CN112973739A - Composite catalyst for catalytic oxidation treatment of antibiotic wastewater - Google Patents
Composite catalyst for catalytic oxidation treatment of antibiotic wastewater Download PDFInfo
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- CN112973739A CN112973739A CN202110199086.5A CN202110199086A CN112973739A CN 112973739 A CN112973739 A CN 112973739A CN 202110199086 A CN202110199086 A CN 202110199086A CN 112973739 A CN112973739 A CN 112973739A
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention belongs to the technical field of antibiotic wastewater treatment, and particularly relates to a composite catalyst for catalytic oxidation treatment of antibiotic wastewater2Introduction into Fe3+In the catalyst, when the catalyst is used for catalytic oxidation treatment of antibiotic wastewater, Fe can be expanded by generating surface complex state ferric iron and accelerating the circulation of iron among different valence states in the reaction process3+The high pH value applicability of the method promotes the generation of free radicals of strong oxidizing species, thereby improving the removal effect of antibiotic pollutants under neutral conditions and reducing the generation of iron mud.
Description
Technical Field
The invention belongs to the technical field of antibiotic wastewater treatment, and particularly relates to a composite catalyst for catalytic oxidation treatment of antibiotic wastewater.
Background
Since penicillin is used for clinical treatment, thousands of antibiotics have been synthesized and widely used for treatment of human infectious diseases and industries such as aquaculture and livestock breeding, and provide effective guarantee for human production and life. However, the overuse of antibiotics has led to the constant detection of various drug-resistant bacteria and drug-resistant genes in the environment. Drug resistance genes can be transmitted between parents and other strains through inheritance and horizontal gene transfer to cause multiple drug resistance of bacteria, and seriously threaten human health, ecological safety and the effectiveness of a global public health system. The sewage treatment plant is the junction of human production and domestic sewage, and is also a storage house of antibiotics. However, the existing sewage treatment plants are difficult to completely remove antibiotics, so that a large amount of antibiotics are released into the environment and become a new pollutant which is widely concerned at home and abroad. Therefore, the development of a control technology for antibiotics in wastewater is one of the research hotspots and leading-edge subjects in the field of environmental science at present.
The advanced oxidation technology based on free radicals has the advantage of strong oxidation capability and has great advantage in the aspect of efficiently removing the organic pollutants difficult to degrade. Wherein, Fe is used2+Is a catalyst, H2O2The traditional Fenton reaction which is an oxidant has the characteristics of simple operation and strong oxidizing capability, is widely applied to the pollution control of organic pollutants, and has a plurality of practical industrial application cases. However, due to Fe3+Is unstable under the condition of high solution pH value, and the traditional Fenton reaction can only be used under the acidic condition (2.5-3). Meanwhile, after the reaction is finished, the pH of the effluent needs to be adjusted to a neutral environment. In this process, a large amount of iron sludge is generated, resulting in increased costs and secondary pollution.
Fe2+Can react with oxidant PMS to generate hydroxyl radical and sulfate radical, but Fe3+The precipitation and reduction difficulties of (a) seriously affect the activity of this technique. In order to solve the problem of iron ion precipitation, various solid iron-containing materials such as iron-containing minerals, iron oxides, and the like are widely used in the research of catalytic PMS. However, since the catalytic degradation of contaminants is a heterogeneous reaction process, limited by surface active sites, the activity of such reactions is often not high, resulting in too slow a degradation kinetics of the target contaminant. Aiming at the problem that the iron is difficult to convert between different valence states, the reduction of the iron is promoted by externally adding some reducing agents such as hydroxylamine hydrochloride, ascorbic acid and the likeAnd further, the generation of the oxidizing species can be significantly accelerated. However, these strong reducing agents are also radical scavengers themselves, have high solubility in aqueous solutions, are difficult to control in their optimal amounts during practical use, and may cause secondary pollution. Therefore, there is a need to develop a new catalyst to accelerate the iron cycling between different valence states and suppress Fe3+Hydrolytic precipitation under neutral/high pH conditions.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a composite catalyst for catalytic oxidation treatment of antibiotic wastewater, which is prepared by adding Fe3+Adding a cocatalyst MoS2The composite catalyst is formed, so that the high pH value applicability of the iron-based catalyst is improved, and the generation of iron mud is reduced.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a composite catalyst, which comprises MoS2And Fe3+。
Preferably, the Fe3+The mass content of the compound is 1-20 per mill.
The invention also provides a preparation method of the composite catalyst, which comprises the following steps:
s1, MoS2Adding the mixture into an aqueous solution of an iron source, and uniformly stirring and mixing to obtain a mixture;
and S2, drying the mixture to obtain the composite catalyst.
Preferably, the iron source is iron nitrate (Fe (NO)3)3)·9H2O。
Preferably, the pH of the aqueous solution of the iron source is 3.0.
Preferably, the stirring is magnetic stirring, and the stirring time is 0.5-1.5 hours. Further, the stirring time was 1 hour.
The invention also provides application of the composite catalyst in catalytic oxidation treatment of antibiotic wastewater.
Preferably, the pH of the antibiotic wastewater is 3.0-7.0.
PreferablySaid MoS2Including but not limited to commercial micron-sized MoS2。
MoS2Has a zero potential point of less than 2.0, and under the condition of water environment-related pH value (3-9), MoS2The surface has a large amount of negative charges, such as MoS2Positively charged Fe in aqueous solution as cocatalyst3+The ionic catalyst will quickly adsorb to the MoS2Surface, becomes iron in a surface complex state, thereby effectively blocking Fe3+Hydrolytic precipitation problems at high pH. Thus, in MoS2Can effectively expand Fe for cocatalyst3+The pH application range of the method solves the problem that the traditional homogeneous Fenton reaction is only suitable for acidic conditions. In addition, the circulation of Fe between different valence states during the catalytic reaction is a big problem. MoS2S in (1)2 6-Has high reducing activity and can accelerate Fe3+To Fe2+To accelerate the cycling of Fe between different valence states. MoS2This property of (2) allows for trace amounts of Fe3+Has high catalytic activity. Thus, by adding the cocatalyst MoS2The iron-based composite advanced oxidation catalyst provided by the invention is wide in applicable pH value and high in efficiency.
Preferably, the antibiotic includes, but is not limited to, sulfadiazine.
The invention also provides an oxidation degradation method of antibiotic wastewater, which is characterized in that the antibiotic in the wastewater can be catalytically degraded by adding the composite catalyst into the antibiotic wastewater containing PMS (peroxymonosulfate used as an oxidant) under stirring.
Preferably, the ratio of the composite catalyst to the antibiotic wastewater is (10-100) mg:100 mL. Further, the ratio of the composite catalyst to the antibiotic wastewater is 50mg to 100 mL.
Preferably, the concentration of PMS is 0.5 mM.
Preferably, the concentration of the antibiotic in the antibiotic wastewater is not more than 5 mg/L.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a composite catalystAdding a cocatalyst MoS2Introduction into Fe3+In the catalyst, when the catalyst is used for catalytic oxidation treatment of antibiotic wastewater, Fe can be expanded by generating surface complex state ferric iron and accelerating the circulation of iron among different valence states in the reaction process3+The high pH value applicability of the method promotes the generation of free radicals of strong oxidizing species, thereby improving the removal effect of antibiotic pollutants under neutral conditions and reducing the generation of iron mud. Overall, the invention has the following advantages:
(1) the composite catalyst adopted by the invention only contains MoS2And Fe3+. The catalyst is very simple in preparation process, can be prepared by simple stirring, mixing and drying, and does not need high-temperature high-pressure atmosphere and toxic and harmful reagent consumption. Therefore, the composite catalyst is environment-friendly and low in cost.
(2) In MoS2As a cocatalyst, Fe can be added3+The applicable range of pH of PMS oxidation system extends from acidic to neutral. Meanwhile, due to MoS2To complex state Fe3+By reductive transformation of MoS2The presence of (B) can significantly increase the trace amount of Fe3+Thereby avoiding the generation of a large amount of iron mud. Therefore, pH adjustment is not required before the reaction, and the iron sludge is not required to be treated after the reaction.
(3) In the composite catalyst, Fe in surface complex state3+Is catalytically active, and MoS2Mainly acts as a cocatalyst and, at the same time, MoS2Is insoluble in water. Thus, MoS2Has high stability and can be repeatedly used.
Drawings
FIG. 1 shows MoS2Electron micrographs of (a);
FIG. 2 shows the effect of the composite catalyst on the treatment of sulfadiazine antibiotic wastewater;
FIG. 3 is an electron spin resonance spectrum of a catalytic reaction with a composite catalyst;
FIG. 4 shows the treatment effect of the composite catalyst on sulfadiazine antibiotic wastewater under different pH conditions.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
MoS selected in the examples2A chemical reagent of commerce with a micro-structure (available from Shanghai Aladdin Biotechnology Co., Ltd.) and a specific surface area of about 14.8m2g-1(see FIG. 1).
Example 1 composite catalyst MoS2-1Fe treatment of antibiotic wastewater
(1) Catalyst preparation
72mg of iron nitrate (Fe (NO) were weighed out3)9·9H2O) to 20mL of deionized water (pH 3.0), after complete dissolution, 10g of MoS was added2Stirring was continued for another 1 hour. Then the mixture is dried in vacuum to prepare the composite catalyst MoS2-1Fe。
(2) Oxidative degradation of sulfadiazine antibiotic wastewater
0.05g of composite catalyst MoS is weighed2-1Fe, added to a sulfadiazine solution (5mg/L, 100mL) containing 0.5mM PMS with magnetic stirring to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from further oxidative degradation. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
MoS prepared in this example was dosed at 0.5mM PMS oxidant and 0.5g/L catalyst2The catalytic oxidation effect of-1 Fe on sulfadiazine is shown in figure 2. After 30 minutes of reaction, the initial concentration wasThe removal rate of 5mg/L sulfadiazine reaches 97 percent.
(3) Reactive oxygen species detection
In 0.5mM PMS oxidant and 0.5g/L MoS2Samples were taken after 5 and 10 minutes of reaction under-1 Fe catalyst, and the free radical scavenger 5, 5-dimethyl-1-pyrroline-N-oxide (DMPO) was added and analyzed for the generation of free radicals using an electron spin resonance spectrometer. As shown in fig. 3, the electron spin resonance spectrum shows signals of hydroxyl radicals and sulfate radicals, and the intensity of the signals increases with the extension of the reaction time. This result demonstrates that hydroxyl radicals and sulfate radicals are simultaneously generated during the catalytic reaction, which undergo oxidative degradation of sulfadiazine.
Example 2 MoS composite catalyst2-10Fe treatment of antibiotic wastewater
(1) Catalyst preparation
720mg of iron nitrate (Fe (NO) was weighed out3)9·9H2O) to 20mL of deionized water (pH 3.0), after complete dissolution, 10g of MoS was added2Stirring was continued for another 1 hour. Then the mixture is dried in vacuum to prepare the composite catalyst MoS2-10Fe。
(2) Oxidative degradation of sulfadiazine antibiotic wastewater
0.05g of composite catalyst MoS is weighed210Fe, added to a sulfadiazine solution (5mg/L, 100mL) containing 0.5mM PMS with magnetic stirring to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from further oxidative degradation. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
(3) MoS prepared in this example was dosed at 0.5mM PMS oxidant and 0.5g/L catalyst2The catalytic oxidation effect of-10 Fe on sulfadiazine is shown in figure 2. After 20 minutes of reaction, the removal rate of sulfadiazine with the initial concentration of 5mg/L is as high as 97%.
Example 3Composite catalyst MoS2Oxidative degradation of sulfadiazine antibiotic wastewater by-1 Fe under different pH conditions
With 0.1M H2SO4Or NaOH to adjust the pH of sulfadiazine solutions containing 0.5mM PMS to 3.0,4.0,5.5 and 7.0, respectively. Then 0.05g of the composite catalyst MoS prepared in example 1 was weighed out2-1Fe, added separately to sulfadiazine solutions of different pH values (5mg/L, 100mL) under magnetic stirring to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from further oxidative degradation. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
MoS prepared in this example was dosed at 0.5mM PMS oxidant and 0.5g/L catalyst2The catalytic oxidation effect of-1 Fe on sulfadiazine wastewater at different pH values is shown in FIG. 4. When the pH value is between 3 and 4, the total removal rate of sulfadiazine reaches 90 to 94 percent; when the pH value is increased to 7.0, the removal rate of sulfadiazine is increased to 97%.
Comparative example 1 using Fe3+Treatment of antibiotic wastewater
(1) Configuration of Fe3+Solutions of
Fe with 2g/L configuration3+Stock solution: 0.72g Fe (NO) was weighed out3)2·9H2O, and dissolved in 50mL of deionized water.
(2)Fe3+Catalytic PMS oxidative degradation of antibiotic sulfadiazine
50 μ L of 2g/L Fe prepared in advance was stirred under magnetic force3+The stock solution was added to sulfadiazine solution (5mg/L, 100mL) containing 0.5mM PMS to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from being further oxidized and degraded. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
At 0.5mM PMS oxidant and 1mg/L Fe3+Under the conditions, Fe in the comparative example3+The catalytic oxidation effect of the catalyst on sulfadiazine is shown in figure 2. After 30 minutes of reaction, the removal of sulfadiazine with an initial concentration of 5mg/L was only 9%.
Comparative example 2 composite catalyst MoS2-1Fe treatment of antibiotic wastewater
(1) Catalyst preparation
72mg of iron nitrate (Fe (NO) were weighed out3)9·9H2O) to 20mL of deionized water (pH 3.0), after complete dissolution, 10g of MoS was added2Stirring was continued for another 1 hour. Then the mixture is dried in vacuum to prepare the composite catalyst MoS2-1Fe。
(2) Adsorption removal of sulfadiazine antibiotic wastewater by composite catalyst
0.05g of composite catalyst MoS is weighed2-1Fe, added to 100mL sulfadiazine solution (5mg/L, 100mL) with magnetic stirring to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from further oxidative degradation. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
At 0.5g/L of composite catalyst MoS2The adsorption effect of the catalyst on sulfadiazine in this comparative example at the addition of-1 Fe is shown in FIG. 2. After 30 minutes of reaction, the removal of sulfadiazine with an initial concentration of 5mg/L was only 15%.
Comparative example 3 catalyst MoS2-0Fe treatment of antibiotic wastewater
(1) Preparation of a non-iron-containing catalyst
To 20mL of deionized water (pH 3.0) was added 10g of MoS2Stirring for 1 hour, and vacuum drying the mixture to obtain the catalyst MoS2-0Fe。
(2) Oxidative degradation of sulfadiazine antibiotic wastewater
0.05g of catalyst MoS is weighed out20Fe, added to a sulfadiazine solution (5mg/L, 100mL) containing 0.5mM PMS with magnetic stirring to start the catalytic degradation reaction. After reacting for a certain time, sampling 1mL by using a syringe, filtering the sample by using a 0.22 mu m PTFE filter membrane, placing the filtered sample in a 2mL liquid chromatography sample bottle, and then quickly adding 50 mu L of methanol to prevent the sulfadiazine from further oxidative degradation. The residual sulfadiazine concentration was analyzed by high performance liquid chromatography (Agilent 1260Infinity II) using water and methanol as mobile phases.
MoS prepared in this control example was treated with 0.5mM PMS oxidant and 0.5g/L catalyst addition2The catalytic oxidation effect of-0 Fe on sulfadiazine is shown in figure 2. After 30 minutes of reaction, the removal rate of sulfadiazine with an initial concentration of 5mg/L was 56%.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. A composite catalyst comprising MoS2And Fe3+。
2. The composite catalyst according to claim 1, wherein the Fe is Fe3+The mass content of the compound is 1-20 per mill.
3. The method for preparing the composite catalyst according to claim 1 or 2, comprising the steps of:
s1, MoS2Adding the mixture into an aqueous solution of an iron source, and uniformly stirring and mixing to obtain a mixture;
and S2, drying the mixture to obtain the composite catalyst.
4. The method according to claim 3, wherein the iron source is iron nitrate (Fe (NO)3)3)·9H2O。
5. The method according to claim 3, wherein the pH of the aqueous solution of the iron source is 3.0.
6. The method according to claim 3, wherein the stirring is magnetic stirring for 0.5 to 1.5 hours.
7. Use of the composite catalyst of claim 1 or 2 in catalytic oxidation treatment of antibiotic wastewater.
8. The use of claim 7, wherein the antibiotic includes, but is not limited to, sulfadiazine.
9. A method for oxidative degradation of antibiotic wastewater, characterized in that the antibiotic in the wastewater can be catalytically degraded by adding the composite catalyst of claim 1 or 2 to antibiotic wastewater containing PMS under stirring.
10. The method for oxidative degradation of antibiotic wastewater according to claim 9, wherein the ratio of the composite catalyst to the antibiotic wastewater is (10-100) mg:100 mL.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114291864A (en) * | 2021-11-19 | 2022-04-08 | 山东大学 | Based on MoS2/BiVO4Method for degrading pollutants by using photo-Fenton system with photocatalyst activated peroxymonosulfate |
| CN115814808A (en) * | 2021-10-27 | 2023-03-21 | 中国矿业大学 | Iron-molybdenum-doped hydrothermal carbon composite material, preparation method thereof and wastewater degradation method |
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| CN110227497A (en) * | 2019-06-19 | 2019-09-13 | 武汉轻工大学 | A kind of heterophase Fenton catalyst and its preparation method and application |
| CN110624569A (en) * | 2019-09-14 | 2019-12-31 | 北京建筑大学 | MoS doped with metal ions2Method for degrading PPCPs by activating monopersulfate |
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| CN115814808A (en) * | 2021-10-27 | 2023-03-21 | 中国矿业大学 | Iron-molybdenum-doped hydrothermal carbon composite material, preparation method thereof and wastewater degradation method |
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Application publication date: 20210618 |