CN114939404A - Be used for degrading aflatoxin B 1 And a method for preparing the same - Google Patents
Be used for degrading aflatoxin B 1 And a method for preparing the same Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000000593 degrading effect Effects 0.000 title abstract description 13
- OQIQSTLJSLGHID-WNWIJWBNSA-N aflatoxin B1 Chemical compound C=1([C@@H]2C=CO[C@@H]2OC=1C=C(C1=2)OC)C=2OC(=O)C2=C1CCC2=O OQIQSTLJSLGHID-WNWIJWBNSA-N 0.000 title abstract description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 28
- 239000011258 core-shell material Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- -1 PVP modified ZIF-8 Chemical class 0.000 claims abstract 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 34
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical class [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 10
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- 238000000197 pyrolysis Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 17
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 17
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 7
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 229930195730 Aflatoxin Natural products 0.000 description 5
- 239000005409 aflatoxin Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 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
- XWIYFDMXXLINPU-UHFFFAOYSA-N Aflatoxin G Chemical compound O=C1OCCC2=C1C(=O)OC1=C2C(OC)=CC2=C1C1C=COC1O2 XWIYFDMXXLINPU-UHFFFAOYSA-N 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
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- 238000002474 experimental method Methods 0.000 description 3
- 239000002636 mycotoxin Substances 0.000 description 3
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- 239000011701 zinc Substances 0.000 description 3
- RULKYXXCCZZKDZ-UHFFFAOYSA-N 2,3,4,5-tetrachlorophenol Chemical compound OC1=CC(Cl)=C(Cl)C(Cl)=C1Cl RULKYXXCCZZKDZ-UHFFFAOYSA-N 0.000 description 2
- 101100449517 Arabidopsis thaliana GRH1 gene Proteins 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 101100434479 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) AFB1 gene Proteins 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229930020125 aflatoxin-B1 Natural products 0.000 description 2
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- 239000004065 semiconductor Substances 0.000 description 2
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 2
- UIVOFKCQIFEAFX-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl.OC1=CC=CC=C1Cl UIVOFKCQIFEAFX-UHFFFAOYSA-N 0.000 description 1
- 241000228197 Aspergillus flavus Species 0.000 description 1
- 241000228230 Aspergillus parasiticus Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
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- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 238000001784 detoxification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/398—Egg yolk like
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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Abstract
The invention provides a method for degrading aflatoxin B 1 The PVP modified ZIF-8 is used as a precursor to synthesize the ZnO @ NPC photocatalyst with a core-shell structure, the PVP modified ZIF-8 is completely converted into polyhedral ZnO after pyrolysis treatment, the surface of the polyhedral ZnO is converted into N-doped porous carbon through in-situ conversion and pyrolysis processes, and the aflatoxin B is treated 1 The degradation rate is greatly improved, and higher repeated cycle degradation stability is shown.
Description
Technical Field
The application relates to the field of photocatalysts, in particular to a photocatalyst for degrading aflatoxin B 1 The photocatalyst and the preparation method thereof.
Background
Food safety issues are a continuing concern for humans. Foodstuffs such as grains, edible oils and meats are easily polluted by the environment during the period of planting, storing or raising. In addition, some pathogenic microorganisms can also grow and form mycotoxins in these foods. These mycotoxins pose significant economic losses and health risks. Aflatoxins, one of the mycotoxins, are secondary metabolites of aspergillus flavus and aspergillus parasiticus, and they are highly toxic, destructive and carcinogenic to humans. Especially yellow rice cakeMycotoxin B 1 （AFB 1 ) They can cause cancer and damage internal organs of the human body. Today, AFB 1 Degradation detoxification of the protein still presents a great challenge for the food industry. Researchers have proposed various techniques for aflatoxin degradation, including physical, chemical and biological methods. These techniques can eliminate AFB to some extent 1 But still have certain limitations. For example, physical adsorption methods are used although AFB can be adsorbed 1 But not the decomposition of AFB 1 And may cause secondary pollution. Whereas chemical methods, such as photocatalytic degradation, may affect food quality under UV irradiation, biological methods take a long time to degrade AFB 1 A molecule. In addition, as the demand for health foods increases, food safety standards also increase. Therefore, there is a need to find a more environmentally friendly, efficient and safe method for degrading AFB 1 。
The photocatalytic degradation is an advanced oxidative degradation technology, and the method has the advantages of low cost, sustainability, no secondary pollution and simple and convenient operation. Above all, under the irradiation of ultraviolet light or visible light, the organic pollutants in wastewater and gas environment can be completely degraded into H 2 O、CO 2 Or other harmless substances. It is generally considered to be the most efficient and environmentally friendly method of removing and degrading contaminants from the environment. To date, there have been many reports of the use of semiconductors to degrade organic contaminants. For example, researchers have utilized aged amorphous peroxytungstic acid to produce WO having high activity 3 Semiconductor and its application as photocatalyst for degrading various organic compounds into CO under the condition of xenon lamp illumination simulating sunlight 2 . High activity WO 3 The photocatalytic activity of the photocatalyst is superior to that of commercial or domestic nitrogen-doped TiO 2 And WO 3 A catalyst. Other researchers have treated NH by heat 3 And the SCN adopts silicon dioxide nano particles as a mother board to synthesize the mesoporous graphite carbonitride. It was found that mesoporous graphitic carbonitrides exhibit excellent photocatalytic activity in degrading chlorophenol (chlorophenol) and phenol (phenol) in the liquid phase. Zinc oxide is of great interest because of its high efficiency, safety and ease of preparation. Many studiesVarious methods of preparing zinc oxide have been reported and used to degrade different contaminants. There are researchers who have synthesized dumbbell-shaped ZnO photocatalysts using microwave heating technology and used them to degrade Methylene Blue (MB). They found that the decolorization and TOC removal rates reached 99.6% and 74.3%, respectively. Synthesizing Fe-doped by adopting sol-gel method 3+ The ZnO photocatalyst is researched on the photocatalytic performance of the ZnO photocatalyst for degrading methylene blue under ultraviolet light and degrading 4-CP (tetrachlorophenol) under visible light. The results show that Fe 0.8 The photocatalytic activity of ZnO is the highest, and the degradation rates of MB and 4-CP (tetrachlorophenol) are respectively as high as 93 percent and 73 percent. However, the photocatalytic performance of ZnO is still limited by its photo-induced electron and hole separation efficiency and absorption capacity, and the photocatalytic activity of zinc oxide is still to be improved.
Disclosure of Invention
On one hand, the invention provides a preparation method of a photocatalyst for degrading aflatoxin, which adopts polyvinylpyrrolidone (PVP) modified ZIF-8 as a precursor, and prepares the photocatalyst of N-doped porous carbon-coated ZnO (ZnO @ NPC for short) by a pyrolysis-in-situ conversion-pyrolysis method. The preparation method comprises the following steps:
c is to be 4 H 6 N 2 And PVP is completely dissolved in the methanol solution to form A solution, Zn (NO) is added 3 ) 2 ·6H 2 Completely dissolving O in a methanol solution to form a solution B, pouring the solution B into the solution A, stirring to fully mix the solution B and the solution A to obtain a mixed solution, aging the mixed solution, centrifuging a precipitate at the bottom of the mixed solution, washing the precipitate with ethanol, and drying to obtain PVP modified ZIF-8; subsequently, sintering the PVP modified ZIF-8 to obtain a ZnO polyhedral structure, and dispersing the ZnO polyhedral structure to the solution of C 4 H 6 N 2 Aging and centrifuging in a PVP methanol solution, washing with ethanol, and drying to obtain a ZnO @ ZIF-8 core-shell polyhedral structure; and finally, sintering the obtained ZnO @ ZIF-8 core-shell polyhedral structure to obtain the ZnO @ ZIF-8 core-shell polyhedral structure.
In another aspect, the present invention provides a photocatalyst prepared by the above preparation method.
After the experimentExperiments prove that the photocatalyst prepared by the preparation method of the invention is used for aflatoxin B 1 The excellent degradation performance is embodied. In addition, the photocatalyst has good repairability and reusability.
Drawings
FIG. 1 is a schematic diagram of the preparation of a ZnO @ NPC core-shell photocatalyst according to the present invention.
FIG. 2 (a) ZnO @ NPC, ZnO @ ZIF-8, ZnO and ZIF-8 and blank group vs. AFB 1 Comparing the photocatalytic degradation rates of the two;
(b) photocatalytic degradation of AFB (atomic fluorescence Spectroscopy) by using ZnO @ NPC (N-propyl-N-phosphate) under ultraviolet light 1 Five repetitive cycle degradation maps of;
(c) x-ray diffraction patterns of ZnO @ NPC before and after the reaction.
Detailed Description
Embodiments for carrying out the present invention will be described in detail with reference to the accompanying drawings. The present invention is not limited to the contents described in the following examples. The components described below include substantially the same components as can be easily conceived by those skilled in the art. Further, the following structures can be combined as appropriate. Various omissions, substitutions, and changes in the structure can be made without departing from the spirit of the invention.
(detailed example 1)
The preparation method of the photocatalyst for degrading aflatoxin in example 1 of the present invention and the photocatalyst prepared thereby are illustrated in the accompanying drawings, and as shown in fig. 1, the preparation method adopts polyvinylpyrrolidone (PVP) modified ZIF-8 as a precursor, and prepares the photocatalyst of N-doped porous carbon-coated ZnO (ZnO @ NPC for short) by a "pyrolysis-in-situ conversion-pyrolysis" method. The preparation method comprises the following steps:
c is to be 4 H 6 N 2 And PVP is completely dissolved in the methanol solution to form A solution, Zn (NO) is added 3 ) 2 ·6H 2 Dissolving O in methanol solution completely to obtain solution B, adding solution B into solution A, stirring to obtain mixed solution, aging, centrifuging to obtain precipitate at the bottom, and adding ethanolWashing and drying to obtain PVP modified ZIF-8; subsequently, sintering the PVP modified ZIF-8 to obtain a ZnO polyhedral structure, and dispersing the ZnO polyhedral structure to the solution of C 4 H 6 N 2 And PVP methanol solution, aging, centrifuging, washing with ethanol, and drying to obtain a ZnO @ ZIF-8 core-shell polyhedral structure; and finally, sintering the obtained ZnO @ ZIF-8 core-shell polyhedral structure to obtain the photocatalyst for degrading aflatoxin.
(detailed example 2)
Referring to the figure 1, the ZnO @ NPC photocatalyst with the core-shell structure is synthesized by taking PVP modified ZIF-8 as a precursor, and the preparation method comprises the following steps: first, 3.8g of C was mixed 4 H 6 N 2 And 10g of PVP were completely dissolved in 100mL of methanol to obtain solution A, and 4.5g of Zn (NO) was added 3 ) 2 ·6H 2 O was completely dissolved in 100mL of methanol solution to form a B solution. And quickly adding the solution B into the solution A, and stirring for 5min to fully mix. The mixed solution is aged for 15 hours at 60 ℃, then the sediment at the bottom of the mixed solution is centrifuged, washed three times by ethanol and dried for 10 hours at 80 ℃, thus obtaining PVP modified ZIF-8. And then, putting the ZIF-8 modified by PVP into a muffle furnace, heating to 550 ℃ at the heating rate of 2 ℃/min in the air atmosphere, and sintering for 30min to obtain the ZnO polyhedral structure. Next, 0.5g of a ZnO polyhedron structure was dispersed in 30mL of a dispersion containing 9.1g of C dissolved therein 4 H 6 N 2 And 3g of PVP in a methanol solution, then aging for 12h at room temperature, centrifuging, washing with ethanol for three times, and drying for 8h at 80 ℃ to obtain the ZnO @ ZIF-8 core-shell polyhedral structure. And finally, heating the obtained ZnO @ ZIF-8 core-shell polyhedral structure to 800 ℃ at the heating rate of 2 ℃/min in Ar atmosphere, and sintering for 90min to obtain the N-doped porous carbon-coated ZnO polyhedral structure (ZnO @ NPC).
To verify the degradation performance of the photocatalyst obtained by the above preparation method, 0.05 g of the photocatalyst was dispersed in 100mL of AFB having a concentration of 5ppm 1 Solution, suspension formation, dark reaction for 30min to reach adsorption-desorption equilibrium. Then, the ultraviolet light is turned on to carry out a photocatalytic degradation experiment. After dark reaction for 30min, ZnO can absorb 6.5% of AFB 1 . However, the method is not limited to the specific methodZnO @ NPC absorbs 64.1% of AFB1, while ZnO @ ZIF-8 and ZIF-8 absorb 24.6% and 54.1% of AFB1, respectively. As shown in FIG. 2a, ZnO @ NPC was applied to AFB 48min after UV irradiation 1 The degradation rate of the zinc oxide is 94.8 percent, and ZnO, ZnO @ ZIF-8 and ZIF-8 are opposite to AFB 1 The degradation rates of the two are respectively 80.4%, 32.3% and 59.9%. AFB 1 The molecular size is larger than the pore size of ZIF-8. AFB 1 Molecules can not enter ZnO to carry out photocatalytic degradation reaction through the ZIF-8 shell. Thus ZnO @ ZIF-8 and ZIF-8 are directed to AFB 1 The photocatalytic degradation activity of (A) is low.
Five-time cyclic degradation experiments were performed using ZnO @ NPC as the catalyst to further demonstrate the stability of the photocatalyst. As shown in FIG. 2b, the degradation rate of ZnO @ NPC is only reduced by 1.71% after five repeated cycle experiments, and the ZnO @ NPC can be proved to have good repairability and reusability. By XRD pattern analysis before and after reaction of ZnO @ NPC, referring to FIG. 2c, XRD diffraction peaks after reaction of ZnO @ NPC are almost the same as those before reaction. This means that the phase structure of the ZnO @ NPC remains unchanged after five repeated cycles. The slight decrease in catalytic activity may be due to a small loss occurring when the catalyst is recovered.
The present invention is not limited to the above embodiments. That is, various modifications can be made without departing from the scope of the present invention.
Claims (4)
1. A method for preparing a photocatalyst is characterized in that C is added 4 H 6 N 2 And PVP is completely dissolved in the methanol solution to form A solution, Zn (NO) is added 3 ) 2 ·6H 2 Completely dissolving O in a methanol solution to form a solution B, adding the solution B into the solution A, stirring to fully mix the solution B and the solution A to obtain a mixed solution, aging the mixed solution, centrifuging a precipitate at the bottom of the mixed solution, washing the precipitate with ethanol, and drying to obtain PVP modified ZIF-8; subsequently, carrying out primary sintering on PVP modified ZIF-8 to obtain a ZnO polyhedral structure, and dispersing the ZnO polyhedral structure to dissolve C 4 H 6 N 2 Aging and centrifuging in PVP methanol solution, washing with ethanol, and drying to obtain ZnO @ ZIF-8 core-shell polyhedral structure(ii) a And finally, sintering the obtained ZnO @ ZIF-8 core-shell polyhedral structure for the second time to obtain the ZnO @ ZIF-8 core-shell polyhedral structure.
2. The method for preparing the photocatalyst according to claim 1, wherein in the first sintering, the PVP-modified ZIF-8 is placed in a muffle furnace, and heated to 550 ℃ at a heating rate of 2 ℃/min in an air atmosphere, and sintered for 30min to obtain a ZnO polyhedron structure.
3. The preparation method of the photocatalyst according to claim 1 or 2, further characterized in that, during the second sintering, the ZnO @ ZIF-8 core-shell polyhedral structure is heated to 800 ℃ at a heating rate of 2 ℃/min in an Ar atmosphere and sintered for 90min to prepare the N-doped porous carbon-coated ZnO polyhedral structure.
4. A photocatalyst produced by the production method according to any one of claims 1 to 3.
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