. known in the art, and are commercially available. The experimental methods, detection methods, and the like in the following examples are conventional experimental methods, detection methods, and the like existing in the prior art unless otherwise specified.
Example 1
The present embodiment provides a Cu 2 O-VO 2 /V 3 O 7 The preparation method of the photocatalyst specifically comprises the following steps:
s1: preparation of Cu 2 O: 7.2g of copper sulfate pentahydrate, 7.2g of potassium sodium tartrate and 6g of sodium hydroxide are weighed into a 250mL beaker, 200mL of deionized water is added, and stirring is carried out for 10min, and after the solution is blue-black, a mixed solution A is obtained; transferring the mixed solution A into a 250mL beaker containing 6g of glucose, continuously stirring, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparation of Cu 2 O-VO 2 /V 3 O 7 Composite material: 0.1274g of Cu prepared in step S1 is taken 2 O is dispersed in 36mL of deionized water, 1.82g of vanadium pentoxide, 12.5mL of isopropanol and 1.5mL of benzyl alcohol are added, and the mixture is vigorously stirred at 1100rpm to obtain a mixed solution B; transferring the mixed solution B into a hydrothermal reaction kettle with a 100mL polytetrafluoroethylene lining, reacting for 48 hours at the constant temperature of 180 ℃ in an electric blowing drying box, cooling to room temperature after the reaction is finished, washing for 3 times by deionized water and absolute ethyl alcohol, drying for 12 hours at 80 ℃, and grinding to obtain 10wt%Cu 2 O-VO 2 /V 3 O 7 The photocatalyst, designated 10-Cu-V.
The embodiment also provides a Cu as described above 2 O-VO 2 /V 3 O 7 Application of photocatalyst for catalytic degradation of metronidazole under visible light, wherein the mass ratio of photocatalyst to metronidazole is 6:1。
Example 2
The present embodiment provides a Cu 2 O-VO 2 /V 3 O 7 The preparation method of the photocatalyst specifically comprises the following steps:
s1: preparation of Cu 2 O: 7.2g of copper sulfate pentahydrate, 7.2g of potassium sodium tartrate and 6g of sodium hydroxide are weighed into a 250mL beaker, 200mL of deionized water is added, and stirring is carried out for 10min, and after the solution is blue-black, a mixed solution A is obtained; transferring the mixed solution A into a 250mL beaker containing 6g of glucose, continuously stirring, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparation of Cu 2 O-VO 2 /V 3 O 7 Composite material: 0.2867g of Cu prepared in step S1 is taken 2 O is dispersed in 36mL of deionized water, 1.82g of vanadium pentoxide, 12.5mL of isopropanol and 1.5mL of benzyl alcohol are added, and the mixture is vigorously stirred at 1100rpm to obtain a mixed solution B; transferring the mixed solution B into a hydrothermal reaction kettle with a 100mL polytetrafluoroethylene lining, reacting for 48 hours at the constant temperature of 180 ℃ in an electric blowing drying box, cooling to room temperature after the reaction is finished, washing for 3 times by deionized water and absolute ethyl alcohol, drying for 12 hours at 80 ℃, and grinding to obtain 20wt% Cu 2 O-VO 2 /V 3 O 7 The photocatalyst, designated 20-Cu-V.
The embodiment also provides a Cu as described above 2 O-VO 2 /V 3 O 7 The photocatalyst is used for catalyzing and degrading metronidazole under visible light, wherein the mass ratio of the photocatalyst to the metronidazole is 6:1.
Example 3
The present embodiment provides a Cu 2 O-VO 2 /V 3 O 7 The preparation method of the photocatalyst specifically comprises the following steps:
s1: preparation of Cu 2 O: 7.2g of copper sulfate pentahydrate, 7.2g of potassium sodium tartrate and 6g of sodium hydroxide are weighed into a 250mL beaker, 200mL of deionized water is added, and stirring is carried out for 10min, and after the solution is blue-black, a mixed solution A is obtained; transfer mixture A to 250mL containing 6g glucoseContinuously stirring in a beaker, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparation of Cu 2 O-VO 2 /V 3 O 7 Composite material: 0.4915g of Cu prepared in step S1 is taken 2 O is dispersed in 36mL of deionized water, 1.82g of vanadium pentoxide, 12.5mL of isopropanol and 1.5mL of benzyl alcohol are added, and the mixture is vigorously stirred at 1100rpm to obtain a mixed solution B; transferring the mixed solution B into a hydrothermal reaction kettle with a 100mL polytetrafluoroethylene lining, reacting for 48 hours at the constant temperature of 180 ℃ in an electric blowing drying box, cooling to room temperature after the reaction is finished, washing for 3 times by deionized water and absolute ethyl alcohol, drying for 12 hours at 80 ℃, and grinding to obtain 30wt% Cu 2 O-VO 2 /V 3 O 7 The photocatalyst, designated 30-Cu-V.
The embodiment also provides a Cu as described above 2 O-VO 2 /V 3 O 7 The photocatalyst is used for catalyzing and degrading metronidazole under visible light, wherein the mass ratio of the photocatalyst to the metronidazole is 6:1.
Example 4
The present embodiment provides a Cu 2 O-VO 2 /V 3 O 7 The preparation method of the photocatalyst specifically comprises the following steps:
s1: preparation of Cu 2 O: 7.2g of copper sulfate pentahydrate, 7.2g of potassium sodium tartrate and 6g of sodium hydroxide are weighed into a 250mL beaker, 200mL of deionized water is added, and stirring is carried out for 10min, and after the solution is blue-black, a mixed solution A is obtained; transferring the mixed solution A into a 250mL beaker containing 6g of glucose, continuously stirring, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparation of Cu 2 O-VO 2 /V 3 O 7 Composite material: 0.7646g of Cu prepared in step S1 is taken 2 O is dispersed in 36mL of deionized water, 1.82g of vanadium pentoxide, 12.5mL of isopropanol and 1.5mL of benzyl alcohol are added, and the mixture is vigorously stirred at 1100rpm to obtain a mixed solution B; transfer mix B to hydrothermal with 100mL polytetrafluoroethylene linerIn a reaction kettle, carrying out constant-temperature reaction for 48h at 180 ℃ in an electric blast drying box, cooling to room temperature after the reaction is finished, washing for 3 times with deionized water and absolute ethyl alcohol, drying for 12h at 80 ℃, and grinding to obtain 40wt% Cu 2 O-VO 2 /V 3 O 7 The photocatalyst, designated 40-Cu-V.
The embodiment also provides a Cu as described above 2 O-VO 2 /V 3 O 7 The photocatalyst is used for catalyzing and degrading metronidazole under visible light, wherein the mass ratio of the photocatalyst to the metronidazole is 6:1.
Comparative example 1
Pure Cu 2 The preparation method of the O photocatalyst comprises the following steps: 7.2g of copper sulfate pentahydrate, 7.2g of potassium sodium tartrate and 6g of sodium hydroxide are weighed and placed in a 250mL beaker, dissolved in 200mL deionized water, stirred for 10min, and after the solution is blue-black, a mixed solution A is obtained; transfer mixture a to a 250ml beaker containing 6g glucose; continuously stirring, and vacuum filtering after the solution presents bright red; washing the filter cake, and drying to obtain the required Cu 2 O。
Comparative example 2
VO 2 /V 3 O 7 The preparation method of the photocatalyst comprises the following steps: dispersing 1.82g of vanadium pentoxide in 36mL of deionized water, adding 12.5mL of isopropanol and 1.5mL of benzyl alcohol, vigorously stirring to obtain a mixed solution, transferring the mixed solution into a hydrothermal reaction kettle for constant temperature reaction, cooling to room temperature after the reaction is finished, washing, drying and grinding to obtain VO 2 /V 3 O 7 A catalyst.
The photocatalysts prepared in the above examples 1-4 and comparative examples 1-2 are used for degrading and dissolving metronidazole under the condition of visible light, and the specific steps are as follows: 15mg of photocatalyst sample is taken and added into 50mL of 50mg/L metronidazole solution (the dosage ratio of the metronidazole to the mass of the photocatalyst is 1:6), ultrasound is carried out for 3min, and magnetons are added. Starting the photocatalytic instrument, starting revolution and starting stirring. The reaction system is placed in a photocatalysis instrument and stirred for 10min under the dark condition, so that the adsorption and desorption balance of the catalyst and the metronidazole is achieved. Sampling 5-6mL every five minutes, taking 2 times, after sampling,the circulating water was turned on, 10mg sodium Persulfate (PDS) was added, and the xenon lamp light source was turned on. Sampling for 4 times every 5min, and 5-6mL each time. After the experiment is finished, the light source is turned off, the photocatalytic instrument is turned off, and the circulating water is turned off. After the sample solution is filtered, an ultraviolet spectrophotometer is used for detecting absorbance, the photocatalytic degradation rate is calculated as shown in a formula 1, and the result is shown in the attached figure 2. The calculation formula is as follows:wherein C 0 At an initial concentration of C t For the concentration of metronidazole at time t, A 0 For the initial absorbance of the metronidazole solution, A t Is the absorbance of the metronidazole solution at time t.
As can be seen from FIG. 2, the 10-Cu-V photocatalyst of example 1 was able to degrade 87% of a 50mg/L metronidazole solution in 20min under irradiation with visible light. The 20-Cu-V photocatalyst of example 2 was able to degrade 93% of a 50mg/L metronidazole solution 20min under visible light irradiation. The 30-Cu-V photocatalyst of example 3 was capable of degrading 94.7% of a 50mg/L metronidazole solution under visible light irradiation for 20 min. The 40-Cu-V photocatalyst of example 4 was capable of degrading 92.2% of a 50mg/L metronidazole solution under visible light irradiation for 20 min. Cu of comparative example 1 2 Under the irradiation of visible light, the O photocatalyst can degrade 6% of 50mg/L metronidazole solution for 20 min. VO of comparative example 2 2 /V 3 O 7 The photocatalyst can degrade 25% of 50mg/L metronidazole solution in 20min under the irradiation of visible light. From this, it can be seen that Cu prepared in this example 1-4 2 O-VO 2 /V 3 O 7 The photocatalyst has good effect of degrading metronidazole, and is obviously superior to comparative examples 1-2.
In summary, the method of the embodiment uses a one-step hydrothermal method to convert cuprous oxide and VO 2 /V 3 O 7 The combination utilizes cuprous oxide to promote the transmission of photo-generated charge, accelerates the rapid separation of photo-generated electrons and holes, further promotes the conversion of persulfate to sulfate free radicals, and simultaneously ensures that the catalyst has good recoverability due to the mutual conversion of metals with different valence states. The photocatalyst composite material prepared by the method of the embodiment has stable performance and p-methyl nitrateThe azole has good degradation effect, high light source utilization rate, low price of all raw materials, no pollution, simple preparation and low energy consumption, has good application prospect in solving the environmental pollution, energy crisis and photocatalysis application fields, and can be produced on a large scale.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (8)
1. A preparation method of a cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst is characterized by comprising the following steps of: the method specifically comprises the following steps:
s1: preparation of Cu 2 O: weighing copper sulfate pentahydrate, potassium sodium tartrate and sodium hydroxide in a beaker, adding deionized water, stirring for 10min, and obtaining a mixed solution A after the solution is blue-black; transferring the mixed solution A into a beaker containing glucose, continuously stirring, vacuum filtering after the solution presents bright red, washing a filter cake, and drying to obtain Cu 2 O；
S2: preparing a cuprous oxide-vanadium dioxide/vanadium pentoxide composite material: taking a certain amount of Cu prepared in the step S1 2 Dispersing O in deionized water, adding vanadium pentoxide, isopropanol and benzyl alcohol, vigorously stirring to obtain a mixed solution B, transferring the mixed solution B into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, carrying out constant-temperature reaction in an electric blast drying box, cooling to room temperature after the reaction is finished, washing with deionized water and absolute ethyl alcohol for 3 times, drying, and grinding to obtain the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst.
2. The method for preparing the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, according to claim 1, which is characterized in that: in the step S1, the mass ratio of the copper sulfate pentahydrate, the potassium sodium tartrate, the sodium hydroxide and the glucose is 1.2:1.2:1:1.
3. The method for preparing the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, according to claim 1, which is characterized in that: in the step S1, the volume of deionized water is 200mL.
4. The method for preparing the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, according to claim 1, which is characterized in that: in the step S2, the volume of deionized water is 36mL, the mass of vanadium pentoxide is 1.82g, the volume of isopropanol is 12.5mL, and the volume of benzyl alcohol is 1.5mL; the volume of polytetrafluoroethylene was 100mL.
5. The method for preparing the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, according to claim 1, which is characterized in that: in the step S2, cu 2 The mass of O is one of 0.1274g, 0.2867g, 0.4915g and 0.7646 g.
6. The method for preparing the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst, according to claim 1, which is characterized in that: in the step S2, the stirring speed is 1100rpm, the constant temperature reaction temperature is 180 ℃, the constant temperature reaction time is 48 hours, the drying temperature is 80 ℃, and the drying time is 12 hours.
7. The use of the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst prepared by the preparation method of the cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst according to any one of claims 1-6, characterized in that: the photocatalyst is used for catalyzing and degrading metronidazole under visible light.
8. The use of a cuprous oxide-vanadium dioxide/vanadium pentoxide photocatalyst as claimed in claim 7, wherein: the mass ratio of the photocatalyst to the metronidazole is 6:1.
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