CN113559903A - Sandwich-shaped Co3O4@ Mxenes composite material and preparation method and application thereof - Google Patents

Sandwich-shaped Co3O4@ Mxenes composite material and preparation method and application thereof Download PDF

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CN113559903A
CN113559903A CN202110701911.7A CN202110701911A CN113559903A CN 113559903 A CN113559903 A CN 113559903A CN 202110701911 A CN202110701911 A CN 202110701911A CN 113559903 A CN113559903 A CN 113559903A
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composite material
sandwich
mxenes
dichlorophenol
shaped
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周雪飞
陈家斌
张亚雷
张龙龙
郑婷露
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Tongji University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/722Oxidation by peroxides
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen

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  • Hydrology & Water Resources (AREA)
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Abstract

The invention relates to a sandwich-shaped Co3O4@ Mxenes composite material, preparation method thereof and application method for removing 2, 4-dichlorophenol in water by adopting @ Mxenes composite material to activate peroxyacetic acid3AlC2Immersing in HF, sealing in a polytetrafluoroethylene cup, and heating to obtain Ti3C2TXThen with Co (NO)3)2·6H2Obtaining sandwich-shaped Co after O mixing reaction3O4@ Mxenes composites. The sandwich Co provided by the invention3O4The @ Mxenes composite material activates peracetic acid to generate organic free radical, oxidizes and degrades 2, 4-dichlorophenol in water body, compared with other materialsActivation method ═ Co3O4The @ Mxenes composite material can efficiently activate peroxyacetic acid with a unique sandwich structure, has low leaching rate of metal cobalt ions, solves the problem of secondary pollution to the environment caused by leaching of the metal ions, and is an environment-friendly catalyst.

Description

Sanming liquorShape-controlling Co3O4@ Mxenes composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of water pollution control, in particular to a sandwich-shaped Co3O4@ Mxenes composite material, a preparation method thereof and an application method for removing 2, 4-dichlorophenol in water by using activated peroxyacetic acid.
Background
2, 4-dichlorophenol (2,4-DCP) is generated from chlorophenol pollutants in a priority pollutant list of China in a plurality of industries such as coking, printing and dyeing, plastics, oil refining and the like, has strong toxicity and odor, can cause anemia, syncope, acne and pruritus, and even can cause cancer. Although the concentration of the natural water is low, the potential threat to human health and ecological environment caused by the natural water is not ignored, and the natural water becomes a pollutant concerned by people. 2, 4-dichlorophenol (2,4-DCP) is a common chlorophenol pollutant, has poor biodegradability, is difficult to degrade by the traditional process, and has high treatment difficulty. Therefore, there is a need to develop an environmentally friendly, efficient and economical treatment method.
In recent years, advanced oxidation technology is considered as one of the most promising technologies for degrading different kinds of organic compounds, microorganisms and emerging pollutants, which oxidize organic pollutants by radicals generated by an oxidizing agent. Peroxyacetic acid is a strong oxidant with a very high standard reduction potential (E)01.96V), close to H2O2Higher than chlorine or chlorine dioxide. The thermal stability of the polymer is mainly determined by the dissociation energy of O-O bonds, and the ratio of O-O bonds (159kJ/mol) to H of the peroxyacetic acid2O2(213kJ/mol) weak, the peracetic acid solution can decompose naturally at room temperature. Compared with other oxidation technologies, peroxyacetic acid based advanced oxidation technologies have the advantages of strong oxidation capacity, low pH dependence, less generation of toxic byproducts in treated wastewater and the like, so that the peroxyacetic acid has more and more attention on the aspects of inactivating pathogens in wastewater and removing newly-appeared difficultly-degradable pollutants. Peroxyacetic acid is required to generate active free radicals to degrade pollutants through an activation process, and the activation of the peroxyacetic acid is reportedMethods including UV irradiation and addition of transition metal ions indicate that these activation methods have great potential for contaminant treatment. However, ultraviolet irradiation has limited permeability to water and cannot be applied to treatment of groundwater. Compared with other metals, the transition metals (Co, Fe, Cu and Mn) have the advantages of low cost and reusability. Wherein Co2+the/PMS system shows the best performance at neutral pH and lower reagent dosage, even better than the traditional Fenton reaction. However, leaching of metallic cobalt may lead to metal contamination and ecotoxicity. Therefore, relatively high stability of Co-based3O4Have been widely studied.
MXenes are two-dimensional materials composed of transition metal carbides, carbonitrides or nitrides. Such two-dimensional materials have Mn+1XnGeneral formula (II) is shown. In the formula, the letter M represents a transition metal (Ti, Mo, V, Ta, Nb, Cr, etc.), and the letter X represents C or N. MXenes have many functional groups on their surface. In this regard, the general formula for MXenes can be generalized to Mn+1XnTxWherein T represents a surface termination (e.g., -O, -F, or-OH). As more and more two-dimensional materials are discovered, the discovery of MXenes has gained wide acceptance and has milestone significance. The structure and excellent performance of MXenes make it widely used in the fields of batteries, capacitors, catalysis, electromagnetic shielding, absorption, etc. Ti3C2TxIs the first MXenes, and is also the most commonly used type of MXenes. It is obtained by selective etching of Ti3AlC2Phase metal aluminum layer. The unique layered structure of MXenes provides a larger space for the immobilization of the functional nano-materials, improves the distribution of the functional nano-materials on the surface of MXenes, and provides a possible application prospect for the MXenes as a potential support material for environmental remediation (such as catalysis and adsorption). However, little is known about its possible use in water purification. It is reported that Fe3O4the/MXenes composite material has excellent removal performance on phosphate in wastewater. In a word, MXenes has rich active centers and high specific surface area in the aspect of pollutant removal, has wide application prospect and belongs to the field of environmental remediation of advanced oxidation technologyThe popularization and the application of the method provide opportunities.
Here we use for the first time sandwich Co3O4The @ Mxenes compound is used as a heterogeneous catalyst to activate peracetic acid to remove 2, 4-dichlorophenol in water. In this system the acetylperoxy radical CH3C (═ O) OO · proved to be the main active component of the reaction, Mxenes material accelerated Co3O4Surface ≡ Co2+-≡Co3+-≡Co2+(see equations 1 and 2), thereby significantly strengthening Co3O4Activating effect on peroxyacetic acid. The leaching condition of the cobalt ions in the system is further researched, and the leaching amount of the cobalt ions after reaction is only about 0.02mg/L and is far lower than the standard cobalt ion concentration limit value (1.0mg/L) of the surface water environment quality in China.
≡Co(II)+CH3CO3H→≡Co(III)+CH3CO2 ·+OH- (1)
≡Co(III)+CH3CO3H→≡Co(II)+CH3CO3 ·+H+ (2)
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a sandwich-shaped Co3O4@ Mxenes composite material, a preparation method thereof and an application method for removing 2, 4-dichlorophenol in water by using activated peroxyacetic acid. The invention mainly overcomes the technical problems that: the catalytic activity of the catalyst is not high, the stability of the catalyst is poor, and the leaching of metal ions influences the ecological environment and causes secondary pollution.
The technical scheme of the invention is as follows: sandwich-shaped Co3O4The preparation method of the @ Mxenes composite material comprises the following steps:
(1) mixing 3g of Ti3AlC2Immersing in 35mL of HF, sealing in a polytetrafluoroethylene cup, reacting at 313K, washing the obtained material with deionized water, centrifuging for 3-5 times to remove residual impurities, and drying in a vacuum oven at 333K overnight until constant weight is achieved to obtain Ti3C2TXWherein T represents surface terminationA terminal end, the surface termination comprising-O, -F, or-OH;
(2) ti obtained in the step (1)3C2TXAnd 0.35g to 1.05g of Co (NO)3)2·6H2Mixing O into deionized water, and violently stirring the mixture to evaporate water at the rotating speed of 400-500 rpm;
(3) grinding the obtained product into powder, heating to 473K at room temperature, and reacting for 12 h; cooling to room temperature, washing with deionized water for three times to remove residual impurities to obtain sandwich-shaped Co3O4@ Mxenes composites.
Further, Co (NO) in the step (2)3)2·6H2The amount of O added was 0.7 g.
Further, Co attached in the composite material3O4The grain diameter is 25 nm-50 nm.
The invention also provides the sandwich Co3O4The application method of the @ Mxenes composite material for activating peracetic acid to remove 2, 4-dichlorophenol in water comprises the following steps: adding peroxyacetic acid and the sandwich Co as catalyst into the sewage containing 2, 4-dichlorophenol as organic pollutant3O4@ Mxenes composites; adding peroxyacetic acid and the sandwich Co3O4In a mixed solution of @ Mxenes composite material, the sandwich-shaped Co3O4The concentration of the @ Mxenes composite material is 5 mg/L-50 mg/L, the concentration of the peroxyacetic acid is 0.05 mM-1.04 mM, and after the reaction is carried out for 2 min-20 min at normal temperature, the pollutant 2, 4-dichlorophenol in the sewage is removed.
Further, the concentration of the oxidant peracetic acid in the catalytic system was 0.26 mM.
Further, the concentration of the catalyst in the catalyst system is 10 mg/L.
Further, the concentration of the target contaminant 2, 4-dichlorophenol was 20. mu.M.
Further, the reaction was carried out at an initial pH of 7.0.
Further, the reaction time was 20 min.
Further, the sandwich-shaped Co3O4The @ Mxenes composite material is repeatedly recycled for 4 times, and the pollutant removal rate can still reach over 90 percent; the catalyst is recovered by filtration and then dried, and can be reused without additional activation.
The invention has the following beneficial technical effects:
mixing the obtained sandwich-shaped Co3O4The @ Mxenes composite material is in a sandwich shape, and Co3O4Nanoparticles are adhered to the surface and interlayer of MXene, Mxene and Co3O4Stable bonding between nanoparticles, Co3O4The particles can be uniformly dispersed, and thus the catalytic activity is high. Co3O4@ Mxenes can effectively activate peroxyacetic acid over a wide pH range, covering most wastewater pH ranges. Sandwich-shaped Co prepared by adopting preparation method of application3O4The @ Mxenes composite material is used as a heterogeneous catalyst, and has good stability and reusability due to the unique morphology structure. Researches show that the sandwich-shaped Co prepared by the preparation method of the application3O4When the @ Mxenes composite material is used as a heterogeneous catalyst to activate peroxyacetic acid to remove 2, 4-dichlorophenol in water, the leaching rate of metal cobalt ions is very low, the problem of secondary pollution to the environment caused by leaching of the metal ions is solved, and the catalyst is an environment-friendly catalyst. The invention uses self-prepared sandwich-shaped Co for the first time3O4The method for activating peroxyacetic acid by the @ Mxenes composite material has a good effect of removing 2, 4-dichlorophenol in water, and after the reaction is carried out for 20min, the removal rate of the 2, 4-dichlorophenol reaches about 98%, so that the research of the activated peroxyacetic acid in the field of sewage treatment is promoted.
Drawings
FIG. 1 shows a sandwich-shaped Co prepared by the preparation method of the present invention3O4Electron microscopy of @ mxexens composites;
FIG. 2 is a schematic representation of the effect of initial pH on the degradation of 2, 4-dichlorophenol in application example 1 of the present invention;
FIG. 3 shows an embodiment of the present invention2 different sandwich Co3O4The schematic diagram of the influence of the added amount of the @ Mxenes composite material on the degradation of 2, 4-dichlorophenol after the peroxyacetic acid is activated;
FIG. 4 shows an application example 3 of the present invention using a sandwich Co3O4Schematic representation of the effect of different concentrations of peroxyacetic acid activated by @ mxexes composite on the degradation of 2, 4-dichlorophenol.
Detailed Description
The present invention will next be described in detail with reference to examples. However, the examples listed below do not limit the scope of the present invention.
Example 1
(1) Mixing 3g of Ti3AlC2Immersing in 35mL of HF, sealing in a polytetrafluoroethylene cup, reacting at 313K, washing the obtained material with deionized water, centrifuging for 3-5 times to remove residual impurities, and drying in a vacuum oven at 333K overnight until constant weight is achieved to obtain Ti3C2TXAnd T represents a surface termination (e.g., -O, -F, or-OH).
(2) Mixing Ti3C2TXAnd 0.35g of Co (NO)3)2·6H2And O is mixed into deionized water, and the mixture is stirred vigorously to evaporate water, wherein the rotating speed is 400-500 rpm.
(3) Grinding the obtained product into powder, heating to 473K at room temperature at the heating rate of 2K/min, and reacting for 12 h. After cooling to room temperature, it was washed three times with deionized water to remove residual impurities, yielding Co as shown in FIG. 13O4@ Mxenes composite, labeled CM-10%.
Example 2
(1) Mixing 3g of Ti3AlC2Immersing in 35mL of HF, sealing in a polytetrafluoroethylene cup, reacting at 313K, washing the obtained material with deionized water, centrifuging for 3-5 times to remove residual impurities, and drying in a vacuum oven at 333K overnight until constant weight is achieved to obtain Ti3C2TXAnd T represents a surface termination (e.g., -O, -F, or-OH).
(2) Mixing Ti3C2TXAnd 0.7g of Co (NO)3)2·6H2And O is mixed into deionized water, and the mixture is stirred vigorously to evaporate water, wherein the rotating speed is 400-500 rpm.
(3) Grinding the obtained product into powder, heating to 473K at room temperature at the heating rate of 2K/min, and reacting for 12 h. Cooling to room temperature, washing with deionized water for three times to remove residual impurities to obtain Co3O4@ Mxenes composite, labeled CM-20%.
Example 3
(1) Mixing 3g of Ti3AlC2Immersing in 35mLHF, sealing in a polytetrafluoroethylene cup, reacting at 313K, washing the obtained material with deionized water, centrifuging for 3-5 times to remove residual impurities, and drying in a vacuum oven at 333K overnight until constant weight is reached to obtain Ti3C2TXAnd T represents a surface termination (e.g., -O, -F, or-OH).
(2) Mixing Ti3C2TXAnd 1.05g of Co (NO)3)2·6H2And O is mixed into deionized water, and the mixture is stirred vigorously to evaporate water, wherein the rotating speed is 400-500 rpm.
(3) Grinding the obtained product into powder, heating to 473K at room temperature at the heating rate of 2K/min, and reacting for 12 h. Cooling to room temperature, washing with deionized water for three times to remove residual impurities to obtain Co3O4@ Mxenes composite, labeled CM-30%.
Application example 1
To the prepared aqueous solution containing 2, 4-dichlorophenol and peracetic acid, a catalyst (CM-20%) was added, and experiments were performed at initial pH values of 4, 5, 6, 7, 8, and 9, respectively. Adding peroxyacetic acid and the sandwich Co3O4The mixed solution of @ Mxenes composite material contains peroxyacetic acid as oxidant 0.26mM and catalyst (Co)3O4@ Mxenes) was added in an amount of 10mg/L, the concentration of the target contaminant 2, 4-dichlorophenol was 20. mu.M, and the reaction time was 20 min. The concentration of 2, 4-dichlorophenol was measured by sampling at predetermined times (0min, 2min, 5min, 10min, 15min, 20 min). 2(C) for removing 4-dichlorophenolt/C0) Is represented by C0Is the initial concentration of 2, 4-dichlorophenol, CtThe concentration of 2, 4-dichlorophenol at time t. As shown in figure 1, the treatment effect is best when the pH value is 7, and the removal rate of the pollutant 2, 4-dichlorophenol after 20min treatment reaches about 98%.
Application example 2
To the prepared aqueous solution containing 2, 4-dichlorophenol and peracetic acid, a catalyst (CM-20%) was added, and experiments were carried out at catalyst (CM-20%) addition levels of 5mg/L, 10mg/L, 20mg/L, 30mg/L, and 50mg/L, respectively. Initial pH 7, adding peracetic acid and the sandwich Co3O4In the mixed solution of the @ Mxenes composite material, the concentration of an oxidant peracetic acid is 0.26mM, the concentration of a target pollutant 2, 4-dichlorophenol is 20 mu M, and the reaction time is 20 min. The concentration of 2, 4-dichlorophenol was measured by sampling at predetermined times (0min, 2min, 5min, 10min, 15min, 20 min). (C) for removing 2, 4-dichlorophenolt/C0) Is represented by C0Is the initial concentration of 2, 4-dichlorophenol, CtThe concentration of 2, 4-dichlorophenol at time t. As shown in fig. 2, the removal efficiency of 2, 4-dichlorophenol increased with increasing catalyst addition in the range of catalyst (CM-20%) for this experimental design. When the addition amount of the catalyst (CM-20%) is 50mg/L, the treatment effect is optimal, and the removal rate of the pollutant 2, 4-dichlorophenol after 9min treatment reaches about 98%.
Application example 3
To the prepared aqueous solution containing 2, 4-dichlorophenol and peracetic acid was added a catalyst (CM-20%), and experiments were conducted at concentrations of the oxidants peracetic acid of 0.05mM, 0.10mM, 0.26mM, 0.52mM, 1.04mM, respectively. Initial pH 7, adding peracetic acid and the sandwich Co3O4In the mixed solution of the @ Mxenes composite material, the addition amount of a catalyst (CM-20%) is 10mg/L, the concentration of a target pollutant 2, 4-dichlorophenol is 20 mu M, and the reaction time is 20 min. The concentration of 2, 4-dichlorophenol was measured by sampling at predetermined times (0min, 2min, 5min, 10min, 15min, 20 min). (C) for removing 2, 4-dichlorophenolt/C0) Is represented by C0Is the initial concentration of 2, 4-dichlorophenol, CtThe concentration of 2, 4-dichlorophenol at time t. As shown in figure 3, the treatment effect is best when the concentration of the peroxyacetic acid oxidant is 0.26mM, and the removal rate of the pollutant 2, 4-dichlorophenol after 20min treatment reaches about 98%.

Claims (10)

1. Sandwich-shaped Co3O4The preparation method of the @ Mxenes composite material is characterized by comprising the following steps of:
(1) mixing 3g of Ti3AlC2Immersing in 35mL of HF, sealing in a polytetrafluoroethylene cup, reacting at 313K, washing the obtained material with deionized water, centrifuging for 3-5 times to remove residual impurities, and drying in a vacuum oven at 333K overnight until constant weight is achieved to obtain Ti3C2TXWherein T represents a surface termination comprising-O, -F, or-OH;
(2) ti obtained in the step (1)3C2TXAnd 0.35g to 1.05g of Co (NO)3)2·6H2Mixing O into deionized water, and violently stirring the mixture to evaporate water at the rotating speed of 400-500 rpm;
(3) grinding the obtained product into powder, heating to 473K at room temperature, and reacting for 12 h; cooling to room temperature, washing with deionized water for three times to remove residual impurities to obtain sandwich-shaped Co3O4@ Mxenes composites.
2. Co produced by the production method according to claim 13O4@ Mxenes composite material characterized in that Co (NO) in said step (2)3)2·6H2The amount of O added was 0.7 g.
3. Co produced by the production method according to claim 13O4@ Mxenes composite material characterized by Co attached in said composite material3O4The grain diameter is 25 nm-50 nm.
4. Using a sandwich-type Co according to claim 23O4The method for removing 2, 4-dichlorophenol in water by activating peracetic acid by the @ Mxenes composite material is characterized by comprising the following steps: adding peroxyacetic acid and the sandwich Co as catalyst into the sewage containing 2, 4-dichlorophenol as organic pollutant3O4@ Mxenes composites; adding peroxyacetic acid and the sandwich Co3O4In a mixed solution of @ Mxenes composite material, the sandwich-shaped Co3O4The concentration of the @ Mxenes composite material is 5 mg/L-50 mg/L, the concentration of the peroxyacetic acid is 0.05 mM-1.04 mM, and after the reaction is carried out for 2 min-20 min at normal temperature, the pollutant 2, 4-dichlorophenol in the sewage is removed.
5. Sandwich-shaped Co according to claim 43O4The application method of the @ Mxenes composite material for activating peroxyacetic acid to remove 2, 4-dichlorophenol in water is characterized in that the concentration of the peroxyacetic acid serving as an oxidant in a catalytic system is 0.26 mM.
6. Sandwich-shaped Co according to claim 43O4The application method of the @ Mxenes composite material for activating peroxyacetic acid to remove 2, 4-dichlorophenol in water is characterized in that the concentration of a catalyst in a catalytic system is 10 mg/L.
7. Sandwich-shaped Co according to claim 43O4The application method of the @ Mxenes composite material for activating peracetic acid to remove 2, 4-dichlorophenol in water is characterized in that the concentration of the target pollutant 2, 4-dichlorophenol is 20 mu M.
8. Sandwich-shaped Co according to claim 43O4Application method of @ Mxenes composite material for activating peroxyacetic acid to remove 2, 4-dichlorophenol in water, which is characterized in that the reaction is carried out at an initial pH of 7.0.
9. Sandwich-shaped Co according to claim 43O4The application method of the @ Mxenes composite material for activating peroxyacetic acid to remove 2, 4-dichlorophenol in water is characterized in that the reaction time is 20 min.
10. Sandwich-shaped Co according to claim 43O4The application method of @ Mxenes composite material for removing 2, 4-dichlorophenol in water by activating peroxyacetic acid is characterized in that the sandwich-shaped Co composite material3O4The @ Mxenes composite material is repeatedly recycled for 4 times, and the pollutant removal rate can still reach over 90 percent; the catalyst is recovered by filtration and then dried, and can be reused without additional activation.
CN202110701911.7A 2021-06-24 2021-06-24 Sandwich-shaped Co3O4@ Mxenes composite material and preparation method and application thereof Pending CN113559903A (en)

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CN114870882A (en) * 2022-06-13 2022-08-09 齐齐哈尔大学 Catalyst for quickly activating peroxyacetic acid to oxidize and degrade antibiotic wastewater based on microwaves and preparation and application methods thereof
CN114870882B (en) * 2022-06-13 2023-06-23 齐齐哈尔大学 Catalyst for oxidizing and degrading antibiotic wastewater based on microwave rapid activation of peroxyacetic acid and preparation and application methods thereof

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