CN113477262A - Preparation method and application of silver chromate/zinc ferrite fibrous composite photocatalyst - Google Patents
Preparation method and application of silver chromate/zinc ferrite fibrous composite photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 60
- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 38
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- OJKANDGLELGDHV-UHFFFAOYSA-N disilver;dioxido(dioxo)chromium Chemical compound [Ag+].[Ag+].[O-][Cr]([O-])(=O)=O OJKANDGLELGDHV-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 33
- 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 claims abstract description 22
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 22
- 241000607142 Salmonella Species 0.000 claims abstract description 14
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 14
- 238000000975 co-precipitation Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 11
- 244000005700 microbiome Species 0.000 claims abstract description 10
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 6
- 239000011701 zinc Substances 0.000 claims description 55
- 239000000243 solution Substances 0.000 claims description 49
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 238000009987 spinning Methods 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 8
- 239000001963 growth medium Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 230000001580 bacterial effect Effects 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000012258 culturing Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 230000001954 sterilising effect Effects 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 101710134784 Agnoprotein Proteins 0.000 claims description 3
- 238000002835 absorbance Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000002609 medium Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 3
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 claims description 2
- 230000001788 irregular Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000000975 dye Substances 0.000 claims 3
- 244000052616 bacterial pathogen Species 0.000 claims 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims 1
- XKINMMDXLUQREP-UHFFFAOYSA-N [Cu].C(=C)N1C(CCC1)=O Chemical compound [Cu].C(=C)N1C(CCC1)=O XKINMMDXLUQREP-UHFFFAOYSA-N 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000000813 microbial effect Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
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- 238000001878 scanning electron micrograph Methods 0.000 description 3
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- 238000005054 agglomeration Methods 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8993—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with chromium, molybdenum or tungsten
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Abstract
The invention discloses a preparation method and application of a silver chromate/zinc ferrite fibrous composite photocatalyst, wherein the silver chromate/zinc ferrite fibrous composite photocatalyst takes zinc ferrite fibers prepared by electrostatic spinning and high-temperature calcination methods as a carrier, silver chromate particles are loaded on the surface of the zinc ferrite fibers by utilizing a coprecipitation method, and the silver chromate particles provide a larger specific surface area and more active sites for the zinc ferrite fibers; by constructing a silver chromate/zinc ferrite heterojunction structure, the recombination probability of photoproduction electrons and holes is reduced, the degradation efficiency of methylene blue and the killing efficiency of salmonella are improved, and the photocatalytic activity of the silver chromate/zinc ferrite composite fiber is promoted. Meanwhile, the reusability of the photocatalyst is improved by virtue of the advantage that the fibers are not easy to agglomerate. The preparation method is simple, the raw materials are cheap, and the preparation method has good practical prospect in the aspects of treating organic pollutants, harmful microorganisms and the like.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and particularly relates to a preparation method and application of a silver chromate/zinc ferrite fibrous composite photocatalyst.
Background
The photocatalysis technology utilizes solar light to excite photoinduced electrons of a semiconductor and dissolved oxygen to generate active oxidation groups, so as to achieve the effect of decomposing and removing pollutants. Because of its advantages of environmental friendliness, low cost, reusability, etc., it has attracted attention in recent years and is widely used in the fields of treating printing and dyeing wastewater, treating waste gas and sterilizing.
The traditional representativeness of photocatalysis isTiO2The TiO-based composite material attracts attention of scholars due to the advantages of environmental friendliness, stable chemical property, strong corrosion resistance and the like, but the TiO-based composite material is2The fatal short plate exists because of the wide forbidden band (about 3.2eV), only 3-5% of ultraviolet light contained in sunlight can be utilized, and the practical application of the fatal short plate is limited. In order to improve the utilization of sunlight, researchers have turned their eyes to semiconductor materials that respond to visible light. Wherein, Zn2FeO4The narrow band gap (about 1.9eV) can be excited by visible light, and has higher photocatalytic activity, which attracts more and more attention, however, although the narrow band gap improves the visible light response, the narrow band gap also causes easy recombination of photo-generated electrons and holes, so that the photo-generated electrons and holes need to be blocked by depositing noble metals, non-metal doping, semiconductor recombination and other modes, so as to improve the photocatalytic activity, but the narrow band gap is prepared in a powder form, so that the narrow band gap has the problems of large grain size and small specific surface area, and the photocatalytic effect is seriously influenced.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method and application of a silver chromate/zinc ferrite fibrous composite photocatalyst.
The technical scheme adopted by the invention is as follows:
a silver chromate/zinc ferrite fibrous composite photocatalyst is Zn prepared by electrostatic spinning and high-temperature calcination2FeO4Using fiber as carrier, and then using coprecipitation method to make Ag2CrO4The particles load the surface of the zinc ferrite fiber.
(1) Preparation of Zn by electrostatic spinning method and high-temperature calcination method2FeO4Fiber: mixing zinc acetate (Zn (AC)2) Iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and polyvinylpyrrolidone (PVP) are added into N, N-Dimethylformamide (DMF), the mixture is stirred for 8-12 h at normal temperature, the obtained precursor solution forms a fiber membrane through electrostatic spinning, and Zn is formed through calcination treatment2FeO4Fibers;
(2) preparation of Ag by coprecipitation method2CrO4/Zn2FeO4Fibrous compositesPhotocatalyst: zn prepared in the step (1)2FeO4The fibres being dispersed in silver nitrate (AgNO) dissolved in water3) Stirring the solution fully until the solution is mixed evenly, and dropwise adding potassium chromate (K) into the solution2CrO4) Continuously stirring the aqueous solution for 30-60 min, and performing suction filtration and drying to obtain Ag2CrO4/Zn2FeO4A fiber-shaped composite photocatalyst.
The precursor solution in the step (1) is Fe (NO)3)3·9H2O and Zn (AC)2The mass ratio of the components is 1: 1.8-2, and the mass fraction of the spinning precursor solution is 11-19%.
The electrostatic spinning parameters in the step (1) are as follows: the spinning distance is 9-13 cm, and the working voltage is 8-15 kv.
The calcination process parameters in the step (1) are as follows: the calcining temperature is 550-750 ℃, the time is 1.5-2.5 h, and the atmosphere is air.
K in the step (2)2CrO4With AgNO3The amount ratio of the substances (A) to (B) is 1:1.5 to 2.
Zn in the step (2)2FeO4The loading amount of the fiber is 20-60 wt%.
Ag2CrO4/Zn2FeO4Application of fibrous composite photocatalyst, and Ag2CrO4/Zn2FeO4The application of the fibrous composite photocatalyst in the aspect of treating wastewater and harmful microorganisms.
Ag2CrO4/Zn2FeO4Application of the fibrous composite photocatalyst, methylene blue is selected in the wastewater treatment test; the antibacterial activity test adopts salmonella.
Ag2CrO4/Zn2FeO4The fibrous composite photocatalyst is applied to water bodies,
degrading methylene blue aqueous solution and killing salmonella under simulated sunlight by using a 500W xenon lamp as a simulated sunlight light source; the concentration of the methylene blue aqueous solution is 5mg/L, and the concentration of the microorganism is 108CFU/mL, said lightThe content of the catalytic bactericide is 0.3mg/mL and 0.5mg/mL respectively.
The specific photocatalysis method comprises the following steps: adopting a 500W xenon lamp as a simulated light source, adding 100mL of methylene blue aqueous solution or 20mL of salmonella-containing microbial solution and 30mg or 10mg of fibrous composite photocatalyst into a container, placing the container on a stirrer which is 20cm away from a light source, stirring the suspension and the photocatalyst for 30min under a dark condition before photoreaction so as to achieve adsorption balance, taking 5mL samples every 20min after starting irradiation for the methylene blue aqueous solution, centrifuging, and testing the absorbance of the samples by using an ultraviolet-visible spectrophotometer; for the microbial solution containing Salmonella, 200. mu.L of the solution was taken three times every 15min after the start of irradiation, and the number of bacteria was measured by plate counting method to calculate the bactericidal rate.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts an electrostatic spinning method and a coprecipitation method to prepare the silver chromate/zinc ferrite fibrous composite photocatalyst, is applied to the aspect of treating organic pollutants and harmful microorganisms in wastewater, and adopts Zn prepared by electrostatic spinning2FeO4The specific surface area of the fiber is large, and simultaneously, the agglomeration phenomenon which is easy to occur in the traditional powder preparation is avoided,
(2) the silver chromate/zinc ferrite fibrous composite photocatalyst with the one-dimensional structure, which is prepared by the invention, has a large specific surface area and good visible light absorption performance.
(3) The silver chromate/zinc ferrite fibrous composite photocatalyst prepared by the invention has higher visible light catalytic performance and is excellent in the aspects of treating organic pollutants in wastewater and killing harmful microorganisms.
(4) The silver chromate/zinc ferrite fibrous composite photocatalyst prepared by the method has good reusability.
(5) The invention adopts the electrostatic spinning method and the coprecipitation method to prepare the silver chromate/zinc ferrite fibrous composite photocatalyst, and has the advantages of low cost and simple process and flow.
Drawings
FIG. 1 is an SEM image of a zinc ferrite fiber and a silver chromate/zinc ferrite fiber-shaped composite photocatalyst prepared by the method.
FIG. 2 is an XRD diagram of the silver chromate/zinc ferrite fiber-shaped composite photocatalyst prepared by the invention.
FIG. 3 is a graph showing the degradation of a methylene blue aqueous solution by the zinc ferrite fiber, silver chromate and the silver chromate/zinc ferrite fiber-shaped composite photocatalyst prepared by the present invention.
FIG. 4 is a graph showing the antibacterial efficiency of the zinc ferrite fiber, silver chromate and the silver chromate/zinc ferrite fiber-shaped composite photocatalyst prepared by the present invention against a Salmonella microbial solution.
Detailed Description
The invention aims to solve the problems in the prior art and provides a preparation method and application of a silver chromate/zinc ferrite fibrous composite photocatalyst.
The technical scheme adopted by the invention is as follows:
the silver chromate/zinc ferrite fibrous composite photocatalyst is prepared by an electrostatic spinning and coprecipitation method, zinc ferrite fibers are used as a carrier, silver chromate particles are loaded on the surfaces of the zinc ferrite fibers, and the silver chromate particles provide a larger specific surface area and more active sites for the zinc ferrite fibers; by constructing a silver chromate/zinc ferrite heterojunction structure, the recombination probability of photoproduction electrons and holes is reduced, the degradation efficiency of methylene blue and the killing efficiency of salmonella are improved, and the photocatalytic activity of the silver chromate/zinc ferrite composite fiber is promoted. Meanwhile, the reusability of the photocatalytic bactericide is improved by virtue of the advantage that the fibers are not easy to agglomerate. The preparation method is simple, the raw materials are cheap, and the preparation method has good practical prospect in the aspects of treating organic pollutants, harmful microorganisms and the like.
Example 1:
preparation of Zn by electrostatic spinning method and high-temperature calcination method2FeO4Fiber:
0.2mmol of Fe (NO)3)3·9H2O、0.4mmol Zn(AC)2And 3g of PVP is added into 20mL of DMF solution, and the mixture is stirred for 12h at normal temperature to obtain spinning precursor solution. The spinning parameters are as follows: the spinning distance was 13cm and the working voltage was 12.53 kV. The dried fiber membrane is calcined in a muffle furnace at 650 ℃ for 2.5hThen cooling to room temperature to obtain Zn2FeO4Fibers, noted ZFO.
Example 2:
preparation of Ag by coprecipitation method2CrO4Granules
Respectively adding 0.2mmol of AgNO3，0.1mmol K2CrO4Dissolving in 20mL deionized water, stirring for 15min, and adding K2CrO4The aqueous solution is added dropwise to AgNO3Stirring in water solution for 30min, washing, centrifuging and drying to obtain Ag2CrO4Monomer, noted ACO.
Example 3:
preparation of Ag by coprecipitation method2CrO4/Zn2FeO4The fibrous composite photocatalyst comprises:
weigh 0.1mmol of AgNO3Dissolving the mixture in 20mL of deionized water, stirring for 10min, and then adding the Zn prepared in example 12FeO4The fiber is dispersed in AgNO3The solution is fully stirred and 0.05mmol K is dropwise added2CrO4Stirring for 30min in 20mL of deionized water, filtering and drying to obtain Ag2CrO4/Zn2FeO4A composite photocatalyst in the form of a fiber, designated 20% -ACO/ZFO.
FIG. 1(a) shows Zn after calcination2FeO4SEM image of fiber with one-dimensional linear structure, uniform thickness and Zn on surface2FeO4The particles were isolated but loosely arranged, and the fiber diameter was about 55 nm. FIG. 1(b) shows Ag2CrO4/Zn2FeO4SEM image of composite fiber, Ag after coprecipitation reaction2CrO4Particles deposited on Zn2FeO4The fiber surface is irregular and the particles are densely distributed, and the fiber diameter is about 100 nm.
Comparative example 4:
Ag2CrO4/Zn2FeO4a preparation method of the fibrous composite photocatalyst;
preparation of Ag by coprecipitation method2CrO4/Zn2FeO4Fibrous composite lightCatalyst, weigh 0.2mmol AgNO3Dissolving the mixture in 20mL of deionized water, stirring for 10min, and then adding the Zn prepared in example 12FeO4The fiber is dispersed in AgNO3The solution is fully stirred and 0.1mmol K is dropwise added2CrO4Continuously stirring the deionized solution with 20mL for 30min, and performing suction filtration and drying to obtain Ag2CrO4/Zn2FeO4A composite photocatalyst in the form of a fiber, designated 40% -ACO/ZFO.
Comparative example 5:
Ag2CrO4/Zn2FeO4a preparation method of the fibrous composite photocatalyst;
preparation of Ag by coprecipitation method2CrO4/Zn2FeO4Weighing 0.3mmol AgNO of the fibrous composite photocatalyst3Dissolving the Zn powder in 20mL of deionized water, stirring for 10min, and adding the Zn powder prepared in example 12FeO4The fiber is dispersed in AgNO3The solution is fully stirred and 0.15mmol K is dropwise added2CrO4Continuously stirring the deionized solution with 20mL for 30min, and performing suction filtration and drying to obtain Ag2CrO4/Zn2FeO4A composite photocatalyst in the form of a fiber, designated 60% -ACO/ZFO.
FIG. 2 shows Ag in different loading amounts2CrO4/Zn2FeO4XRD pattern of the fibrous composite photocatalyst. As can be seen from FIG. 2, each curve in FIG. 2 corresponds to Ag prepared in example 3, comparative example 4, and comparative example 52CrO4/Zn2FeO4A fiber-shaped composite photocatalyst. It can be found from the graph that the sample diffraction angle is 29.7 degrees, 35.1 degrees, 42.5 degrees, 56.7 degrees and 62.1 degrees at 2 theta, and ZnFe is matched with standard card2O4[PDF#89-4926]Compared with ZnFe of isometric system2O4The characteristic diffraction peaks of the (220), (311), (400), (511) and (440) crystal planes of (A) and (B) are coincident. And at diffraction angles 2 θ of 31.40 °, 32.29 °, 33.71 °, 39.11 °, 45.38 °, 55.82 °, 57.02 °, 61.98 ° with Ag2CrO4Standard card [ PDF #26-0952]In contrast, it is respectively compared with orthorhombic Ag2CrO4The peaks of (120), (031), (131), (022), (122), (242), (231) and (431) characteristic of the crystal plane of (A) coincide. The XRD pattern of the ACO/ZFO fibrous composite photocatalyst has no other impurity peaks, which indicates that the composite catalyst has better purity.
Application example 1:
ag obtained as described above2CrO4/Zn2FeO4The application of the fibrous composite photocatalyst in treating organic pollutants and harmful microorganisms in wastewater degrades Methylene Blue (MB) aqueous solution.
A 500W xenon lamp is used as a simulated light source, and 30mg Ag is used2CrO4/Zn2FeO4Adding the fibrous composite photocatalyst into a container containing 100mL of MB solution, placing the container on a stirrer 20cm away from a light source, stirring the suspension and the photocatalyst for 30min in a dark condition before photoreaction to ensure that the photocatalyst and the solution to be reacted reach adsorption balance, taking 5mL samples every 20min after starting irradiation of the MB solution, centrifuging, and testing the absorbance of the MB solution by using an ultraviolet visible spectrophotometer.
FIG. 3 is Ag2CrO4/Zn2FeO4Graph of MB degradation in methylene blue aqueous solution. As can be seen from FIG. 3, the degradation effect of the composite photocatalyst is better than that of ZFO and the monomer of ACO along with the prolonging of time, and in both of the ZFO and the ACO, ZFO monomer has poor degradation effect on MB, and the degradation rate of 40% ACO/ZFO is as high as 91.7%.
Application example 2: ag obtained as described above2CrO4/Zn2FeO4The application of the fibrous composite photocatalyst in treating organic pollutants and harmful microorganisms in wastewater is used for killing the harmful microorganisms salmonella.
Firstly, preparing bacterial suspension, inoculating salmonella into a sterilized NB medium, then culturing for 12h in a constant temperature shaking table at 37 ℃, and then diluting by 10 times and 10 times step by step through sterilized 0.85% NaCl solution 210 times of310 times of410 times of510 times of6Multiple and 107Taking 100 mul of the suspension to be coated on a solid culture medium respectively, putting the suspension into a constant temperature incubator at 37 ℃ for 12 hours,the number of colonies was observed and recorded, the number of colonies in the selection medium was a multiple of about 300, and according to the results we chose 105And (4) doubling.
The specific photocatalytic antibacterial experiment process is as follows: bacterial suspension was diluted to 104After doubling, 1mL of the bacterial solution was aspirated and added to 18mL of 0.85% NaCl solution, followed by 10mg of Ag2CrO4/Zn2FeO4And starting stirring the fibrous composite photocatalyst in a dark place to uniformly mix the fibrous composite photocatalyst, sucking the solution in the dark place into a 0min sample, taking 200 mu L of the solution for 3 times at intervals of 15min after starting irradiation, sucking 100 mu L of the solution respectively after the reaction is finished, coating the solution on a solid culture medium, putting the solid culture medium into a constant-temperature incubator at 37 ℃ for culturing for 12h, observing and recording the number of bacterial colonies, and calculating the sterilization rate.
FIG. 4 shows Ag2CrO4/Zn2FeO4A graph of the fiber-shaped composite photocatalyst for killing salmonella. As can be seen from figure 4, the sterilizing effect of the composite photocatalyst is better than that of the ZFO monomer and the ACO monomer along with the prolonging of the time, in the both, the ZFO monomer has poor degradation effect on the salmonella, and the killing rate of 40% ACO/ZFO is as high as 98.7% within 60 min.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the silver chromate/zinc ferrite fibrous composite photocatalyst is characterized in that the fibrous composite photocatalyst is zinc ferrite (Zn) prepared by electrostatic spinning and high-temperature calcination2FeO4) The fiber is used as a carrier, and silver chromate (Ag) is added by a coprecipitation method2CrO4) The particle-loaded zinc ferrite fiber surface is prepared by the following specific preparation method:
(1) preparation of Zn by electrostatic spinning method and high-temperature calcination method2FeO4Fiber: mixing zinc acetate (Zn (AC)2) Iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and polyethyleneAdding copper vinylpyrrolidone (PVP) into N, N-Dimethylformamide (DMF), stirring at normal temperature for 8-12 h, forming a fiber membrane from the obtained precursor solution through electrostatic spinning, and calcining to obtain Zn2FeO4Fibers; fe (NO)3)3·9H2O and Zn (AC)2The mass ratio of the spinning precursor solution is 1: 1.8-2, and the mass fraction of the spinning precursor solution is 11-19%; the electrostatic spinning parameters are as follows: the spinning distance is 9-13 cm, and the working voltage is 8-15 kv; the calcination temperature is 550-750 ℃, the heat preservation time is 1.5-2.5 h, and the atmosphere is air;
(2) preparation of Ag by coprecipitation method2CrO4/Zn2FeO4The fibrous composite photocatalyst comprises: zn prepared in the step (1)2FeO4The fibres being dispersed in silver nitrate (AgNO) dissolved in water3) Stirring the solution fully until the solution is mixed evenly, and dropwise adding potassium chromate (K) into the solution2CrO4) Continuously stirring the aqueous solution for 30-60 min, and performing suction filtration and drying to obtain Ag2CrO4/Zn2FeO4A fibrous composite photocatalyst; AgNO3And K2CrO4The amount ratio of the substances (A) to (B) is 1.5 to 2: 1; zn2FeO4The loading amount of the fiber is 20-60 wt%.
2. The method for preparing the silver chromate/zinc ferrite fiber-shaped composite photocatalyst according to claim 1, wherein Zn is calcined in the step (1)2FeO4The fiber is in a one-dimensional linear structure and has Zn on the surface2FeO4The particles are separated out, and the diameter of the fiber is about 55 nm.
3. The method for preparing the silver chromate/zinc ferrite fiber-shaped composite photocatalyst according to claim 1, wherein Ag is used in the step (2)2CrO4/Zn2FeO4In the fibrous composite photocatalyst, Ag2CrO4Particles deposited on Zn2FeO4The fiber surface is irregular and the fiber diameter is about 100 nm.
4. AUse of a silver chromate/zinc ferrite fibrous composite photocatalyst prepared by the method of any one of claims 1 to 3, characterized in that Ag is used2CrO4/Zn2FeO4The fibrous composite photocatalyst is applied to killing of food-borne pathogenic bacteria and removal of organic dyes in dye wastewater.
5. The use as claimed in claim 4, wherein the killed food-borne pathogenic bacteria are Salmonella, but not limited thereto; the organic dye in the wastewater is removed, but is not limited to, methylene blue.
6. Use according to claim 5, characterized in that the method for degrading the Methylene Blue (MB) aqueous solution is: a 500W xenon lamp is used as a simulated light source, and 30mg Ag is used2CrO4/Zn2FeO4Adding the fibrous composite photocatalyst into a container containing 100mL of MB solution, placing the container on a stirrer 20cm away from a light source, stirring the suspension and the photocatalyst for 30min in a dark condition before photoreaction to ensure that the photocatalyst and the solution to be reacted reach adsorption balance, taking 5mL samples every 20min after starting irradiation of the MB solution, centrifuging, and testing the absorbance of the MB solution by using an ultraviolet visible spectrophotometer.
7. The use as claimed in claim 5, wherein the method of killing the harmful microorganism Salmonella is: inoculating Salmonella to sterilized NB medium, culturing in 37 deg.C constant temperature shaking table for 12 hr, and gradually diluting with sterilized 0.85% NaCl solution by 10 times and 10 times210 times of310 times of410 times of510 times of6Multiple and 107Doubling, namely respectively sucking 100 mu L of the suspension solution and coating the suspension solution on a solid culture medium, putting the suspension solution into a constant-temperature incubator at 37 ℃ for culturing for 12 hours, observing and recording the number of colonies, and selecting the number of the colonies in the culture medium to be about 300 times;
bacterial suspension was diluted to 104After doubling, 1mL of the suspension was aspirated and added to 18mL of 0.85% NaCl solution, followed by 10mg of the suspensionAg2CrO4/Zn2FeO4And starting stirring the fibrous composite photocatalyst in a dark place to uniformly mix the fibrous composite photocatalyst, sucking the solution in the dark place into a 0min sample, taking 200 mu L of the solution for 3 times at intervals of 15min after starting irradiation, sucking 100 mu L of the solution respectively after the reaction is finished, coating the solution on a solid culture medium, putting the solid culture medium into a constant-temperature incubator at 37 ℃ for culturing for 12h, observing and recording the number of bacterial colonies, and calculating the sterilization rate.
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