CN111348728B - MOF and HrGO co-modified bismuth vanadate electrode and preparation method and application thereof - Google Patents
MOF and HrGO co-modified bismuth vanadate electrode and preparation method and application thereof Download PDFInfo
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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
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- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses an MOF and HrGO co-modified bismuth vanadate electrode, a preparation method thereof and application thereof in the field of photoelectrocatalysis, wherein the preparation method comprises the following steps: (1) dissolving bismuth nitrate in nitric acid, adding ammonium metavanadate and polyvinyl alcohol, and performing ultrasonic treatment to obtain a seed solution; coating the seed solution on clean conductive glass, drying and calcining the conductive glass, and taking the conductive glass out to be used as a substrate electrode for later use; (2) dissolving bismuth nitrate and ammonium metavanadate in nitric acid, putting the nitric acid and the ammonium metavanadate into the substrate electrode prepared in the step (1), performing hydrothermal reaction, and calcining the obtained product after the reaction is finished to obtain BiVO4An electrode; (3) dissolving 2-amino terephthalic acid in DMF (dimethyl formamide), dissolving butyl titanate in methanol, mixing and stirring the two solutions uniformly, adding reduced graphene oxide obtained by hydrogen plasma treatment, mixing uniformly, and finally adding the BiVO4Electrode, carrying out solvothermal reaction to obtain BiVO4/NH2MIL125-HrGO composite thin film electrode.
Description
Technical Field
The invention relates to the technical field of photoelectrocatalysis electrode materials, in particular to a MOF and HrGO co-modified bismuth vanadate electrode and a preparation method and application thereof.
Background
Under the promotion of industrial process and rapid economic development, the use of a large amount of organic matters causes water pollution caused by the enrichment of waste water containing the organic matters in a water environment, and how to economically, effectively and low-energy-consumption water pollution treatment is urgent. Solar energy is a green energy, has abundant resources and does not generate secondary pollution, thereby drawing wide attention. The photocatalysis with sunlight as the driving force can generate photoproduction electron and hole pairs under the light irradiation, and is widely applied to the degradation of organic pollutants. However, the development of a novel photocatalyst/electrode using visible light as a driving force is one of the current research focuses, due to the defects that photo-generated electrons and holes are easily recombined, powder recovery is difficult, and solar energy utilization rate is low. The photocatalytic electrode film is prepared, and the separation of photoproduction electrons and holes can be promoted by proper external bias, so that the problems are hopeful to be solved.
In the field of photoelectrocatalysis, the search for a photoelectrocatalysis electrode with low cost, high efficiency and high stability is key. Since the band position of the photocatalytic electrode semiconductor has a significant influence on the photocatalytic efficiency, bismuth vanadate (BiVO) is currently known as an n-type semiconductor4) Has higher photocatalytic activity, durability and chemical stability due to proper positions of a conduction band and a valence band, is an ideal material for preparing a photocatalytic electrode, but is simply BiVO4The specific surface area is low, the photogenerated electron-hole pairs are easy to recombine, and the performance still needs to be greatly improved.
The Metal Organic Frameworks (MOFs) are a kind of hybrid porous materials composed of metal-oxygen clusters and organic structural units, are novel inorganic-organic hybrid materials, have wide application prospects, and have been proved to have photocatalytic activity in recent years due to the fact that diversified and easily-regulated structures attract various concerns.
Yang et al prepared powdered BiVO by two-step hydrothermal method4The first step of the method is to prepare MIL-125(Ti) in a hydrothermal mode, the MIL-125(Ti) is used as a carrier, and BiVO is grown in situ on the MIL-125(Ti) through a hydrothermal method4. When the molar ratio of Bi to Ti is 3:2, the obtained composite material has the best photocatalytic activity on rhodamine B. However, the powder material is prepared by the technical scheme, and BiVO grows in situ on MIL-125(Ti)4And can not be directly applied to electrode preparation. Because the electrode preparation must be substrate/BiVO4The structure of MIL-125(Ti) cannot implement the in-situ growth of BiVO on MIL-125(Ti)4Means of (4).
Among carbon-based materials, carbon nanotubes, Graphene Oxide (GO), and carbon nitride have been studied as effective architectures for substance adsorption and separation. In recent years, GO has attracted attention because of its excellent electrical conductivity, special quantum characteristics, unique mechanical properties, and the like, and is widely used as a modifier in the preparation of high-efficiency photocatalysts. The reduced GO (namely rGO) can be obtained by reduction treatment.
Therefore, further MOF and rGO modifications on bismuth vanadate electrodes still need to be explored further.
Disclosure of Invention
Aiming at the defects in the field, the invention provides a preparation method of an MOF and HrGO co-modified bismuth vanadate electrode, and the obtained electrode can be used as a photoelectrocatalysis electrode, has better visible light response and better photoelectrocatalysis capability, and has wide prospects in the field of catalytic degradation of organic wastewater.
A preparation method of a MOF and HrGO co-modified bismuth vanadate electrode comprises the following steps:
(1) dissolving bismuth nitrate in nitric acid, adding ammonium metavanadate and polyvinyl alcohol, and performing ultrasonic treatment to obtain a seed solution; coating the seed solution on clean conductive glass, drying and calcining the conductive glass, and taking the conductive glass out to be used as a substrate electrode for later use;
(2) dissolving bismuth nitrate and ammonium metavanadate in nitric acid, putting the nitric acid and the ammonium metavanadate into the substrate electrode prepared in the step (1), performing hydrothermal reaction, and calcining the obtained product after the reaction is finished to obtain BiVO4An electrode;
(3) dissolving 2-amino terephthalic acid in DMF (dimethyl formamide), dissolving butyl titanate in methanol, mixing the two solutions, stirring, adding reduced graphene oxide (HrGO) obtained by hydrogen plasma treatment, mixing, and adding the BiVO4Electrode, carrying out solvothermal reaction to obtain BiVO4/NH2MIL125-HrGO composite thin film electrode.
The invention is in BiVO4BiVO of electrode4In-situ growth and uniform NH loading on semiconductor surface2MIL125 and very small amount of HrGO, forming a heterogeneous massThe junction structure improves the efficiency of photoproduction electron separation, thereby improving photoelectric conversion efficiency, improving photoelectric response and improving photoelectric catalysis efficiency, and the obtained electrode is applied to photocatalytic degradation of waste water containing organic matters, so that an excellent degradation effect can be generated.
The step (1) is used for forming the bismuth vanadate film on the conductive glass, which is beneficial to the more uniform and better performance of the hydrothermal reaction and bismuth vanadate deposition in the step (2).
In the step (1), the molar ratio of bismuth nitrate to ammonium metavanadate is 1: 1.
Preferably, in step (1), the calcining temperature is 450 ℃ and the time is 2 h.
Preferably, in the step (2), the temperature of the hydrothermal reaction is 180 ℃ and the time is 12 h.
Preferably, in the step (2), the calcining temperature is 450 ℃ and the calcining time is 2 h.
Preferably, in the step (3), the ratio of the 2-aminoterephthalic acid, butyl titanate and reduced graphene oxide is 0.5-1 mmol: 1/6-1/3 mmol: 1-5 mg.
Preferably, in the step (3), the molar ratio of the 2-aminoterephthalic acid to the butyl titanate is 3:1, and the volume ratio of the DMF to the methanol is 1: 1. NH with special shape and structure prepared according to the preferable molar ratio of 2-amino terephthalic acid to butyl titanate2MIL125 may better perform a synergistic effect in the electrode system of the present invention.
Compared with general reduced graphene oxide (rGO), the reduced graphene oxide (HrGO) obtained by hydrogen plasma treatment can be combined with BiVO4、NH2The MIL125 plays a synergistic role, and the photoelectric catalytic performance of the obtained material is further promoted to be improved.
The preferred preparation method of the reduced graphene oxide (HrGO) obtained by the hydrogen plasma treatment in the invention comprises the following steps: and putting GO into a plasma processing device, vacuumizing, introducing hydrogen until the air pressure is 10-20 Pa, and starting discharging, wherein the discharging processing time is 10-60 min, and the optimal time is 40 min.
Preferably, in the step (3), the temperature of the solvothermal reaction is 150 ℃ and the time is 12 h.
Preferably, the hydrothermal reaction process of step (2) and the solvothermal reaction process of step (3) are both performed with the conductive surface of the conductive glass facing downward.
The invention also provides BiVO prepared by the preparation method4/NH2MIL125-HrGO composite film electrode.
BiVO is firstly added in the invention4Growing on the surface of the conductive glass material, and then adding NH2Semiconductor BiVO loaded with MIL125 and HrGO4Surface of BiVO to4A heterojunction structure is formed, and the recombination of photogenerated electrons can be effectively inhibited in the application of photoelectrocatalysis. The obtained electrode has lower charge transfer resistance, higher photoelectric conversion efficiency and separation efficiency of photon-generated carriers, and has good photoelectrocatalysis activity. Photoelectrochemical tests show that BiVO4/NH2MIL125-HrGO composite film electrode is BiVO4The electrode has higher photocurrent, lower impedance and higher photocatalytic activity.
The invention also provides the BiVO4/NH2The MIL125-HrGO composite membrane electrode can be applied to the field of photoelectrocatalysis, for example, can be used as a photoelectrocatalysis working electrode for treating phenol-containing wastewater.
Compared with the prior art, the invention provides BiVO prepared by a solvothermal method4/NH2The MIL125-HrGO composite film electrode realizes that a catalyst is uniformly loaded on the surface of a semiconductor to form a heterojunction structure, improves the efficiency of photoproduction electron separation, thereby improving the photoelectric conversion efficiency, improving the photoelectric response and improving the photoelectric catalysis efficiency, is applied to photocatalytic degradation of waste water containing organic matters, and can generate a better degradation effect. The main advantages of the invention include:
1. the invention relates to a novel high-efficiency photoelectrocatalysis BiVO4/NH2MIL125-HrGO composite membrane electrode by NH2MIL125 and HrGO in BiVO4BiVO is improved by one-step solvothermal loading on the electrode4The photoelectrocatalysis performance of the electrode realizes effective separation and efficient utilization of photon-generated carriers.
2. The photoelectrode can be repeatedly used and has good cycle performance.
3. The secondary filtration of the treated water body is not needed, and the cost is saved.
Drawings
FIG. 1 is a graph comparing the degradation effects of different photoelectrocatalytic electrodes prepared in example 4;
FIG. 2 is a graph comparing the effect of photoelectric degradation of the non-composite electrode and the composite electrode in example 5;
FIG. 3 is an I-T plot of different photocatalytic electrodes prepared in example 6;
FIG. 4 is a graph of the impedance of various photocatalytic electrodes prepared in example 7 under visible light;
fig. 5 is a graph showing the cycling effect of the composite photoelectrocatalysis electrode prepared in example 8.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are conducted under conditions not specified, usually according to conventional conditions, or according to conditions recommended by the manufacturer.
In the following examples, the FTO electrode was specified to be 2X 5cm, 2.2mm thick, 7 ohm resistance, and 80% transmittance.
Example 1
A preparation method of a photoelectrocatalysis electrode comprises the following steps:
(1) 0.3234g Bi (NO)3·5H2O is dissolved in 1mL of concentrated nitric acid (70 wt%), then 2mL of distilled water is added, and after mixing uniformly, 0.078g of NH is added4VO3And 0.167g of polyvinyl alcohol (PVA, 99%) were dissolved in the above solution, and sonicated for 30min to obtain a seed solution.
(2) 20 μ L of the seed solution was smeared on clean FTO, dried in vacuum for 1h and calcined in a muffle furnace at 450 ℃ for 2 h.
(3) 0.06mmol of Bi (NO)3·5H2O and 0.06mmol NH4VO3Dissolving in 400 μ L concentrated nitric acid (70 wt%), addingAdding distilled water to 15mL, then placing the mixture into an autoclave, placing the BiVO obtained in the step (2) after the mixture is burnt in a muffle furnace with the conductive surface facing downwards4The sheet is hydrothermal at 180 ℃ for 12h, washed with distilled water and calcined in a muffle furnace at 450 ℃ for 2h to obtain BiVO4And an electrode.
(4) Dissolving 0.75mmol of 2-amino terephthalic acid in 7.5mL of dimethylformamide, dissolving 0.25mmol of butyl titanate in 7.5mL of methanol, uniformly mixing the two solutions, adding 2mg of HrGO, uniformly mixing by ultrasound for 30 minutes, putting the mixture into an autoclave, and adding the BiVO obtained in the step (3)4Placing the electrode in the container with the conductive surface facing downwards, and solvothermal at 150 ℃ for 12h to obtain BiVO4/NH2MIL125-HrGO electrode.
The HrGO used in the present example was prepared by the following method: 100mg of GO was reduced in a plasma treatment device. First, a vacuum is drawn to ensure that air is exhausted. And finally, regulating the flow meter to introduce hydrogen until the air pressure is 15Pa, and starting discharging for 40 min.
Example 2
This example prepares BiVO4/NH2MIL125-GO and BiVO4/NH2The procedure for the MIL125-rGO electrode was substantially the same as in example 1, except that:
after the two solutions are uniformly mixed in the step (4), 2mg of GO and 2mg of rGO are respectively added, the mixture is uniformly mixed by ultrasonic for 30 minutes and then is put into a high-pressure kettle, and the prepared BiVO is respectively put into the high-pressure kettle4Placing the electrode with the conductive surface facing downwards in the solution, and carrying out solvothermal at 150 ℃ for 12h to obtain BiVO4/NH2MIL125-GO electrode and BiVO4/NH2MIL125-rGO electrode.
The GO and rGO used in this example were prepared by the following method:
preparing Graphene Oxide (GO) by adopting an improved Hummers method and a chemical oxidation method by taking natural graphite powder as a raw material; the preparation method comprises the steps of preparing rGO by a chemical synthesis method, pre-reducing the prepared graphene oxide by sodium borohydride at 80 ℃ for 1h, sulfonating the graphene oxide by aryl diazonium salt containing sulfanilic acid in ice bath for 2h, and reacting the graphene oxide with hydrazine at 100 ℃.
Example 3
This example prepares BiVO4/NH2The procedure for the MIL125 electrode was substantially the same as in example 1, except that:
the two solutions are stirred evenly in the step (4) and then directly put into the prepared BiVO4Placing the electrode in the solution with the conductive surface facing downwards, and carrying out solvothermal at 150 ℃ for 12h to obtain BiVO4/NH2MIL125 electrode.
Example 4
BiVO prepared for testing4/NH2MIL125-HrGO electrode and BiVO4/NH2MIL125-GO electrode and BiVO4/NH2The photocatalytic activity of the MIL125-rGO electrode, with phenol as the target contaminant.
The following method was used for the experiments:
20mL of phenol wastewater with the concentration of 5mg/L is prepared, 0.1M anhydrous sodium sulfate is added to serve as an electrolyte, the prepared electrode serves as an anode, a polished titanium sheet serves as a cathode, and the applied direct-current voltage is controlled to be 2V. Stirring in dark for 30min to reach adsorption equilibrium, passing light source through 420nm filter to filter out ultraviolet light, turning on the light source while electrifying, reacting for 90min, detecting phenol residue by high performance liquid chromatography, and recording data, with the result shown in FIG. 1. As can be seen from FIG. 1, the phenol degradation effects after compounding rGO and GO are not very different, and the phenol degradation rate can be remarkably improved by compounding a very small amount of HrGO, which indicates that BiVO in the invention4、NH2HrGO and BiVO in a three-component system of MIL125 and graphene4、NH2MIL125 has a good synergistic effect. BiVO4/NH2The MIL125-HrGO electrode has the best degradation effect on phenol degradation.
Example 5
To test the BiVO prepared in example 14/NH2MIL125-HrGO electrode and BiVO in example 34/NH2MIL125 electrode and uncomplexed BiVO prepared according to the steps (1) to (3) of example 14The photoelectrocatalytic activity of the electrode was tested by the same method as in example 4, using phenol degradation as a model.
As shown in fig. 2, it can be seen that after 90min of light irradiation, the electrode prepared in example 1 can remove more than 99% of phenol, while the electrode without supported HrGO has a phenol removal rate of about 83% under the same conditions. From FIG. 2, it can be seen that BiVO is a complex4/NH2MIL125-HrGO electrode vs BiVO4/NH2The photoelectrocatalysis activity of the MIL125 electrode is obviously improved.
As can be seen from FIGS. 1 and 2, BiVO is a substance4/NH2The photoelectrocatalysis activity obtained by combining general GO and rGO on the basis of MIL125 is not greatly improved, which shows that the general GO, the rGO and the BiVO are not greatly improved4、NH2The synergy between MIL125 is weak, while HrGO is particularly suited to BiVO4/NH2MIL125 system.
Example 6
BiVO prepared in test example 14/NH2MIL125-HrGO electrode and BiVO in example 34/NH2MIL125 electrode and uncomplexed BiVO prepared according to the steps (1) to (3) of example 14The photocurrent-time curve of the electrode under the bias voltage of 0.2V (vs. Ag/AgCl) is as follows: the current-time curve was tested in a 0.2V (vs. Ag/AgCl) bias in 0.1M anhydrous sodium sulfate and 0.1M anhydrous sodium sulfite solution using a standard three-electrode system, the prepared electrode as the working electrode, an Ag/AgCl electrode as the reference electrode, and a platinum sheet electrode as the counter electrode. As can be seen from FIG. 3, BiVO4/NH2The MIL125-HrGO electrode had the best visible response.
Example 7
BiVO prepared in test example 14/NH2MIL125-HrGO electrode and BiVO in example 34/NH2MIL125 electrode and uncomplexed BiVO prepared according to the steps (1) to (3) of example 14The electrode has alternating current impedance under visible light, and the specific test conditions are as follows: adopting a standard three-electrode system, taking a prepared electrode as a working electrode, an Ag/AgCl electrode as a reference electrode, a platinum sheet electrode as a counter electrode, taking 0.5M anhydrous sodium sulfate solution as an electrolyte solution in an impedance box, and adopting an impedance point location program to test under the irradiation of visible light, wherein the amplitude is 5mM, and the frequency range is 10-2-105Hz. As can be seen from FIG. 4, BiVO4/NH2The MIL125-HrGO electrode had the smallest radius of resistance, indicating the least resistance to electron transport.
Example 8
The cyclicity is an important index for verifying the stability of the photoelectrocatalysis electrode. In practical application, the photoelectrocatalysis electrode with higher stability can reduce the cost and improve the utilization rate. In order to explore the BiVO prepared by the invention4/NH2The stability of the MIL125-HrGO composite electrode on phenol degradation is that on the basis of phenol degradation in the embodiment 5, the phenol degradation operation in the embodiment 5 is repeated after the electrode is washed and dried, and the change of phenol degradation performance after multiple cycles is compared.
After several cycles, BiVO, as shown in FIG. 54/NH2The removal effect of the MIL125-HrGO composite electrode on phenol can still reach more than 94 percent, so that the BiVO prepared by the method is considered4/NH2The MIL125-HrGO composite electrode has good cycle performance and can be used for carrying out continuous photoelectrocatalysis degradation on phenol-containing wastewater.
In conclusion, the composite photocatalytic BiVO of the invention4/NH2MIL125-HrGO electrode relative to BiVO4The electrode has higher photoelectrocatalysis activity and has potential application prospect in the fields of solar energy utilization and wastewater.
Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention defined by the appended claims.
Claims (6)
1. A preparation method of a MOF and HrGO co-modified bismuth vanadate electrode is characterized by comprising the following steps:
(1) dissolving bismuth nitrate in nitric acid, adding ammonium metavanadate and polyvinyl alcohol, and performing ultrasonic treatment to obtain a seed solution; coating the seed solution on clean conductive glass, drying and calcining the conductive glass, and taking the conductive glass out to be used as a substrate electrode for later use;
(2) dissolving bismuth nitrate and ammonium metavanadate in nitric acidPutting the substrate electrode prepared in the step (1) into the reaction kettle for hydrothermal reaction, and calcining the reaction kettle after the reaction is finished to obtain BiVO4An electrode;
(3) dissolving 2-amino terephthalic acid in DMF (dimethyl formamide), dissolving butyl titanate in methanol, mixing and stirring the two solutions uniformly, adding reduced graphene oxide obtained by hydrogen plasma treatment, mixing uniformly, and finally adding the BiVO4Electrode, carrying out solvothermal reaction to obtain BiVO4/NH2MIL125-HrGO composite thin film electrodes;
the proportion of the 2-amino terephthalic acid, the butyl titanate and the reduced graphene oxide is 0.5-1 mmol: 1/6-1/3 mmol: 1-5 mg;
the preparation method of the reduced graphene oxide comprises the following steps: and putting GO into a plasma processing device, vacuumizing, introducing hydrogen until the air pressure is 10-20 Pa, and starting discharging for 10-60 min.
2. The method according to claim 1, wherein in step (3), the molar ratio of 2-aminoterephthalic acid to butyl titanate is 3:1, and the volume ratio of DMF to methanol is 1: 1.
3. The method according to claim 1, wherein in the step (3), the temperature of the solvothermal reaction is 150 ℃ and the time is 12 hours.
4. The production method according to claim 1 or 3, wherein the hydrothermal reaction process of step (2) and the solvothermal reaction process of step (3) are performed while the conductive surface of the conductive glass is placed downward.
5. BiVO prepared by the preparation method according to any one of claims 1 to 44/NH2MIL125-HrGO composite film electrode.
6. BiVO according to claim 54/NH2MIL125-HrGO composite thin film electrode in the field of photoelectrocatalysisThe use of (1).
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