CN116351471A - Prussian blue/g-C 3 N 4 Composite photocatalyst, preparation method and application thereof - Google Patents
Prussian blue/g-C 3 N 4 Composite photocatalyst, preparation method and application thereof Download PDFInfo
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- CN116351471A CN116351471A CN202310242005.4A CN202310242005A CN116351471A CN 116351471 A CN116351471 A CN 116351471A CN 202310242005 A CN202310242005 A CN 202310242005A CN 116351471 A CN116351471 A CN 116351471A
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- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229960003351 prussian blue Drugs 0.000 title claims abstract description 98
- 239000013225 prussian blue Substances 0.000 title claims abstract description 98
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 239000000047 product Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
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- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- -1 potassium ferricyanide Chemical compound 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 239000000243 solution Substances 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 8
- 238000012546 transfer Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- 229960003405 ciprofloxacin Drugs 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- VMXUWOKSQNHOCA-LCYFTJDESA-N ranitidine Chemical compound [O-][N+](=O)/C=C(/NC)NCCSCC1=CC=C(CN(C)C)O1 VMXUWOKSQNHOCA-LCYFTJDESA-N 0.000 description 4
- 229960000620 ranitidine Drugs 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
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- 239000002135 nanosheet Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
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- 229910052742 iron Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
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- 238000002560 therapeutic procedure Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
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- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
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- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- 230000036541 health Effects 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
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- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 229940040944 tetracyclines Drugs 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
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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
-
- 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
- B01J27/24—Nitrogen compounds
-
- 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
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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
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- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention provides Prussian blue/g-C 3 N 4 The preparation method and application of the composite photocatalyst comprise the following steps: dissolving urea in deionized water, heating to 30deg.C, transferring the solution into a ceramic crucible with a cover, and calcining at high temperature to obtain product g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Polyvinylpyrrolidone, potassium ferricyanide and product g-C 3 N 4 Dripping into HCl solution to obtain suspension, and performing hydrothermal reaction in a stainless steel autoclave; after the reaction, the precipitate was centrifuged by cooling andwashing with deionized water and absolute ethanol for three times, and vacuum drying to obtain Prussian blue/g-C 3 N 4 A composite photocatalyst. Prussian blue/g-C 3 N 4 The visible light absorption area of the composite photocatalyst is enlarged, the absorption capacity is enhanced, the visible light utilization rate is high, and the Prussian blue/g-C 3 N 4 The composite photocatalyst has obvious effect on photodegradation of environmental pollutants such as antibiotic medicines, dyes and the like.
Description
Technical Field
The invention relates to the technical field of photocatalysts, in particular to Prussian blue/g-C 3 N 4 A composite photocatalyst, a preparation method and application thereof.
Background
Over the last decades, with the continued development of urbanization, a large number of antibiotics have been widely used to treat human and animal infections. Tetracyclines, a typical antibiotic, have been widely used in human therapy, animal therapy and agricultural production. It has been reported that about 21 ten thousand tons of tetracycline are discharged into the aquatic ecosystem together with wastewater each year due to incomplete treatment by conventional methods. In addition, it has been found that even at nanogram levels, tetracycline in the aquatic ecosystem poses a serious threat to the environment and human health. The heterogeneous light Fenton technology is regarded as an effective method for degrading persistent organic pollutants as an advanced oxidation process due to high efficiency, good circularity, simple operation and no generation of a large amount of iron mud. However, most of the reported photo-Fenton catalysts absorb only ultraviolet rays, accounting for only about 5% of the solar spectrum, which makes it difficult to use natural solar ultraviolet rays as an energy source. In addition, some photo-Fenton catalysts exhibit high activity only at low pH values, or require expensive chemicals and time consuming synthetic processes. Therefore, developing a visible light response pH analyzer with a simple synthesis procedure and a wide operating pH is critical to facilitate the application of the photo Fenton technique.
Graphite carbonitride (g-C) 3 N 4 ) The method has the characteristics of abundant resources, simple preparation, unique belt structure and the like, and is widely applied to environmental remediation and water treatment. However, its degradation performance is severely limited due to its low surface area, limited visible light utilization, and poor charge separation and transfer efficiency.
From previous reports, it has been demonstrated that when g-C 3 N 4 When coupled with transition metal-based materialsBy expanding the light absorption range, increasing the charge separation and transfer ability, and activating the photo Fenton (-like) reaction, the g-C can be greatly improved 3 N 4 Is a degradation property of the polymer. Prussian blue is a class of metal-organic frameworks with face-centered cubic cells in which ferrous (Fe II) and ferric (Fe III) ions are alternately bridged by cyano ligands (C≡N), where high spin FeHS (Fe III) is coupled to N and low spin Fe LS (Fe II) is coordinated to C. Prussian blue and analogues thereof are considered to be g-C due to their low cost, low toxicity, relative stability and unique chemical composition 3 N 4 Ideal materials for coupling. Although Prussian blue degradation contaminants have been reported in Fenton systems, few studies on the g-C used by Prussian blue and light Fenton systems have been made 3 N 4 Is a combination of (a) and (b).
Structural defect engineering as enhancement of g-C 3 N 4 Another popular strategy for photocatalytic performance has received much attention, which not only allows for the modulation of electronic structure, but also increases active sites. In particular, when defects (N, C, O, etc.) are introduced into g-C having a larger surface area 3 N 4 When in the framework of (2), shows the synergistic improvement effect of the photocatalytic performance. In addition, g-C 3 N 4 Various forms (including macropores, nanoplatelets, microtubes) of (a) have been widely studied, compared with conventional g-C 3 N 4 Bulk photocatalysts exhibit better photocatalytic performance in the photo Fenton reaction than bulk photocatalysts. The two-dimensional ultrathin nanosheets with the porous structures not only provide more pollutant exposure, but also shorten the charge transfer distance and prolong the charge recombination time. Therefore, porous two-dimensional ultrathin g-C with pollutant degradation defects is constructed 3 N 4 Nanoplatelets are very viable.
Based on the background above, we introduce carbon vacancies into porous two-dimensional ultrathin g-C 3 N 4 The nano-sheet, combined with the crystalline Prussian blue nano-particles, can construct the high-efficiency photo-Fenton catalyst with enhanced degradation performance. A series of Prussian blue loaded and carbon vacancy g-C were successfully synthesized by simple hydrothermal methods 3 N 4 (Prussian blue/porous defective g-C) 3 N 4 Nanoplatelets) hybrid catalysts.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the defects existing in the prior art, the invention provides Prussian blue/g-C 3 N 4 Composite photocatalyst, preparation method and application thereof, prussian blue/g-C 3 N 4 The visible light absorption area of the composite photocatalyst is enlarged, the absorption capacity is enhanced, the visible light utilization rate is high, and the Prussian blue/g-C 3 N 4 The composite photocatalyst has obvious effect on photodegradation of environmental pollutants such as antibiotic medicines, dyes and the like.
The technical scheme is as follows: prussian blue/g-C 3 N 4 The preparation method of the composite photocatalyst comprises the following steps:
step one: dissolving urea in deionized water, heating to 30deg.C, transferring the solution into a ceramic crucible with a cover, and calcining at high temperature to obtain product g-C 3 N 4 Wherein the mass ratio of urea to deionized water is 1:1;
step two: polyvinylpyrrolidone, potassium ferricyanide and the product g-C prepared in the step one 3 N 4 Dropwise adding into HCl solution to obtain suspension, placing the suspension into a stainless steel autoclave for hydrothermal reaction to obtain a product g-C 3 N 4 The mass ratio of polyvinylpyrrolidone to potassium ferricyanide is (50-350) to (2500-3500) to (25-28), 1mg of product g-C 3 N 4 Corresponds to (0.08-0.35) mLHCl solution.
Step three: after the reaction of the second step is finished, cooling to room temperature, centrifuging the precipitate, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, and then drying the precipitate in vacuum to obtain Prussian blue/g-C 3 N 4 A composite photocatalyst.
The calcination temperature in the first step is 550 ℃ and the time is 4 hours.
The concentration of the HCl solution in the second step is 0.01mol/L.
The specific procedure for the hydrothermal reaction in step two described above was to place the suspension in a stainless steel autoclave with a 50mL capacity teflon liner and to react in an oven at 80 ℃ for 20h.
And in the third step, the vacuum drying temperature is 60 ℃ and the time is 12 hours.
Prussian blue/g-C as described above 3 N 4 Prussian blue/g-C prepared by preparation method of composite photocatalyst 3 N 4 A composite photocatalyst.
Prussian blue/g-C as described above 3 N 4 Prussian blue/g-C prepared by preparation method of composite photocatalyst 3 N 4 The application of the composite photocatalyst in degrading antibiotic medicines and dye pollutants.
The beneficial effects are that: the Prussian blue/g-C provided by the invention 3 N 4 The composite photocatalyst, the preparation method and the application thereof have the following beneficial effects:
1. the invention is due to g-C 3 N 4 The interfacial interaction with Prussian blue and the synergistic effect of carbon defects effectively improve the utilization rate of the material to visible light, maximize the photogenerated charge transfer efficiency, have stronger charge transfer and conduction capacity, and also keep the higher oxidation-reduction capacity of the material; the visible light absorption capacity of the prepared catalyst is improved, the absorption area is enlarged, and the utilization rate of visible light is improved;
2. the composite photocatalyst prepared by the invention has obvious effect on photodegradation of environmental pollutants such as antibiotic medicines, dyes and the like;
3. the preparation method has the advantages of simplicity in operation, good repeatability, low cost, easiness in condition control and the like;
4. the invention selects urea to prepare g-C at high temperature 3 N 4 Prussian blue loaded and carbon vacancy g-C was synthesized by simple hydrothermal methods 3 N 4 (Prussian blue/porous defective g-C) 3 N 4 Nanosheets) hybridized catalyst, which is applied to degrading environmental pollutants such as antibiotic medicines, dyes and the like, and shows better photocatalytic activity;
5. the invention provides new insight for designing a high-efficiency photoelectric Fenton catalyst for environmental remediation.
Drawings
FIG. 1 shows Prussian blue/g-C 3 N 4 (I) Scanning Electron Microscope (SEM) image of the composite photocatalyst.
FIG. 2 shows Prussian blue/g-C 3 N 4 (I) A composite photocatalyst Transmission Electron Microscope (TEM) image and an energy spectrum element image.
FIG. 3 Prussian blue/g-C 3 N 4 (I) X-ray photoelectron (XPS) spectrum of composite photocatalyst.
FIG. 4 shows Prussian blue/g-C 3 N 4 (I) Composite photocatalyst, g-C 3 N 4 X-ray diffraction (XRD) patterns of prussian blue.
FIG. 5 Prussian blue/g-C 3 N 4 (I) Prussian blue/g-C 3 N 4 (II) and Prussian blue/g-C 3 N 4 The photo-Fenton degradation tetracycline graph of (III).
FIG. 6 shows bulk g-C 3 N 4 、g-C 3 N 4 And Prussian blue/g-C 3 N 4 (I) Is a graph of photo-Fenton degradation of tetracycline.
FIG. 7 shows different Prussian blues/g-C 3 N 4 (I) Photo Fenton degradation tetracycline graph of composite photocatalyst dosage.
FIG. 8 shows Prussian blue/g-C at different pH conditions 3 N 4 (I) Photo Fenton degradation tetracycline graph of composite photocatalyst.
FIG. 9 Prussian blue/g-C 3 N 4 (I) And a degradation rate diagram of the composite photocatalyst for degrading the tetracycline for 20 times.
FIG. 10 shows Prussian blue/g-C 3 N 4 (I) photo-Fenton degradation ciprofloxacin, ranitidine, methylene blue and rhodamine B graph of the composite photocatalyst.
FIG. 11 is bulk g-C 3 N 4 、g-C 3 N 4 And Prussian blue/g-C 3 N 4 (I) Is a diffuse reflection absorption spectrum of ultraviolet-visible light.
FIG. 12 shows bulk g-C 3 N 4 、g-C 3 N 4 And Prussian blue/g-C 3 N 4 (I) Is a photo-current and electrochemical impedance spectrum of (a).
Detailed Description
Example 1
This example provides a Prussian blue/g-C 3 N 4 (I) The preparation method of the composite photocatalyst comprises the following steps:
step one: 20g of urea was dissolved in 20mL of deionized water, warmed to 30℃and then transferred to a ceramic crucible (100 mL) with a lid, and calcined at 550℃for 4h to give the product g-C 3 N 4 ；
Step two: 3g of polyvinylpyrrolidone, 26.4mg of potassium ferricyanide and 172mg of the product obtained in the step one 3 N 4 Dropwise adding the mixture into 30mL of 0.01mol/L HCl solution to obtain a suspension, placing the suspension into a stainless steel autoclave with a 50mL capacity Teflon lining, and placing the stainless steel autoclave into an oven at 80 ℃ for hydrothermal reaction for 20h;
step three: after the reaction of the second step is finished, cooling to room temperature, centrifuging the precipitate, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, and vacuum drying the precipitate for 12 hours at 60 ℃ to obtain Prussian blue/g-C 3 N 4 (I) A composite photocatalyst.
Prussian blue/g-C prepared in this example 3 N 4 (I) SEM image of the composite photocatalyst is shown in FIG. 1, and it can be seen from FIG. 1 that Prussian blue/g-C 3 N 4 (I) The composite photocatalyst has a porous layered structure.
Prussian blue/g-C prepared in this example 3 N 4 (I) TEM image of the composite photocatalyst is shown in FIG. 2, and it can be seen from FIG. 2 that Prussian blue/g-C 3 N 4 (I) Prussian blue Nanoparticles (NPS) having a porous layered structure with a diameter of about 250nm are tightly adhered to the porous g-C 3 N 4 In the above, the apparent and homogeneous Fe signal demonstrates successful doping and homogeneous distribution of prussian blue.
Prussian blue/g-C prepared in this example 3 N 4 (I) The XPS spectrum of the composite photocatalyst is shown in FIG. 3, and as can be seen from FIG. 3,prussian blue/g-C 3 N 4 (I) The successful loading of Prussian blue was confirmed by having C, N, O and Fe elements, with two peaks 705.1eV and 717.8eV appearing in the Fe2p spectrum corresponding well to Fe2p3/2 and Fe2p 1/2.
Prussian blue/g-C prepared in this example 3 N 4 (I) As can be seen from FIG. 4, the XRD spectrum of the composite photocatalyst is shown in FIG. 4, prussian blue/g-C 3 N 4 (I) Has Prussian blue and g-C 3 N 4 Characteristic peaks of the two prove Prussian blue/g-C 3 N 4 (I) Successful synthesis of the composite photocatalyst.
Example 2
Example 2 differs from example 1 in that: g-C in step two 3 N 4 The mass of polyvinylpyrrolidone and potassium ferricyanide are 344mg, 3g and 26.4mg respectively.
This example gives Prussian blue/g-C 3 N 4 (II) composite photocatalyst.
Example 3
Example 3 differs from example 1 in that: g-C in step two 3 N 4 The mass of polyvinylpyrrolidone and the mass of potassium ferricyanide are 86mg, 3g and 26.4mg respectively.
This example gives Prussian blue/g-C 3 N 4 (III) composite photocatalyst.
Prussian blue/g-C prepared in examples 1, 2 and 3 3 N 4 (I) Prussian blue/g-C 3 N 4 (II) Prussian blue/g-C 3 N 4 (III) the three composite photocatalysts are subjected to performance test, and the process and the result are as follows:
prussian blue/g-C 3 N 4 (I) Prussian blue/g-C 3 N 4 (II) Prussian blue/g-C 3 N 4 (III) 50mg each, then added to 30mL50mg/L tetracycline solution, and stirred continuously for 30min to bring the suspension to adsorption equilibrium. Then 150 mu L H was added to the suspension 2 O 2 (30%). Retraction at specific time intervals and desired time intervals using a 0.45mm syringeTwo milliliter aliquots were collected. The concentration was assessed by taking the supernatant after centrifugation of the suspension and recording the maximum absorbance with a UV-vis spectrophotometer. The resulting tetracycline degradation graph is shown in FIG. 5. As can be seen from FIG. 5, after 120min of illumination, prussian blue/g-C 3 N 4 (I) Prussian blue/g-C 3 N 4 (II) Prussian blue/g-C 3 N 4 (III) is above 85%, wherein Prussian blue/g-C 3 N 4 (I) The highest photocatalytic efficiency.
In addition, bulk g-C was taken separately 3 N 4 (homemade), g-C 3 N 4 (homemade), prussian blue/g-C 3 N 4 (I) 50mg each was then added to 30ml of 50mg/L tetracycline solution, and the suspension was allowed to reach adsorption equilibrium by continuous stirring for 30 min. Then 150. Mu. LH was added to the suspension 2 O 2 (30%). Two milliliter aliquots were collected at specific time intervals and at desired intervals using a 0.45mm syringe. The concentration was assessed by taking the supernatant after centrifugation of the suspension and recording the maximum absorbance with a UV-vis spectrophotometer. The resulting tetracycline degradation graph is shown in FIG. 6. As can be seen from FIG. 6, after 120min of illumination, prussian blue/g-C 3 N 4 (I) The degradation effect on the tetracycline is highest, and the degradation rate can reach about 93.3 percent. Single catalyst bulk-C 3 N 4 And g-C 3 N 4 The degradation to tetracycline is lower, and the photocatalysis efficiency of the composite material is obviously higher than that of a single catalyst.
bulk g-C 3 N 4 The preparation method of the (self-made) comprises the following steps: transferring 3g melamine into a covered ceramic crucible, and calcining at 550 ℃ to obtain bulk-C product 3 N 4 。
g-C 3 N 4 (homemade) is the product obtained in step one of example 1.
And, for Prussian blue/g-C prepared in example 1 3 N 4 (I) The composite photocatalyst has the following processes and results after specific tests are carried out on each influencing factor:
(1) Degradation efficiency and Prussian blue/g-C 3 N 4 (I) Adding inRelation of quantity
Prussian blue/g-C 3 N 4 (I) 1mg, 5mg, 10mg, 25mg and 50mg of the suspension are respectively taken and then respectively added into 30mL of 50mg/L tetracycline solution, and the suspension is continuously stirred for 30min to reach adsorption equilibrium. Then 150. Mu. LH was added to the suspension 2 O 2 (30%). Two milliliter aliquots were collected at specific time intervals and at desired intervals using a 0.45mm syringe. The concentration was assessed by taking the supernatant after centrifugation of the suspension and recording the maximum absorbance with a UV-vis spectrophotometer. The resulting tetracycline degradation graph is shown in FIG. 7. As can be seen from FIG. 7, after 120min of illumination, prussian blue/g-C 3 N 4 (I) The degradation effect on the tetracycline is positively correlated with the addition amount.
(2) Relation between visible light degradation performance and acid and alkali conditions
50mg Prussian blue/g-C 3 N 4 (I) Adding into 30mL of 50mg/L tetracycline solution, adjusting pH to 3-9, and continuously stirring for 30min to make the suspension reach adsorption equilibrium. Then 150. Mu. LH was added to the suspension 2 O 2 (30%). Two milliliter aliquots were collected at specific time intervals and at desired intervals using a 0.45mm syringe. The concentration was assessed by taking the supernatant after centrifugation of the suspension and recording the maximum absorbance with a UV-vis spectrophotometer. The resulting tetracycline degradation graph is shown in FIG. 8. As can be seen from FIG. 8, after 120min of illumination, the pH value of the solution is between 3 and 9, prussian blue/g-C 3 N 4 All are more than 89.6%, and the degradation efficiency is high. When the pH of the solution is 7, the degradation efficiency can reach 98.4 percent. Description Prussian blue/g-C 3 N 4 Has good visible light degradation performance under acidic or weak alkaline conditions.
(3) Cyclic degradation of tetracycline
Prussian blue/g-C prepared from example 1 3 N 4 (I) The results of the photocatalytic experiment for circularly degrading tetracycline by the composite photocatalyst are shown in fig. 9. As can be seen from fig. 9, the photocatalyst was not significantly deactivated after 20 consecutive cycles. The stability is good, and the environment purification has huge potential valueValues.
(4) Universality of application
50mg Prussian blue/g-C 3 N 4 (I) Respectively adding into 30mL of 50mg/L ciprofloxacin, ranitidine, methylene blue and rhodamine solution, and continuously stirring for 30min to ensure that the suspension reaches adsorption equilibrium. Then 150 mu L H was added to the suspension 2 O 2 (30%). Two milliliter aliquots were collected at specific time intervals and at desired intervals using a 0.45mm syringe. The concentration was assessed by taking the supernatant after centrifugation of the suspension and recording the maximum absorbance with a UV-vis spectrophotometer. The resulting degraded ciprofloxacin, ranitidine, methylene blue and rhodamine solutions are shown in the graph of fig. 10. As can be seen from FIG. 10, after 120min of illumination, the degradation efficiencies of ciprofloxacin, ranitidine, methylene blue and rhodamine can reach 59.8%, 98.4%, 99.4% and 100.0%, respectively, and the results show that Prussian blue/g-C 3 N 4 Has good universality.
(5) Visible light absorption capacity, absorption region
The light absorption characteristics of the different samples were measured using uv-vis diffuse reflectance spectroscopy as shown in fig. 11. As can be seen from FIG. 11, prussian blue/g-C was confirmed 3 N 4 (I) The composite material has Prussian blue and g-C 3 N 4 And Prussian blue/g-C 3 N 4 Has wider and stronger light absorption, which indicates improved light collection after Prussian blue loading, prussian blue/g-C 3 N 4 (I) The visible light absorption capacity of (a) is also improved and the absorption area is also widened.
(6) Charge transfer and conductivity capabilities
The photocurrent testing process comprises the following steps: 2.0mg of the sample was ultrasonically dispersed in 50. Mu.L of ethanol, 10. Mu.L of Nafion solution (5 wt%) and 50. Mu.L of ultra pure water to form a uniform slurry, and 20. Mu.L of the slurry was dropped to deposit on the FTO electrode. FTP electrode, platinum sheet and saturated Ag/AgCl deposited by slurry are used as working electrode, counter electrode and reference electrode. Using 300W Xe lamps (truncated lambda)<420 nm) and Na 2 SO 4 (0.5M) as light source and electrolyte, CHI66 was used in the analysis of photocurrent over timeThe 0C electrochemical workstation collects photocurrent data.
Electrochemical impedance spectroscopy testing process: on the CHI760e workstation, a standard three electrode system (Pt foil, ag/AgCl and working electrode, electrolyte 0.1M K was used 4 Fe(CN) 6 ·3H 2 O、0.1M K 3 [Fe(CN) 6 ]0.1M KCl mixed solution), 5 mu L of slurry is added dropwise to a working electrode, and electrochemical impedance spectrum is measured under the open circuit potential range of 0.01-1000 kHz.
The test results of the photocurrent and electrochemical impedance spectra are shown in FIG. 12, and it can be seen from FIG. 12 that Prussian blue/g-C is loaded with Prussian blue 3 N 4 (I) The highest photocurrent response and the smallest arc radius are shown, which show that the synergistic effect of Prussian blue and carbon defects maximizes photogenerated charge transfer efficiency and has the strongest charge transfer and conduction capacity.
While the embodiments of the present invention have been described in detail, those skilled in the art should not understand that the present invention is limited to the specific embodiments and applications.
Claims (7)
1. Prussian blue/g-C 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps:
step one: dissolving urea in deionized water, heating to 30deg.C, transferring the solution into a ceramic crucible with a cover, and calcining at high temperature to obtain product g-C 3 N 4 Wherein the mass ratio of urea to deionized water is 1:1;
step two: polyvinylpyrrolidone, potassium ferricyanide and the product g-C prepared in the step one 3 N 4 Dropwise adding into HCl solution to obtain suspension, placing the suspension into a stainless steel autoclave for hydrothermal reaction, wherein the product g-C 3 N 4 The mass ratio of polyvinylpyrrolidone to potassium ferricyanide is (1-7) to (50-70) to (0.5-0.56), 1mg of product g-C 3 N 4 Corresponding to (0.08-0.35) mL of HCl solution;
step three: after the reaction of the second step is finished, cooling to room temperature, centrifuging the precipitate, washing the precipitate with deionized water and absolute ethyl alcohol for three times respectively, and then drying the precipitate in vacuum to obtain Prussian blue/g-C 3 N 4 A composite photocatalyst.
2. Prussian blue/g-C according to claim 1 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps: the calcination temperature in the first step is 550 ℃ and the time is 4 hours.
3. Prussian blue/g-C according to claim 1 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps: the concentration of the HCl solution in the second step is 0.01mol/L.
4. Prussian blue/g-C according to claim 1 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps: the specific process of the hydrothermal reaction in the step two is that the suspension is placed in a stainless steel autoclave with a teflon liner with a capacity of 50mL and placed in an oven at 80 ℃ for reaction for 20h.
5. Prussian blue/g-C according to claim 1 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps: and in the third step, the vacuum drying temperature is 60 ℃ and the time is 12 hours.
6. Prussian blue/g-C according to any one of claims 1-5 3 N 4 Prussian blue/g-C prepared by preparation method of composite photocatalyst 3 N 4 A composite photocatalyst.
7. Prussian blue/g-C according to any one of claims 1-5 3 N 4 Prussian blue/g-C prepared by preparation method of composite photocatalyst 3 N 4 Composite photocatalyst in degradation of antibiotic medicines and dye pollutantsApplication.
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