CN115463654B - Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, preparation method and application - Google Patents

Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, preparation method and application Download PDF

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CN115463654B
CN115463654B CN202211054775.8A CN202211054775A CN115463654B CN 115463654 B CN115463654 B CN 115463654B CN 202211054775 A CN202211054775 A CN 202211054775A CN 115463654 B CN115463654 B CN 115463654B
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nano
loaded
photocatalyst
icosahedron
sheet
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CN115463654A (en
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王文霞
刘小丰
陈炜睿
金保胜
陈浠
蒙振邦
李震
周丽华
何其
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Guangdong University of Technology
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    • B01J35/39—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • 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
    • B01J23/50—Silver
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/04—Disinfection
    • 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
    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
    • 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
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The application belongs to the technical field of photocatalytic materials, and particularly relates to Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, and preparation method and application thereof; pd-Ag loaded g-C provided herein 3 N 4 In the nano-sheet photocatalyst, both nano Pd and nano Ag can promote g-C 3 N 4 Effective separation of photogenerated carriers to enhance g-C 3 N 4 The nano Pd icosahedron and the nano Ag cube can be loaded on g-C by physically mixing reactant suspension through magnetic stirring according to the photocatalytic activity of the nano-sheet photocatalyst 3 N 4 Nano-sheet surface, g-C 3 N 4 The nano-sheets have no agglomeration and large specific surface area, and meanwhile, the nano Pd icosahedron and the nano Ag cube are uniformly dispersed in the g-C 3 N 4 On the nano-sheet substrate, thereby solving the problem of g-C based in the prior art 3 N 4 The technical problem that the photocatalytic sterilization performance of the semiconductor photocatalyst needs to be improved.

Description

Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, preparation method and application
Technical Field
The application belongs to the technical field of photocatalytic materials, and particularly relates to a Pd-Ag loaded g-C3N4 nanosheet photocatalyst, a preparation method and application thereof.
Background
The large number of pathogenic microorganisms present in the wastewater may cause cholera, dysentery, schistosomiasis, etc., and thus, it is necessary to kill the pathogenic microorganisms as much as possible before the wastewater is discharged into the environment.
The traditional method for killing pathogenic microorganisms in wastewater is a chlorine disinfection method, an ultraviolet radiation method and the like, however, the traditional method has the defects that the chlorine disinfection method is easy to generate chlorinated disinfection byproducts with cancerogenic action in the process of killing pathogenic microorganisms in wastewater, the ultraviolet radiation method has poor penetrating effect, the pathogenic microorganisms in the wastewater are killed and revived easily due to low effect, and the heterogeneous photocatalytic disinfection technology based on the semiconductor photocatalyst can generate active oxygen to inhibit the growth of harmful microorganisms, so that the method is a green environment-friendly disinfection method, has the advantages of strong disinfection capability, no toxic byproducts, realization of self-purification of a system and the like, and is a widely applied method for killing pathogenic microorganisms in wastewater.
g-C 3 N 4 The semiconductor has the advantages of narrow forbidden bandwidth (eg=2.70 eV), good stability, high visible light utilization rate, easy modification and the like, so that the semiconductor shows excellent performances in the aspects of hydrolysis, photocatalytic sterilization and the like, however, g-C 3 N 4 Semiconductor photogenerated carriersIs inefficient in the separation, which results in g-C based 3 N 4 The performance of the semiconductor photocatalyst is to be improved.
Disclosure of Invention
In view of this, the present application provides a Pd-Ag supported g-C 3 N 4 Nanosheet photocatalyst, preparation method and application thereof, and is used for solving the problem of g-C-based in the prior art 3 N 4 The technical problem that the photocatalytic sterilization performance of the semiconductor photocatalyst needs to be improved.
The first aspect of the present application provides a Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, comprising g-C 3 N 4 Nanoplatelets and nanoplatelets;
the g-C 3 N 4 The nanosheets support the nano Pd and the nano Ag.
Preferably, the nano Pd is nano Pd icosahedron;
the nanometer Ag is a nanometer Ag cube.
In a second aspect, the present application provides a Pd-Ag loaded g-C 3 N 4 The preparation method of the nano-sheet photocatalyst comprises the following steps:
step S1, g-C 3 N 4 Mixing the nanosheet suspension with the nano Pd icosahedron suspension, and then carrying out a first magnetic stirring reaction to obtain the g-C loaded with nano Pd icosahedron 3 N 4 A nanosheet;
s2, loading the nano Pd icosahedron g-C 3 N 4 The nanosheets and the nano Ag cube suspension undergo a second magnetic stirring reaction to obtain Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst;
wherein the time of the first magnetic stirring reaction is 24-36 hours, and the temperature is room temperature;
the second magnetic stirring reaction time is 24-36 hours, and the temperature is room temperature.
It should be noted that the Pd-Ag loaded g-C provided by the application 3 N 4 The preparation method of the nano-sheet photocatalyst has simple process and only needs magnetic stirring physical mixing reactionThe nano Pd icosahedron and the nano Ag cube can be loaded on the g-C by the suspension 3 N 4 The nano-sheet surface has low cost, good repeatability and low energy consumption, and avoids the need of a photochemical reaction device and inert gas N in the traditional photo-reduction deposition method 2 The preparation conditions caused by protection are harsh, and the Pd-Ag loaded g-C provided by the application 3 N 4 g-C prepared by nano-sheet photocatalyst preparation method 3 N 4 The nano-sheets are free from agglomeration, the specific surface area is large, and meanwhile, the nano-Pd icosahedron and the nano-Ag cube are uniformly distributed, and the nano-Pd icosahedron and the nano-Ag cube are stable in attachment and are not easy to fall off.
Preferably, after the first magnetic stirring reaction is carried out, the g-C of the nano Pd icosahedron is obtained 3 N 4 Before the nano-sheet, the method further comprises: centrifugal filtration, washing and drying;
after the second magnetic stirring reaction, pd-Ag loaded g-C is obtained 3 N 4 Before the nanosheet photocatalyst, further comprises: centrifugal filtration, washing and drying.
Preferably, the g-C 3 N 4 The concentration of the nano-sheet suspension is 0.5-1.0 mg/mL, and the concentration of the nano-Pd icosahedron suspension is 0.1-0.3 mg/mL.
Preferably, the concentration of the nano Ag cube suspension is 0.5-1.0 mg/mL, and the nano Pd icosahedron loaded g-C 3 N 4 The concentration of the nano-sheet is 0.5-1.0 mg/mL.
Preferably, the g-C 3 N 4 The preparation method of the nanosheet suspension comprises the following steps: will g-C 3 N 4 The nano-sheet is placed in deionized water, and is dispersed by ultrasonic to obtain g-C 3 N 4 Nanosheet suspension.
Preferably, the preparation method of the nano Pd icosahedron suspension comprises the following steps: and placing the nano Pd icosahedron in deionized water, and performing ultrasonic dispersion to obtain nano Pd icosahedron suspension.
Preferably, the preparation method of the nano Ag cube suspension comprises the following steps: and placing the nano Ag cube in deionized water, and performing ultrasonic dispersion to obtain nano Ag cube suspension.
Preferably, the nano Pd icosahedral-supported g-C 3 N 4 The preparation method of the nanosheet suspension comprises the following steps: g-C of nano Pd icosahedron 3 N 4 The nano-sheet is placed in deionized water, and ultrasonic dispersion is carried out to obtain g-C of the nano Pd icosahedron 3 N 4 Nanosheet suspension.
In a third aspect the present application provides a Pd-Ag loaded g-C 3 N 4 The application of the nano-sheet photocatalyst in photocatalysis and microorganism killing.
Preferably, the microorganisms include bacteria, viruses and fungi.
Preferably, the bacteria include escherichia coli and staphylococcus aureus.
Preferably, the application specifically includes: pd-Ag loaded g-C with concentration of 1.0-1.5 mg/mL 3 N 4 The nano-sheet photocatalyst is added into a system containing microorganisms, and the microorganisms are killed by photocatalysis under the irradiation of ultraviolet light.
In summary, the present application provides a Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, preparation method and application thereof, pd-Ag loaded g-C 3 N 4 The nanosheet photocatalyst comprises g-C 3 N 4 Nanosheets and nano Pd and nano Ag loaded by nanosheets, wherein both nano Pd and nano Ag can promote g-C 3 N 4 Effective separation of photogenerated carriers to enhance g-C 3 N 4 Performance of nanosheet photocatalyst photocatalytic Activity, and g-C 3 N 4 The nano-sheets have no agglomeration and large specific surface area, and simultaneously, nano Pd and nano Ag are uniformly dispersed in g-C 3 N 4 On the nanoplatelet substrate, so that the Pd-Ag loaded g-C provided by the application 3 N 4 The nano-sheet has excellent photocatalytic activity, and is obvious in inactivation efficiency on escherichia coli under irradiation of visible light, so that the problem of g-C-based in the prior art is solved 3 N 4 The technical problem that the photocatalytic sterilization performance of the semiconductor photocatalyst needs to be improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the g-C of the nano Pd-loaded icosahedron prepared in example 1 of the present invention 3 N 4 Transmission Electron Microscope (TEM) images of the nanoplatelets;
FIG. 2 shows Pd-Ag-supported g-C prepared in example 1 of the present invention 3 N 4 Transmission Electron Microscope (TEM) images of the nanoplatelets photocatalyst;
FIG. 3 shows the g-C of example 1 of the present invention 3 N 4 Nanosheets and g-C loaded with nano Pd icosahedron 3 N 4 Nanosheets and Pd-Ag loaded g-C 3 N 4 XRD pattern of nanoplatelet photocatalyst;
FIG. 4 shows the growth of E.coli on agar plates in the absence of a catalyst for various periods of time under the action of visible light: a, b, c, d, e, f, g represent 0,10,20,30,40,50,60min, respectively;
FIG. 5 shows the Pd-Ag supported g-C of E.coli 3 N 4 The growth states of the nano-sheet photocatalyst on the agar plate under the action of visible light for different times are a, b, c, d, e, f and g respectively represent 0,10,20,30,40,50 and 60min;
FIG. 6 g-C using Pd-Ag loading 3 N 4 The nanosheet photocatalyst can be used for treating Escherichia coli (1×10) under irradiation of visible light 7 CFU/mL,50 mL).
Detailed Description
The application provides a Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, preparation method and application thereof, and is used for solving the problem of g-C-based in the prior art 3 N 4 The technical problem that the photocatalytic sterilization performance of the semiconductor photocatalyst needs to be improved.
The following description of the embodiments of the present application will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
Example 1
The embodiment of the application provides a Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, the photocatalyst comprising g-C 3 N 4 Nanoplatelets and nanoplatelets; and g-C 3 N 4 Nano-sheet loaded nano Pd and nano Ag form Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, because noble metals Pd and Ag can promote g-C 3 N 4 Efficient separation of photogenerated carriers, thereby enabling Pd-Ag loaded g-C provided herein 3 N 4 The nanosheet photocatalyst has excellent photocatalytic activity and is loaded on g-C 3 N 4 The noble metal on the nano-sheet photocatalyst comprises Ag, so that compared with the method for only loading Pd, the preparation cost of the photocatalyst is saved, and the nano-sheet photocatalyst has excellent photocatalytic activity, so that the practical application value is high.
For a load in g-C 3 N 4 The nanometer Pd and nanometer Ag on the surface of the nanometer sheet are preferably selected from nanometer Pd icosahedron and nanometer Ag cube, and the nanometer Pd icosahedron and nanometer Ag cube provided by the application can be uniformly dispersed in g-C 3 N 4 On the nano-sheet substrate, and g-C 3 N 4 The nano-sheets are not agglomerated, so that the Pd-Ag loaded g-C provided by the application 3 N 4 The nano-sheet photocatalyst has higher specific surface area, and further improves the Pd-Ag loaded g-C 3 N 4 Photocatalytic activity of nanoplatelets photocatalyst.
Example 2
The embodiment of the application provides a Pd-Ag loaded g-C 3 N 4 The preparation method of the nano-sheet photocatalyst comprises the following steps: preparation of g-C carrying nano Pd icosahedron 3 N 4 Nanoplatelets and preparation of Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
Step 1, preparing g-C of nano Pd-loaded icosahedron 3 N 4 The nano-sheet comprises the steps of: 234mg of g-C is prepared by a thermal polymerization method and is peeled off by ultrasonic wave of glucose solution 3 N 4 Dispersing the nanosheets in 468mL deionized water, and placing the nanosheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nanosheets to obtain g-C with the concentration of 0.5mg/mL 3 N 4 Dispersing the nano-sheet suspension and the Pd icosahedron prepared from 31mg of Pd precursor in 36mL of deionized water, and placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the mixture so as to obtain nano-Pd icosahedron suspension; and then g-C 3 N 4 The nano-sheet suspension and the nano-Pd icosahedron suspension are divided into two parts averagely, and are magnetically stirred for 24 hours respectively, centrifugally washed and dried after the reaction is finished to obtain the g-C loaded with nano-Pd icosahedron 3 N 4 A nano-sheet.
Step 2, preparation of Pd-Ag Supported g-C 3 N 4 The nano-sheet photocatalyst comprises the following steps: dispersing 30mg of prepared nano Ag cube in 36mL of deionized water, placing in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano Ag cube to obtain nano Ag cube suspension and loading 234mg of nano Pd icosahedron g-C 3 N 4 Dispersing the nano-sheets in 468mL deionized water, and placing the nano-sheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano-sheets so as to obtain g-C loaded with nano Pd icosahedron with the concentration of 0.5mg/mL 3 N 4 Nanosheet suspension; then the nano Ag cube suspension and the nano Pd icosahedron loaded g-C are mixed 3 N 4 The nanosheet suspension is mixed and divided into two parts evenly and magnetically stirred for 24 hours respectively. Centrifugal washing and drying after the reaction is finished to obtain Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
For g-C in steps 1, 2 3 N 4 Nanosheets and g-C loaded with nano Pd icosahedron 3 N 4 Nanoplatelets and Pd-Ag loaded g-C 3 N 4 As can be seen from FIG. 3, the nano-Pd two were physically mixed by magnetic stirring, as can be seen from FIG. 3, by X-ray diffraction spectroscopy analysis of the nano-sheet photocatalystDecahedral suspension and g-C 3 N 4 The nano Pd icosahedron can be loaded on g-C by the nano sheet suspension 3 N 4 The nano-Pd icosahedron-loaded g-C is prepared on the surface of the nano-sheet 3 N 4 Nano sheet, then loading nano Pd icosahedron g-C 3 N 4 The nanosheet suspension and the nanosheet suspension are magnetically stirred and physically mixed, so that the nanosheet suspension and the nanosheet suspension can be loaded on the g-C of the nano Pd icosahedron 3 N 4 The surface of the nano sheet is provided with Pd-Ag loaded g-C 3 N 4 The nano-sheet photocatalyst can load nano Pd icosahedron and nano Ag cube to g-C by magnetically stirring and physically mixing reactant suspension 3 N 4 The nano-sheet surface has low cost, good repeatability and low energy consumption, and avoids the need of a photochemical reaction device and inert gas N in the traditional photo-reduction deposition method 2 The test conditions resulting from the protection are severe.
g-C for Pd-Ag loading in step 2 3 N 4 The result of electron microscope analysis of the nanosheet photocatalyst is shown in fig. 1-2, and g-C can be seen from the graph 3 N 4 The nano sheet maintains the original ultrathin sheet structure, no agglomeration exists, and the nano Pd icosahedron and Ag cube are uniformly dispersed in g-C 3 N 4 No obvious agglomeration exists on the nano-sheet substrate, which indicates the g-C prepared by the preparation method 3 N 4 The nano-sheets have no agglomeration and large specific surface area, and the loaded nano Pd icosahedron and nano Ag cube are uniformly distributed, and are stable in attachment and not easy to fall off, so that the g-C 3 N 4 The nano-sheet photocatalyst has excellent photocatalytic activity.
Example 3
The embodiment of the application provides a Pd-Ag loaded g-C 3 N 4 The preparation method of the nano-sheet photocatalyst comprises the following steps: preparation of g-C carrying nano Pd icosahedron 3 N 4 Nanosheets and preparation of Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
Step 1, preparing g-C of nano Pd-loaded icosahedron 3 N 4 The nano-sheet comprises the steps of: 234mg of g-C is prepared by a thermal polymerization method and is peeled off by ultrasonic wave of glucose solution 3 N 4 Dispersing the nanosheets in 468mL deionized water, and placing the nanosheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nanosheets to obtain g-C with the concentration of 0.5mg/mL 3 N 4 Dispersing the nano-sheet suspension and the Pd icosahedron prepared from 15.5mg of Pd precursor in 36mL of deionized water, and placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the mixture so as to obtain nano-Pd icosahedron suspension; and then g-C 3 N 4 The nano-sheet suspension and the nano-Pd icosahedron suspension are divided into two parts averagely, and are magnetically stirred for 24 hours respectively, centrifugally washed and dried after the reaction is finished to obtain the g-C loaded with nano-Pd icosahedron 3 N 4 A nano-sheet.
Step 2, preparation of Pd-Ag Supported g-C 3 N 4 The nano-sheet photocatalyst comprises the following steps: dispersing 30mg of prepared nano Ag cube in 36mL of deionized water, placing in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano Ag cube to obtain nano Ag cube suspension and loading 234mg of nano Pd icosahedron g-C 3 N 4 Dispersing the nano-sheets in 468mL deionized water, and placing the nano-sheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano-sheets so as to obtain g-C loaded with nano Pd icosahedron with the concentration of 0.5mg/mL 3 N 4 Nanosheet suspension; then the nano Ag cube suspension and the nano Pd icosahedron loaded g-C are mixed 3 N 4 Mixing the nanosheet suspension, dividing into two parts, magnetically stirring for 24 hr, centrifuging, washing, and oven drying to obtain Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
Example 4
The embodiment of the application provides a Pd-Ag loaded g-C 3 N 4 The preparation method of the nano-sheet photocatalyst comprises the following steps: preparation of g-C carrying nano Pd icosahedron 3 N 4 Nanosheets and preparation of Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
Step 1, preparing g-C of nano Pd-loaded icosahedron 3 N 4 The nano-sheet comprises the steps of: firstly taking234mg of g-C prepared by thermal polymerization and peeled off by ultrasonic with glucose solution 3 N 4 Dispersing the nanosheets in 468mL deionized water, and placing the nanosheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nanosheets to obtain g-C with the concentration of 0.5mg/mL 3 N 4 Dispersing the nano-sheet suspension and the Pd icosahedron prepared by 46.5mg of Pd precursor in 36mL of deionized water, and placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the mixture so as to obtain nano-Pd icosahedron suspension; and then g-C 3 N 4 The nano-sheet suspension and the nano-Pd icosahedron suspension are divided into two parts averagely, and are magnetically stirred for 24 hours respectively, centrifugally washed and dried after the reaction is finished to obtain the g-C loaded with nano-Pd icosahedron 3 N 4 A nano-sheet.
Step 2, preparation of Pd-Ag Supported g-C 3 N 4 The nano-sheet photocatalyst comprises the following steps: dispersing 30mg of prepared nano Ag cube in 36mL of deionized water, placing in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano Ag cube to obtain nano Ag cube suspension and loading 234mg of nano Pd icosahedron g-C 3 N 4 Dispersing the nano-sheets in 468mL deionized water, and placing the nano-sheets in an ultrasonic cleaner for ultrasonic treatment for 30min to uniformly disperse the nano-sheets so as to obtain g-C loaded with nano Pd icosahedron with the concentration of 0.5mg/mL 3 N 4 Nanosheet suspension; then the nano Ag cube suspension and the nano Pd icosahedron loaded g-C are mixed 3 N 4 Mixing the nanosheet suspension, dividing into two parts, magnetically stirring for 24 hr, centrifuging, washing, and oven drying to obtain Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst.
Test example 1
This test example is a Pd-Ag supported g-C prepared in test example 2 3 N 4 The sterilization performance of the nano-sheet photocatalyst under the photocatalysis condition is tested, and the test comprises the following steps: preparation of E.coli suspension and Pd-Ag Supported g-C 3 N 4 And (3) performing photocatalysis sterilization test on the nanosheet photocatalyst.
Step 1, preparing escherichia coli bacterial suspension, which comprises the following steps: one E.coli colony was picked and incubated in 50mL LB liquid medium for 12 hours at 37℃and 220 RPM.Cell count was about 1X 10 9 Colony forming unit (CFU/mL), centrifuging 5mL of bacterial liquid at 8000RPM and 25deg.C for 2min, separating Escherichia coli from LB liquid medium, dispersing Escherichia coli into 5mL of sterilized normal saline, centrifuging at 5000RPM and 25deg.C for 4min, washing, discarding supernatant, adding 5mL of sterilized normal saline to obtain initial bacterial liquid, and measuring OD of the initial bacterial liquid by ultraviolet spectrophotometer 600 The absorbance is 1.0 to 1.2A. Diluting the initial bacterial solution with physiological saline to make its absorbance approach 0.1A, at this time, the concentration of the coliform bacterial solution is about 1×10 8 CFU/mL。
Step 2 Pd-Ag Supported g-C 3 N 4 The nano-sheet photocatalyst photocatalytic sterilization test comprises the following steps: firstly, mixing two identical parts of coliform bacteria liquid with absorbance close to 0.1A and 45mL of sterilized normal saline respectively, wherein one part of the coliform bacteria liquid is added with 50mg of Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst, another part of the nanosheet photocatalyst without photocatalyst added is used as a blank control test, wherein Pd-Ag loaded g-C 3 N 4 The concentration of the nano-sheet photocatalyst in an agar plate after adding is 1mg/mL, a 300W xenon lamp with a 420nm ultraviolet cut-off filter is used as a photocatalysis light source, 100 mu L of bacterial suspension is taken out respectively at 0,10,20,30,40,50 and 60 minutes under the irradiation of the light source, 100 mu L of bacterial suspension is evenly coated on LB solid culture medium after 10 multiplied by 10, each sterilizing plate is repeated for 3 times, then the culture is carried out in a constant temperature incubator at 37 ℃ for 24 hours, and the g-C of Pd-Ag load is evaluated by observing the colony number of escherichia coli 3 N 4 The antibacterial activity of the nanosheet photocatalyst.
As a result, as shown in FIGS. 4 to 6, it can be seen from FIGS. 4 to 5 that Pd-Ag-loaded g-C is added as shown in FIG. 5, compared with the blank test in FIG. 4 in which no photocatalyst is added 3 N 4 The nanosheet photocatalyst can be used for preparing 10% of the photocatalyst in 60min under the action of visible light 8 The CFU/mL colibacillus is completely killed, and the photocatalytic sterilization activity is obvious.
The above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims (4)

1. Pd-Ag loaded g-C 3 N 4 The application of the nano-sheet photocatalyst in photocatalysis and killing of microorganism escherichia coli is characterized by comprising g-C 3 N 4 Nanoplatelets and nanoplatelets;
the g-C 3 N 4 The nanosheets load the nano Pd and the nano Ag;
the nano Pd is nano Pd icosahedron;
the nano Ag is a nano Ag cube;
the preparation method of the photocatalyst comprises the following steps:
step S1, g-C 3 N 4 Mixing the nanosheet suspension with the nano Pd icosahedron suspension, and then carrying out a first magnetic stirring reaction to obtain the g-C loaded with nano Pd icosahedron 3 N 4 A nanosheet;
s2, loading the nano Pd icosahedron g-C 3 N 4 The nanosheets and the nano Ag cube suspension undergo a second magnetic stirring reaction to obtain Pd-Ag loaded g-C 3 N 4 Nanosheet photocatalyst;
wherein the time of the first magnetic stirring reaction is 24-36 hours, and the temperature is room temperature;
the second magnetic stirring reaction time is 24-36 hours, and the temperature is room temperature.
2. A Pd-Ag supported g-C according to claim 1 3 N 4 The application of the nano-sheet photocatalyst in photocatalysis and killing of microorganism escherichia coli is characterized in that the g-C 3 N 4 The concentration of the nanosheet suspension is 0.5-1.0 mg/mL, and the nano Pd icosahedron suspensionThe concentration of the liquid is 0.1-0.3 mg/mL.
3. A Pd-Ag supported g-C according to claim 1 3 N 4 The application of the nano-sheet photocatalyst in the photocatalysis and killing of microorganism escherichia coli is characterized in that after the first magnetic stirring reaction, the g-C of the nano Pd icosahedron is obtained 3 N 4 Before the nano-sheet, the method further comprises: centrifugal filtration, washing and drying;
after the second magnetic stirring reaction, pd-Ag loaded g-C is obtained 3 N 4 Before the nanosheet photocatalyst, further comprises: centrifugal filtration, washing and drying.
4. Pd-Ag loaded g-C according to claim 1 3 N 4 The application of the nano-sheet photocatalyst in the photocatalysis and killing of microorganism escherichia coli is characterized in that Pd-Ag loaded g-C with the concentration of 1.0-1.5 mg/mL 3 N 4 The nano-sheet photocatalyst is added into a system containing microorganism escherichia coli, and the microorganism escherichia coli is killed by photocatalysis under the irradiation of visible light.
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