CN116062850B - Reinforced Fe 2+ Concentration of bifunctional MoS 2 GF composite cathode, photoelectric Fenton system and application thereof - Google Patents
Reinforced Fe 2+ Concentration of bifunctional MoS 2 GF composite cathode, photoelectric Fenton system and application thereof Download PDFInfo
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Abstract
The invention relates to a method for enhancing Fe 2+ Concentration of bifunctional MoS 2 GF composite cathode, photoelectric Fenton system and application thereof, wherein the photoelectric Fenton system comprises a photo anode, a composite cathode, electrolyte solution and an external circuit, and the composite cathode is formed by modifying 0.2-0.6 mMMoS on the surface of GF electrode 2 (to prepare the Na for the composite cathode) 2 MoO 4 ·2H 2 O concentration gauge) formed MoS 2 -GF composite cathode, the electrolyte solution having Fe added thereto 2+ The method comprises the steps of carrying out a first treatment on the surface of the GF in the composite cathode can generate H in situ 2 O 2 And Fe in the electrolyte 2+ Initiating a free radical reaction; moS on the composite cathode 2 Can reduce Fe in solution 3+ Fe generation 2+ Ensure Fe in the solution 2+ HO. High efficiency and continuous generation, thereby improving the degradation and power generation performance of the organic wastewater of the photoelectric Fenton system.
Description
Technical Field
The invention relates to a composite cathode and a photoelectric Fenton system, in particular to a reinforced Fe 2+ Concentration of bifunctional MoS 2 -GF composite cathode material, electro-optical Fenton system based on the cathode and use thereof.
Background
A large amount of organic matters are discharged into the environmental water body in the modes of industrial wastewater, municipal sewage and the like, so that the environment is polluted, and the human health is seriously threatened. The traditional water treatment method has higher efficiency, but the process is complex and the energy consumption is higher; the organic wastewater also contains huge organic chemical energy, so that the energy requirement of water treatment can be met, and the organic wastewater has potential for external power generation (Sci Total Environ, 2019.668: p.966-978). If the energy can be utilized, the unnecessary consumption in the background of energy shortage can be reduced, and two problems of environmental protection and energy recovery are solved.
The photocatalytic wastewater fuel cell (PFC) can utilize solar energy to generate electron/hole pairs to oxidize and decompose organic matters and generate electricity externally, and has good application prospect. On the basis, B.X. Zhou et al describes Fe 2+ Introducing PFC to form a photoelectric Fenton (Fenton) system, fe 2+ Hydrogen peroxide (H) generated by the cathode 2 O 2 ) Fenton reaction is carried out to generate a large amount of hydroxyl free radicals (reaction 1), so that the degradation performance of organic matters is greatly improved (Water Research, 2017.108: p.293-300). However, in the photoelectric Fenton system, fe 2+ The consumption rate is far greater than the regeneration ratek 1 >>k 2 ) And can only play a role in a strong acid environment, which greatly limits the application and popularization of the compound.
H 2 O 2 + Fe 2+ → Fe 3+ + OH - + HO•k 1 = 76 M -1 •S -1 (1)
H 2 O 2 + Fe 3+ → Fe 2+ + O 2 • - + 2H + k 2 = 0.02 M -1 •S -1 (2)
In recent years, a great deal of research has been devoted to the promotion of Fe 2+ Regeneration rates, including methods of adding organic complexes and inorganic co-catalysts. However, these methods are not suitable for the photoelectric Fenton system, for example, secondary pollution is caused by adding an organic complex, light absorption efficiency of a photo-anode is greatly reduced by adding an inorganic co-catalyst, and performance of the photoelectric Fenton system is greatly reduced. Therefore, how to raise Fe 2+ The regeneration rate is not reduced, and the performance of the photoelectric Fenton system is not reduced and secondary pollution is not causedThe technical bottlenecks affecting the application of the system.
Disclosure of Invention
The invention aims to provide a reinforced Fe 2+ Concentration of bifunctional MoS 2 GF composite cathode material, photoelectric Fenton system based on cathode and application thereof, so as to solve the problem that the existing photoelectric Fenton system is capable of improving Fe 2+ The regeneration rate simultaneously causes the problems of system performance reduction and secondary pollution.
The invention is realized in the following way:
MoS-based 2 The photoelectric Fenton system of the GF composite cathode comprises a photo-anode, a composite cathode, an electrolyte solution and an external circuit, wherein the composite cathode is formed by modifying MoS on the surface of the GF electrode 2 Formed MoS 2 -GF composite cathode, the electrolyte solution having Fe added thereto 2+ The method comprises the steps of carrying out a first treatment on the surface of the In situ generation of H by GF in the composite cathode 2 O 2 And Fe in the electrolyte solution 2+ Reacting to generate HO; moS on the composite cathode 2 Reduction of Fe in solution using cathodic electrons 3+ Fe generation 2+ Enhancing Fe in system 2+ The concentration ensures the high-efficiency and continuous generation of HO. Free radicals, and finally realizes the high-efficiency degradation of organic wastewater and power generation of the PFC system.
The photo anode is WO 3 Nanometer film and PVC (Si solar cell slice, put in WO) 3 Subsequent absorption of transmitted light energy) to a substrate 3 And (3) PVC, wherein the electrolyte solution is 0.1-M sodium sulfate solution, and the pH value of the electrolyte solution is 3-11.
The composite cathode utilizes sodium molybdate crystals and thiourea to carry out MoS through a one-step hydrothermal method 2 Loaded on a carbon felt (GF) to form a molybdenum disulfide-carbon felt (MoS) 2 -GF), the concentration and the dosage of sodium molybdate crystals are 0.2-0.6 and mM, and the specific preparation method comprises the following steps:
1) Ultrasonically cleaning GF with acetone and deionized water for 30min, and drying at 60deg.C for 12 h; the washed GF was heated in a muffle furnace at 500℃for 1 h at a heating rate of 10℃per minute.
2) 0.2 to 0.6mM Na 2 MoO 4 ·2H 2 O and 1.6. 1.6 mM SulfurUrea as a precursor was dissolved in 60 mL deionized water and mixed sonicated for 30min.
3) The treated GF was immersed in the above solution and the mixture was transferred to a 100 mL reactor and heated at 220 ℃ for 36 h.
4) After cooling to room temperature, the mixture was washed 3 times with absolute ethanol and deionized water.
5) Drying at 60deg.C for 12 h to obtain MoS 2 -GF composite cathode.
The photoelectric Fenton system is used for treating organic wastewater, and can efficiently degrade organic matters in the wastewater and generate power.
The invention has the main advantages that:
(1) The invention modifies MoS with different concentrations on the surface of GF electrode 2 Forming the MoS 2 GF material is used as a cathode of a photoelectric Fenton system, and the GF is utilized to generate H in situ 2 O 2 And Fe in electrolyte 2+ Initiating a free radical reaction; at the same time MoS 2 Can utilize cathode electrons to reduce Fe 3+ Fe generation 2+ Thereby ensuring Fe in the solution 2+ And the concentration and the free radical reaction efficiency are achieved, and finally the high-efficiency degradation of organic matters and power generation of the photoelectric Fenton system are achieved. The reactions involved are as follows (reactions 3 and 4):
Mo 4+ + 2Fe 3+ → 2Fe 2+ + Mo 6+ (3)
Mo 6+ + H 2 O 2 → 2H + + Mo 4+ + O 2 (4)
(2) The invention does not need to additionally add H 2 O 2 GF on the composite cathode favors O 2 In situ generation of H by 2-electron process 2 O 2 。
(3) The invention does not need to continuously add Fe 2+ Fe is formed in the solution 3+ Can pass through MoS 2 Mo exposed in (b) 4+ Ion reduction back to Fe 2+ Ensure Fe in solution 2+ The concentration and radical reaction proceed efficiently and continuously.
(4) MoS of the invention 2 The performance of the GF composite cathode for the photoelectric Fenton system is superior to that of MoS 2 The powder does not need to be recovered for the second time.
(5) The photoelectric Fenton system is suitable for the environment with the pH value of 3-11, and the application range of the photoelectric Fenton system is greatly enlarged.
Drawings
Fig. 1 is a schematic diagram of the apparatus and operation of the present invention.
FIG. 2 shows GF electrode and MoS in the present invention 2 Scanning electron microscope image of GF electrode.
In the figure, a and c are surface electron micrographs of original GF electrodes; b and d are MoS 2 GF electrode surface electron microscopy.
FIG. 3 is a MoS of the present invention 2 Transmission electron microscopy of GF electrodes.
FIG. 4 shows the result of the simulation of sunlight AM1.5 (100 mW/cm) in example 1 2 ) MoS under irradiation conditions 2 GF cathode photoelectric Fenton system, pt electrode (comparative example 1), GF cathode (comparative example 2) and additive powder MoS 2 The organic matter degradation effect of the GF cathode (comparative example 3) system is compared.
FIG. 5 is a graph of example 1 in the case of simulated sunlight AM1.5 (100 mW/cm 2 ) MoS under irradiation conditions 2 GF cathode photoelectric Fenton system, pt electrode (comparative example 1), GF cathode (comparative example 2) and additive powder MoS 2 The power generation effect of the GF cathode (comparative example 3) system is compared.
FIG. 6 is a graph of the result of example 1 in the case of simulated sunlight AM1.5 (100 mW/cm 2 ) MoS under irradiation conditions 2 GF cathode photoelectric Fenton system and GF cathode system (comparative example 2), powder MoS is added 2 GF cathode system (comparative example 3) Fe 2+ Content comparison.
FIG. 7 is a graph of example 1 in the case of simulated sunlight AM1.5 (100 mW/cm 2 ) MoS under irradiation conditions 2 GF cathode photoelectric Fenton system and GF cathode system (comparative example 2), powder MoS is added 2 Ho. content comparison of GF cathode system (comparative example 3).
FIG. 8 is a graph of example 1 in the case of simulated sunlight AM1.5 (100 mW/cm 2 ) M under irradiation conditionsoS 2 -rhodamine B degradation performance comparison under different pH (3, 5, 7, 9, 11) conditions of GF cathodic photo-Fenton system.
FIG. 9 is a graph of MoS at various concentrations 2 (0 mM, 0.2. 0.2 mM, 0.3. 0.3 mM, 0.6. 0.6 mM) modification to MoS 2 -influence of GF cathode performance.
In the figure, a is MoS with different concentrations 2 Fe during modification 2+ Concentration comparison; b is MoS with different concentrations 2 HO. comparing the concentrations during modification; c is MoS with different concentrations 2 Comparing cyclic voltammograms during modification; d is MoS with different concentrations 2 Impedance contrast at modification.
FIG. 10 is a graph of MoS at various concentrations 2 (0.2 mM, 0.3 mM, 0.6mM, 1.0 mM, 3.0 mM, 6.0 mM) 2 -scanning electron microscopy of GF composite cathode.
In the figure, a and a' are 0.2 mM MoS 2 Modifying; b and b' are 0.3 mM MoS 2 Modifying; c and c' are 0.6mM MoS 2 Modifying; d and d' are 1.0 mM MoS 2 Modifying; e and e' are 3.0 mM MoS 2 Modifying; f and f' are 6.0 mM MoS 2 And (5) modification.
The MoS described in FIGS. 9-10 2 Concentration of Na used for preparing the composite cathode 2 MoO 4 ·2H 2 O concentration meter.
Detailed Description
The invention is further illustrated by the following examples, in which the processes and methods not described in detail are conventional and well known in the art, and in which the starting materials or reagents used are commercially available unless otherwise indicated.
FIG. 1 is a schematic diagram of the structure and operation principle of the electro-optic Fenton system according to the present invention, as shown in FIG. 1, moS 2 The GF composite cathode, the photo anode, the electrolyte solution and the external circuit form a photoelectric Fenton system. The photo anode is WO 3 PVC anode, which is connected with the three-dimensional MoS 2 The GF composite cathode was connected by copper wires and the electrodes were placed in a quartz reaction cell of 0.1M sodium sulfate solution. Ferrous sulfate is added into the electrolyte solution, and under the irradiation of simulated sunlight of a xenon lampH generated with cathode 2 O 2 Initiating chain radical reaction to produce a large amount of HO for degrading pollutants; moS (MoS) 2 Mo in GF composite cathode 4+ Fe can be extracted by cathode electrons 3+ Reduction to Fe 2+ Promote Fe 2+ The regeneration efficiency and the free radical generation are realized, and finally the degradation of organic pollutants and the improvement of the power generation efficiency of the photoelectric Fenton system are realized.
MoS for enhancing photoelectric Fenton performance 2 -a synthesis method of GF composite cathode, comprising the steps of:
1) Ultrasonically cleaning GF with acetone and deionized water for 30min, and drying at 60deg.C for 12 h; the washed GF was heated in a muffle furnace at 500℃for 1 h at a heating rate of 10℃per minute.
2) 0.2-6 mM Na 2 MoO 4 ·2H 2 O and 1.6 mM thiourea were dissolved as precursors in 60 mL deionized water and mixed sonicated for 30min.
3) The treated GF was immersed in the above solution and the mixture was transferred to a 100 mL reactor and heated at 220 ℃ for 36 h.
4) After cooling to room temperature, the mixture was washed 3 times with absolute ethanol and deionized water.
5) Drying at 60deg.C for 12 h to obtain MoS 2 -GF composite cathode material.
Selection of Na 2 MoO 4 ·2H 2 The concentration of O is 0.2 mM, 0.3 mM, 0.6mM, 1.0 mM, 3.0 mM and 6.0 mM, and the different concentrations of MoS for the surface modification of the GF electrode are respectively prepared 2 MoS of (F) 2 -GF composite cathode material. MoS (MoS) 2 Scanning electron microscope images and transmission electron microscope images of the GF composite cathode material are shown in figures 2, 3 and 10.
FIG. 9 is a graph of MoS at various concentrations 2 (0 mM, 0.2. 0.2 mM, 0.3. 0.3 mM, 0.6. 0.6 mM) modification to MoS 2 -influence of GF cathode performance.
Example 1
In WO 3 PVC as photoanode, moS 2 The GF composite cathode material is used as a reference electrode, and is connected by copper wires and is put into a quartz reaction tank containing 40 ml of 0.1M sodium sulfate solution (30 mg/L of the solution)The pellet B) was added with 0.5. 0.5 mM ferrous sulfate, the pH of the electrolyte was adjusted to 7.0, and a xenon lamp light source (100 mW/cm 2 ) Irradiating the photoanode, the MoS 2 The GF composite cathode is formed by modifying 0.3 mM MOS on the surface of GF electrode 2 (to prepare MoS as described above) 2 When GF is combined with cathode, na 2 MoO 4 ·2H 2 O concentration meter, hereinafter the same), wherein GF can generate H in situ 2 O 2 And Fe in the electrolyte 2+ Initiating a free radical reaction; moS on the composite cathode 2 Can reduce Fe in solution 3+ Fe generation 2+ Realize Fe in the system 2+ And HO. Continuous generation, so as to strengthen the high-efficiency degradation and power generation performance of the photoelectric Fenton system.
MoS-based as described in this embodiment 2 Fe at 60min in photoelectric Fenton system of GF composite cathode 2+ HO. Content 17.46 mg/L and 6.68X10, respectively -4 mol/L, rhodamine B removal rate of 96.03 percent and photocurrent density of 6.98 mA cm -2 。
The pH of the system (3, 5, 9 and 11) is changed, and the degradation performance of rhodamine B is shown in the figure 8, for example, and the removal rate of rhodamine B is 60 minutes on the ordinate of the figure.
The effects of example 1 are described below with 3 comparative examples.
Comparative example 1
As a control, moS was performed under the same conditions as those of example 1 2 The GF composite cathode is replaced by a Pt electrode, the rhodamine B removal rate of the system is 19.74% after 60min, 76.29% is reduced compared with the embodiment 1, and the photocurrent density is 0.372 mA cm -2 About 1/20 of the example.
Comparative example 2
As a control, moS was performed under the same conditions as those of example 1 2 -GF composite cathode was replaced with GF electrode, fe measured at 60min of system 2+ HO. Content of 5.96 mg/L and 1.85×10, respectively -4 mol/L, 1/3 and 1/4 of that in example 1, the removal rate of rhodamine B was 46.46%, 49.57% lower than that in example 1, and the photocurrent density was 5.66 mA cm -2 About 4/5 of the example.
Comparative example 3
As a control, moS was performed under the same conditions as those of example 1 2 -GF composite cathode replacement with GF electrode and MoS addition 2 Powder, fe at 60min of the system 2+ HO. Content of 7.79 mg/L and 3.55X10, respectively -4 mol/L, only reaching 2/5 and 1/2 of the example 1, the 60min rhodamine B removal rate of the battery is 69.07 percent, which is reduced by 26.96 percent compared with the example 1, and the photocurrent density is 4.77 mA cm -2 About 7/10 of the example.
Organic matter degradation effect, power generation effect and Fe of four systems of example 1, comparative example 2 and comparative example 3 2+ The content and ho were compared with each other, and the results are shown in fig. 4 to 7.
Example 2
In WO 3 PVC as photoanode, the MoS 2 The GF composite cathode material is used as a reference electrode, and is connected by copper wires, and is put into a quartz reaction tank containing 40 ml of 0.1M sodium sulfate solution (50 mg/L rhodamine B is contained in the tank), 0.5 mM ferrous sulfate is added, the pH value of the electrolyte is adjusted to 3.0, and a xenon lamp light source (100 mW/cm is added 2 ) Irradiating the photo anode, moS 2 The GF composite cathode is formed by modifying 0.2 mM MOS on the surface of GF electrode 2 Wherein GF may generate H in situ 2 O 2 And Fe in the electrolyte 2+ Initiating a free radical reaction; moS on the composite cathode 2 Can reduce Fe in solution 3+ Fe generation 2+ Realize Fe in the system 2+ And HO. Continuous generation, so as to strengthen the high-efficiency degradation and power generation performance of the photoelectric Fenton system.
MoS as described in this embodiment 2 At 60min, the removal rate of rhodamine B is 92.13 percent, and the photocurrent density is 6.03 mA cm in the photoelectric Fenton system of the GF composite cathode -2 。
Example 3
In WO 3 PVC as photoanode, the MoS 2 The GF composite cathode material is used as a reference electrode and is connected with the reference electrode through copper wiresPlacing into a quartz reaction tank containing 40 ml of 0.1M sodium sulfate solution (30 mg/L rhodamine B is contained in the tank), adding 0.25 mM ferrous sulfate, adjusting pH of the electrolyte to 9.0, adding xenon lamp light source (100 mW/cm) 2 ) Irradiating the photo anode, moS 2 The GF composite cathode is formed by modifying 0.3 mM MOS on the surface of GF electrode 2 Wherein GF may generate H in situ 2 O 2 And Fe in the electrolyte 2+ Initiating a free radical reaction; moS on the composite cathode 2 Can reduce Fe in solution 3+ Fe generation 2+ Realize Fe in the system 2+ And HO. Continuous generation, so as to strengthen the high-efficiency degradation and power generation performance of the photoelectric Fenton system.
MoS as described in this embodiment 2 At 60min, the removal rate of rhodamine B is 94.78% and the photocurrent density is 5.48 mA cm in the photoelectric Fenton system of the GF composite cathode -2 。
Example 4
In WO 3 PVC as photoanode, the MoS 2 The GF composite cathode material is used as a reference electrode, is connected by copper wires, is put into a quartz reaction tank containing 40 mL of 0.1M sodium sulfate solution (100 mg/L rhodamine B is contained in the tank), and is added with 0.5 mM ferrous sulfate, the pH value of the electrolyte is adjusted to 7.0, and a xenon lamp light source (100 mW/cm is added 2 ) Irradiating the photo anode, moS 2 The GF composite cathode is prepared by modifying the surface of a GF electrode by 0.6mM MoS 2 Wherein GF may generate H in situ 2 O 2 And Fe in the electrolyte 2+ Initiating a free radical reaction; moS on composite cathode 2 Can reduce Fe in solution 3+ Fe generation 2+ Realize Fe in the system 2+ And HO. Continuous generation, so as to strengthen the high-efficiency degradation and power generation performance of the photoelectric Fenton system.
MoS as described in this embodiment 2 At 60min, the removal rate of rhodamine B is 64.03% and the photocurrent density is 4.12 mA cm in the photoelectric Fenton system of the GF composite cathode -2 The method comprises the steps of carrying out a first treatment on the surface of the At 180 min, rhodamine B removal was 94.82%.
Claims (4)
1. MoS-based 2 The photoelectric Fenton system of the GF composite cathode comprises a photo-anode, a composite cathode, an electrolyte solution and an external circuit, and is characterized in that: the composite cathode utilizes sodium molybdate crystals and thiourea to carry out MoS through a one-step hydrothermal method 2 The concentration of sodium molybdate crystals loaded on GF is 0.2-0.6 mM; the preparation method of the composite cathode comprises the following steps:
1) Cleaning GF, drying and calcining in a muffle furnace for later use;
2) 0.2 to 0.6mM Na 2 MoO 4 ·2H 2 Dissolving O and 1.6 mM thiourea as precursors in deionized water, mixing and ultrasonic treatment for 30 min;
3) Immersing GF treated in the step 1) into the solution obtained in the step 2), and transferring the mixture into a reaction kettle to heat at 220 ℃ for 36 h;
4) Cooling to room temperature, and cleaning with absolute ethyl alcohol and deionized water;
5) Drying at 60deg.C to obtain MoS 2 -GF composite cathode;
the electrolyte solution is added with Fe 2+ The electrolyte solution has a pH of 3-11.
2. MoS-based according to claim 1 2 -a photoelectric Fenton system of GF composite cathode, characterized in that the photo anode is WO 3 PVC, the electrolyte solution is 0.1M Na 2 SO 4 A solution.
3. MoS-based according to claim 1 2 -a photoelectric Fenton system of GF composite cathodes, characterized in that: the step 1) is as follows: ultrasonically cleaning GF with acetone and deionized water for 30min, and drying at 60deg.C for 12 h; the washed GF was heated in a muffle furnace at 500℃for 1 h at a heating rate of 10℃per minute.
4. A MoS-based composition according to any one of claims 1-3 2 The use of a photoelectric Fenton system of a GF composite cathode in the treatment of organic waste water and in the recovery of electrical energy.
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