CN110803745B - Polyoxometallate composite particle electrode and preparation method and application thereof - Google Patents
Polyoxometallate composite particle electrode and preparation method and application thereof Download PDFInfo
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- CN110803745B CN110803745B CN201911295179.7A CN201911295179A CN110803745B CN 110803745 B CN110803745 B CN 110803745B CN 201911295179 A CN201911295179 A CN 201911295179A CN 110803745 B CN110803745 B CN 110803745B
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F1/46114—Electrodes in particulate form or with conductive and/or non conductive particles between them
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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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
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Abstract
The invention discloses a polyoxometallate composite particle electrode and a preparation method and application thereof, wherein the preparation method of the catalyst comprises the following steps: mixing PMO12Iron salt and CH3COOK is dissolved in ultrapure water, and the solution A is formed by stirring and mixing the solution A uniformly; adding methanol with the same volume into the solution A, adding a mesoporous titanium dioxide molecular sieve, and stirring and reacting at the temperature of 1-60 ℃ for 12-72 hours to react iron salt and PMO12React to form FePMO12Loading active ingredients onto the mesoporous titanium dioxide molecular sieve, filtering, drying filter residues to obtain the mesoporous titanium dioxide molecular sieve loaded FePMO12The material is the polyoxometallate composite particle electrode. The polyoxometallate composite particle electrode provided by the invention is used as a particle electrode of a three-dimensional electrode, so that the polyoxometallate composite particle electrode has the advantages of higher electrocatalysis performance, high current utilization efficiency, corrosion resistance and the like.
Description
Technical Field
The invention relates to a polyoxometallate composite particle electrode and a preparation method and application thereof.
Background
Backhurst first proposed the concept of Three-dimensional electrode (particle electrode) in 1969, which is a novel electrochemical reactor for filling granular or other forms of working electrode materials between electrodes of a traditional two-dimensional electrolytic cell. The charged working material surface is charged by an applied voltage to become an independent electrode (third stage), and electrochemical reaction is generated on each working material surface to form numerous micro-electrolysis baths. Compared with the traditional two-dimensional electrode, the three-dimensional electrode has larger specific surface area and higher electrolytic cell surface area ratio, can provide larger current intensity by using lower current density, provides faster mass transfer speed and reaction speed by using tiny particle spacing, improves current efficiency and space-time efficiency, and has better treatment effect.
The core of the three-dimensional electrode electrocatalytic oxidation technology is the particle electrode material, and the performance of the particle electrode determines the treatment efficiency and the operation cost of the electrocatalytic reaction. The traditional electrode material has poor electrocatalysis effect and low oxidation reduction capability, and in practical wastewater treatment application, the current efficiency is lower, the stability is poor, and meanwhile, the corrosion resistance of the material is poor, so that the service life of the electrode is shorter. Therefore, the research and the preparation of a novel three-dimensional particle electrode material are the key points for solving the problems.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a polyoxometallate composite particle electrode and a preparation method and application thereof.
The preparation method of the polyoxometallate composite particle electrode is characterized by comprising the following steps of: mixing PMO12Iron salt and CH3COOK is dissolved in ultrapure water, and the solution A is formed by stirring and mixing the solution A uniformly; adding methanol with the same volume into the solution A, adding a mesoporous titanium dioxide molecular sieve, and stirring and reacting at the temperature of 1-60 ℃ for 12-72 hours to react iron salt and PMO12React to form FePMO12Loading active ingredients onto the mesoporous titanium dioxide molecular sieve, filtering, drying filter residues to obtain the mesoporous titanium dioxide molecular sieve loaded FePMO12The material is the polyoxometallate composite particle electrode.
The preparation method of the polyoxometallate composite particle electrode is characterized by comprising the following steps of: the ferric salt is ferric nitrate; preparing the resulting solution A, the PMO12The molar ratio of the iron salt to the iron salt is 1: 1; the CH3COOK and PMO12The molar ratio of (A) to (B) is 0.1 to 2: 1.
The preparation method of the polyoxometallate composite particle electrode is characterized by comprising the following steps:
1) dissolving a titanium source in ultrapure water, and preparing a titanium sol solution for later use; taking a cationic surfactant cetyl trimethyl ammonium bromide as a structure directing agent, dissolving the structure directing agent in ultrapure water, and preparing to obtain a template agent sol solution for later use;
2) adding the template agent sol solution obtained in the step 1) into a titanium sol solution under the condition of stirring, carrying out stirring reaction at the temperature of 20-70 ℃ for 2-48 h, carrying out centrifugal separation, washing the obtained solid with ultrapure water, and drying to obtain a mesoporous titanium dioxide molecular sieve precursor;
3) placing the mesoporous titanium dioxide molecular sieve precursor obtained in the step 2) in a muffle furnace, and roasting in air atmosphere to obtain the mesoporous titanium dioxide molecular sieve.
The preparation method of the polyoxometallate composite particle electrode is characterized in that in the step 1), a titanium source is one or a mixture of more than two of butyl titanate, titanium nitrate, titanium sulfate and titanium hydrochloride; the concentration of the titanium sol solution prepared in the step 1) is 0.01-10 mol/L.
The preparation method of the polyoxometallate composite particle electrode is characterized in that in the step 2), the feeding molar ratio of a titanium source to cetyl trimethyl ammonium bromide is 0.05-1: 1; the rotating speed of the stirring reaction in the step 2) is 10-600 r/min.
The preparation method of the polyoxometallate composite particle electrode is characterized in that in the step 3), the roasting process is as follows: heating the mixture from room temperature to 120-1500 ℃ at the speed of 1-15 ℃/min, roasting at constant temperature for 0.5-10 h, and then naturally cooling to room temperature.
The polyoxometallate composite particle electrode prepared by the method.
The polyoxometallate composite particle electrode is applied to catalyzing organic matters in ozone oxidation wastewater.
The invention adopts self-made mesoporous titanium dioxide molecular sieve as a carrier to prepare FePMO12The catalyst is loaded into the internal pore channel structure of the self-made mesoporous titanium dioxide molecular sieve, the carrier material in the particle electrode is also formed by active components, and the catalytic activity is high when the content of the active components in the catalytic material is extremely high; simultaneous Ti and FePMO12The synergistic effect can be generated between the two, and hydroxyl free radicals (OH) with strong oxidizability can be generated under the electrolysis condition to degrade organic matters.
Specifically, compared with the prior art, the invention has the following beneficial effects:
1. the invention uses a homemade mediumTaking a porous titanium dioxide molecular sieve as a carrier, and loading FePMO on the carrier12The prepared catalytic material is porous, has large specific surface area, strong adsorption performance, no other inert components and good catalytic performance, and is a novel particle electrode;
2. the catalyst of the present invention utilizes TiO2And FePMO12The synergistic catalysis between the above two components generates OH with strong oxidizing property, and the catalyst has the characteristics of high strengthening efficiency and strong oxidizing capability;
3. the particle electrode of the invention is FePMO with catalytic function12Loaded on TiO with catalytic function2In the framework, the catalytic materials are all formed by active components, the surface-to-surface ratio of the active components is greatly improved, the loss of a small amount of catalytic materials cannot influence the catalytic activity of the catalyst in the use process, the service life of the catalyst is long, only a small amount of catalytic materials need to be supplemented under the long-time operation condition, and the treatment cost is greatly reduced.
4. The preparation method of the catalyst is simple and easy to implement, and is convenient for large-scale popularization. In the preparation process of the catalyst, the stabilizer is added to prevent butyl titanate from being hydrolyzed rapidly.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1:
a preparation method of a polyoxometallate composite particle electrode comprises the following steps:
1) dissolving butyl titanate in ultrapure water with the temperature of 50 ℃ and the pH =4 to prepare a titanium sol solution with the concentration of 0.5 mol/L;
2) CTAB (cetyl trimethyl ammonium bromide) is used as a structure guiding agent, and the structure guiding agent is dissolved in ultrapure water at 50 ℃ to prepare a CTAB solution with the concentration of 2.5 mol/L;
3) dropwise and slowly dropping the titanium sol solution obtained in the step 1) into the CTAB solution obtained in the step 2) with the same volume at a stirring speed of 200r/min, stirring and reacting for 8 hours at 55 ℃ to obtain a suspension containing a mesoporous titanium dioxide molecular sieve precursor, carrying out centrifugal separation, washing the obtained solid with ultrapure water to obtain a mesoporous titanium dioxide molecular sieve precursor, and drying the mesoporous titanium dioxide molecular sieve precursor in a drying oven at 95 ℃ for later use;
4) placing the mesoporous titanium dioxide molecular sieve precursor prepared in the step 3) in a muffle furnace, heating the precursor to 1200 ℃ from room temperature at a speed of 5 ℃/min, calcining the precursor at constant temperature for 4 hours, and naturally cooling the calcined precursor to room temperature to obtain the mesoporous titanium dioxide molecular sieve. Grinding the obtained mesoporous titanium dioxide molecular sieve sample through a 80-mesh screen, and drying the obtained powder in an oven at 115 ℃ for later use;
5）PMO12and Fe (NO)3)3Dissolving in ultrapure water, and preparing to obtain PMO12And Fe (NO)3)3Adding CH into solution A with the concentration of 1mol/L3COOK（CH3COOK and PMO in solution A12The molar ratio of (1) to (0.2), stirring and mixing uniformly, cooling, adding methanol with the same volume as the solution A, and mixing to obtain a mixed solution B. Adding the mesoporous titanium dioxide molecular sieve powder obtained in the step 4) into the mixed solution B (the dosage of the mesoporous titanium dioxide molecular sieve in the mixed solution B is 10 g/L), slowly stirring and reacting at the temperature of 40 ℃ for 8 hours, filtering, drying filter residues, and obtaining the mesoporous titanium dioxide molecular sieve loaded FePMO12The material is the polyoxometallate composite particle electrode.
Application example 1:
the polyoxometallate composite particle electrode, activated carbon and commercially available particle electrode (commercially available particle electrode as active ingredient TiO) obtained in example 1 were used2TiO with 0.1% loading2/Al2O3Particle electrodes) were compared for electrolytic performance, the procedure was as follows:
1) dissolving chloramphenicol into deionized water, and preparing to obtain chloramphenicol simulation wastewater. The pH of the chloramphenicol simulated wastewater was adjusted to 4, and the initial COD concentration of the chloramphenicol simulated wastewater was 950 mg/L.
2) The iridium tantalum/titanium plate and the graphite plate are respectively used as an anode and a cathode, and the polyoxometallate composite particle electrode prepared in example 1, activated carbon or a commercially available particle electrode are put into a three-phase reactor according to the particle electrode filling amount of 20g/L to prepare a three-phase three-dimensional electrode reactor. Carrying out a pre-adsorption test before electrolysis to eliminate the influence of adsorption, wherein the electrolytic solution is the chloramphenicol simulation wastewater prepared in the step 1), the voltage is 5V, the electrolyte conductivity is 3500 mu S/cm, and the ozone aeration rate is 1.2L/min, and the electrolytic solution with the volume of 650ml is subjected to electrifying electrolysis for 240min and then is sampled and analyzed. The comparative results after 240min of the electrolysis experiment using the polyoxometallate composite particle electrode prepared in example 1, activated carbon or commercially available particle electrode as the particle electrode are shown in table 1.
From table 1, it can be found that under the same operation conditions, the effect of the polyoxometallate composite particle electrode prepared by the invention is much higher than that of activated carbon, and compared with a commercially available particle electrode, the COD removal rate of chloramphenicol simulated wastewater by the catalyst of the invention is improved by about 20%, which indicates that the polyoxometallate composite particle electrode prepared by the invention has excellent performance.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (7)
1. A preparation method of a polyoxometallate composite particle electrode is characterized by comprising the following steps: will PMo12Iron salt and CH3COOK is dissolved in ultrapure water, and the solution A is formed by stirring and mixing the solution A uniformly; adding methanol with the same volume into the solution A, adding a mesoporous titanium dioxide molecular sieve, and stirring and reacting at the temperature of 1-60 ℃ for 12-72 hours to react iron salt and PMo12Reacted to form FePMo12Loading active ingredients onto the mesoporous titanium dioxide molecular sieve, filtering, drying filter residues to obtain the mesoporous titanium dioxide molecular sieve loaded FePMo12The material is the polyoxometallate composite particle electrode;
the ferric salt is ferric nitrate; preparing the resulting solution A, the PMo12And mols of iron saltsThe molar ratio is 1: 1; the CH3COOK and PMo12The molar ratio of (A) to (B) is 0.1 to 2: 1.
2. The method of claim 1, wherein the mesoporous titanium dioxide molecular sieve comprises the following steps:
1) dissolving a titanium source in ultrapure water, and preparing a titanium sol solution for later use; taking a cationic surfactant cetyl trimethyl ammonium bromide as a structure directing agent, dissolving the structure directing agent in ultrapure water, and preparing to obtain a template agent sol solution for later use;
2) adding the template agent sol solution obtained in the step 1) into a titanium sol solution under the condition of stirring, carrying out stirring reaction at the temperature of 20-70 ℃ for 2-48 h, carrying out centrifugal separation, washing the obtained solid with ultrapure water, and drying to obtain a mesoporous titanium dioxide molecular sieve precursor;
3) placing the mesoporous titanium dioxide molecular sieve precursor obtained in the step 2) in a muffle furnace, and roasting in air atmosphere to obtain the mesoporous titanium dioxide molecular sieve.
3. The method for preparing the polyoxometallate composite particle electrode as claimed in claim 2, wherein in the step 1), the titanium source is one or a mixture of more than two of butyl titanate, titanium nitrate, titanium sulfate and titanium hydrochloride; the concentration of the titanium sol solution prepared in the step 1) is 0.01-10 mol/L.
4. The method for preparing the polyoxometallate composite particle electrode as claimed in claim 2, wherein in the step 2), the feeding molar ratio of the titanium source to the cetyl trimethyl ammonium bromide is 0.05-1: 1; the rotating speed of the stirring reaction in the step 2) is 10-600 r/min.
5. The method of claim 2, wherein the step 3) of calcining comprises: heating the mixture from room temperature to 120-1500 ℃ at the speed of 1-15 ℃/min, roasting at constant temperature for 0.5-10 h, and then naturally cooling to room temperature.
6. A polyoxometalate composite particle electrode prepared by the process of any one of claims 1 to 5.
7. The use of the polyoxometallate composite particle electrode of claim 6 in catalyzing organic matter in ozone oxidation wastewater.
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