CN112408555B - Preparation and application of cuprous oxide/carbon nanotube/copper foam composite electrode for heterogeneous electro-Fenton system - Google Patents
Preparation and application of cuprous oxide/carbon nanotube/copper foam composite electrode for heterogeneous electro-Fenton system Download PDFInfo
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- CN112408555B CN112408555B CN202011273641.6A CN202011273641A CN112408555B CN 112408555 B CN112408555 B CN 112408555B CN 202011273641 A CN202011273641 A CN 202011273641A CN 112408555 B CN112408555 B CN 112408555B
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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
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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
- C02F1/46—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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
A preparation and application of a cuprous oxide/carbon nanotube/copper foam composite electrode for a heterogeneous electro-Fenton system relate to the technical field of electrochemical water treatment. According to the preparation method, the foamy copper is used as a matrix, the carboxylated carbon nanotubes are uniformly distributed in a three-dimensional porous structure of the foamy copper by a dip-coating method, then a two-electrode system is adopted for electrodeposition on the surface of the foamy copper, and finally the foamy copper/cuprous oxide/carbon nanotube composite electrode is prepared by placing the foamy copper in a muffle furnace for high-temperature calcination. The method has the advantages of simple and easy preparation, convenience and controllability, stable reaction system, no need of catalyst recovery, no subsequent pollution problem, capability of degrading organic pollutant wastewater well under a neutral condition and good application prospect.
Description
Technical Field
The invention relates to the technical field of electrochemical water treatment, in particular to a preparation method of a novel copper foam composite electrode loaded with cuprous oxide and carbon nano tubes and application of the electrode in a heterogeneous electro-Fenton system.
Background art:
the Copper Foam (CF) is a net structure material composed of a Copper matrix and three-dimensional holes, and compared with solid metal materials such as Copper plates and Copper sheets, the CF material not only has the excellent characteristic of good conductivity of the metal, but also has the advantages of large specific surface area, good permeability, high specific strength and the like. In recent years, the copper foam as a novel functional and structural material is widely applied and researched in many fields, and the research on pollutant degradation in an electro-Fenton system proves the application prospect of the copper foam in the field of water treatment. Carbon Nanotubes (CNTs) have the characteristic of large specific surface area and excellent electrochemical catalytic performance; research shows that the carbon nano tube can also improve the hydrogen peroxide (H) production by two-electron oxygen reduction 2 O 2 ) And can promote electron transfer; after the carbon nano tubes are modified on the foam copper, the specific surface area among pores is increased, and the catalytic activity of the electrode is further increased.
The traditional Fenton technique is to use external Fe feeding 2+ And H 2 O 2 The reaction generates hydroxyl radicals (. OH) with strong oxidizing property to remove the pollutants. But H 2 O 2 Is unstable in nature and dangerous in storage; and during the reaction, fe 2+ Will gradually generate Fe 3+ When the pH is more than 3, a large amount of iron sludge which is difficult to recover is easily formed.
The heterogeneous electro-Fenton technology overcomes the prior artThe Fenton technology has the defects of easy loss and difficult recovery of the catalyst, strict pH adjustment, easy sludge generation and the like, and gradually becomes a research hotspot in the advanced oxidation technology of water treatment. The composite electrode loaded with metal oxide is prepared and used as a cathode in the water treatment process to carry out in-situ catalytic oxidation, so that the defect that the catalyst is difficult to recover and separate can be effectively avoided; under near neutral conditions, cuprous oxide (Cu) 2 O) (containing monovalent copper) capable of forming strongly oxidizing hydroxyl radicals and Cu with hydrogen peroxide 2+ And does not produce sludge, cu 2+ Under the action of an electric field, electrons can be reduced into Cu + Thereby widening the pH value suitable for the traditional Fenton and improving the reusability of the electrode.
The cuprous oxide/carbon nanotube/copper foam composite electrode applied to the heterogeneous electro-Fenton system is prepared by utilizing the structural advantages of strong conductivity and three-dimensional porosity of copper foam and the capability of the carbon nanotube for promoting electron transfer and utilizing the good catalytic performance of cuprous oxide and directly loading the cuprous oxide on the copper foam coated with the carbon nanotube by an electrodeposition method, and the electrode is used for carrying out in-situ catalytic degradation on organic pollutants under the near-neutral condition and realizing the high-efficiency degradation of the pollutants; not only broadens the pH value applicable to the traditional Fenton, but also can not cause secondary pollution, and has no problem of subsequent catalyst recovery.
Disclosure of Invention
The invention aims to provide preparation and application of a cuprous oxide/carbon nanotube/copper foam composite electrode for a heterogeneous electro-Fenton system. The synthesis process is simple, convenient and controllable, the prepared electrode is applied to a heterogeneous electro-Fenton system under a near-neutral condition, the catalytic effect is good, and the defects that the traditional Fenton system needs strict pH adjustment, iron sludge is easy to generate, and the catalyst is difficult to recover are overcome.
A preparation method of a cuprous oxide/carbon nanotube/copper foam composite electrode for a heterogeneous electro-Fenton system comprises the following specific steps:
(1) Soaking and ultrasonically cleaning the foamy copper by using acetone, hydrochloric acid and absolute ethyl alcohol in sequence to remove oil stains and an oxidation layer on the surface of the foamy copper, and drying in vacuum for later use;
(2) Adding a nafion membrane solution (with the preferred mass fraction concentration of 5 wt%) into absolute ethyl alcohol to prepare a nafion solution with the mass fraction of 0.1-0.3 wt%; then adding carbon nanotubes (original carbon nanotubes and carbon nanotubes with different functional groups such as carboxylated carbon nanotubes, hydroxylated carbon nanotubes, aminated carbon nanotubes and the like, preferably carboxylated carbon nanotubes) with certain mass into the nafion solution, and carrying out ultrasonic treatment for 30min to obtain a uniform carbon nanotube dispersion liquid; the concentration of the carbon nano tube in the dispersion liquid is preferably 4-6g/L;
(3) Soaking the foamy copper obtained in the step (1) in the carbon nano tube dispersion liquid obtained in the step (2), uniformly pulling out the dispersion liquid at a speed of 1cm/s, repeatedly pulling for multiple times, putting the dispersion liquid into a blast drying oven to dry at the temperature of 40-60 ℃, obtaining a foamy copper cathode loaded with the carbon nano tube, which is marked as CNTs/CF, wherein the loading capacity of the carbon nano tube on the foamy copper is 1mg/cm 2 ～3mg/cm 2 Preferably 2mg/cm 2 ；
(4) Preparing 0.1-0.3M CuSO 4 Adding triethanolamine with a certain concentration, wherein the concentration is 0-4 g/L and is not 0, preferably 2.5g/L, and uniformly stirring and mixing to obtain an electrodeposition solution;
(5) The CNTs/CF electrode in the step (3) is used as a cathode, a Pt sheet is used as an anode, the distance between the electrodes is 1-5cm, the CNTs/CF electrode is placed in the electrodeposition solution prepared in the step (4), a two-electrode system is adopted at room temperature, the constant current is 360-800 mA, the deposition time is 1-5 min, the electrode is washed three times by deionized water, and the electrode is dried at room temperature;
(6) Placing the electrode obtained in the step (5) in a muffle furnace, heating to 150-250 ℃ at the speed of 4 ℃/min under the condition of continuously introducing air, calcining at constant temperature for 1-3h, and cooling to room temperature to obtain Cu 2 O/CNTs/CF electrode.
Cu obtained by the above preparation method 2 The O/CNTs/CF electrode is applied to a heterogeneous electro-Fenton system as a cathode, and is used for removing organic wastewater difficult to degrade by in-situ catalytic oxidation under a near-neutral condition.
Compared with the prior art, the invention has the following excellent effects:
1. according to the invention, the foamy copper is used as the electrode substrate, on one hand, the three-dimensional porous structure advantage of the foamy copper is utilized, and the three-dimensional pores can be formed without tabletting, so that the mass transfer efficiency is increased. On the other hand, the carbon nano tube is impregnated on the substrate, so that the capacity of hydrogen peroxide generation through two-electron oxygen reduction is promoted, the specific surface area among pores of the foam copper is increased, and the catalytic capacity of the electrode is also improved.
2. The method loads cuprous oxide in an electrodeposition mode, is simple, convenient and controllable to manufacture, and solves the problem that oxides are easily dispersed unevenly in the traditional coating, dipping, solvothermal and other modes.
3. The invention has better effect on degrading pollutants in water under the near-neutral condition, and widens the pH of the traditional Fenton. Meanwhile, cuprous oxide and carbon nanotubes are directly loaded on the foamy copper to be used as a cathode for in-situ electrocatalysis, hydrogen peroxide and a catalyst do not need to be added externally, secondary pollution is avoided, and the problem of subsequent catalyst recovery is solved.
Drawings
FIG. 1 shows Cu prepared in example 1 2 XRD result pattern of O/CNTs/CF electrode and the CNTs/CF electrode prepared and finished in comparative example 1.
In FIG. 2, a is the degradation of sulfamethoxazole wastewater by the original carbon nanotubes in comparative example 2; b is the degradation condition of the CNTs/CF electrode to the sulfamethoxazole wastewater in the comparative example 1, and c is Cu in the example 1 2 And (3) degrading sulfamethoxazole wastewater by using the O/CNTs/CF electrode. Wherein the ordinate corresponds to the ratio of the sulfamethoxazole concentration in the solution during degradation relative to the original sulfamethoxazole.
FIG. 3 is the effect of different concentrations of triethanolamine added in example 2 on the degradation of sulfamethoxazole wastewater. Wherein the ordinate corresponds to the ratio of the sulfamethoxazole concentration in the solution during degradation relative to the original sulfamethoxazole.
FIG. 4 is a graph showing the effect of different loading amounts (expressed as mass per unit area) of the carboxylated carbon nanotubes on the degradation of sulfamethoxazole wastewater in example 3. Wherein the ordinate corresponds to the ratio of the sulfamethoxazole concentration in the solution during degradation relative to the original sulfamethoxazole.
Detailed Description
The following description is given in conjunction with the accompanying drawings and specific embodiments, but the present invention is not limited to the following embodiments.
Example 1
(1) Soaking foamy copper (area size 2cm multiplied by 3 cm) in acetone, 0.1M hydrochloric acid and absolute ethyl alcohol in sequence, ultrasonically cleaning to remove oil stains and oxide layers on the surface of the foamy copper, and drying in vacuum for later use;
(2) Adding 0.4g of nafion membrane solution with the mass fraction of 5wt% into 9.6g of absolute ethyl alcohol to prepare nafion solution with the mass fraction of 0.2 wt%; then 0.063g of carboxylated carbon nanotube (the concentration of the carboxylated carbon nanotube is 5 g/L) is added into the nafion solution with the mass fraction of 0.2wt%, and ultrasonic treatment is carried out for 30min to obtain uniform carbon nanotube dispersion liquid;
(3) Soaking the foamy copper obtained in the step (1) in the carbon nano tube dispersion liquid obtained in the step (2), pulling out the dispersion liquid at a constant speed of 1cm/s, repeatedly pulling for many times, putting the dispersion liquid into a blast drying oven to dry at 60 ℃, and weighing the mass difference between the front and the back of the electrode, wherein when the mass difference is 0.024g, the loading capacity of the carboxylated carbon nano tube is 2mg/cm 2 The foamed copper cathode of (1), denoted as CNTs/CF;
(4) 100mL of 0.2M CuSO is prepared 4 Adding 0.25g of triethanolamine (the concentration is 2.5 g/L) into the solution, and uniformly stirring and mixing to obtain an electrodeposition solution;
(5) And (3) taking the CNTs/CF electrode in the step (3) as a cathode, taking a Pt sheet as an anode, placing the electrode with the electrode distance of 3cm in the electrodeposition solution prepared in the step (4), adopting a two-electrode system under the condition of water bath at 25 ℃, keeping constant current of 600mA, depositing for 3min, washing the electrode with deionized water for three times after deposition, and drying at room temperature.
(6) Placing the electrode obtained in the step (5) in a muffle furnace, heating to 200 ℃ at a speed of 4 ℃/min under the condition of continuously introducing air, calcining at constant temperature for 2h, and cooling to room temperature to obtain Cu 2 O/CNTs/CF electrode.
When the electrode is used as a cathode, a platinum sheet is used as an anode, a sodium sulfate solution with a positive-negative electrode spacing of 3cm and 0.05M is used as an electrolyte, the pH is =5.7, I =72mA, the aeration amount is 0.6L/min, 200mL sulfamethoxazole wastewater with a concentration of 10mg/L is degraded, and the degradation rate of sulfamethoxazole reaches 100% at 75min as shown by a curve c in FIG. 2.
Example 2
The preparation process is the same as that of example 1, but the concentration of triethanolamine in step (4) is changed to 0g/L, 1.0g/L, 2.5g/L and 4.0g/L in sequence. When the electrode is used as a cathode, a platinum sheet is used as an anode, a 0.05M sodium sulfate solution is used as an electrolyte, the pH is =5.7, I is =72mA, the aeration amount is 0.6L/min, 200mL sulfamethoxazole wastewater with the concentration of 10mg/L is degraded, and when the time is 75min, the degradation rate of sulfamethoxazole is optimal and reaches 100% when the addition amount of triethanolamine is 0.25g, namely the concentration of triethanolamine is 2.5g/L, as shown by a curve c in FIG. 3.
Example 3
The specific preparation process is the same as that of example 1, except that the steps (4), (5) and (6) are omitted, that is, electrodeposition is not performed, and only the loading amount of the carboxylated carbon nanotubes is changed to 1mg/cm in sequence 2 、2mg/cm 2 、3mg/cm 2 . When the above electrode was used as a cathode, a platinum sheet was used as an anode, 0.05M sodium sulfate was used as an electrolyte, pH =5.7, I =72mA, aeration amount was 0.6L/min, 200mL sulfamethoxazole wastewater with a concentration of 10mg/L was degraded, and at 120min, as shown by curve b in FIG. 4, when the loading amount of the carboxylated carbon nanotubes was 2mg/cm 2 The degradation rate of sulfamethoxazole is optimal and reaches 95%.
Comparative example 1
(1) Soaking foamy copper (area size 2cm multiplied by 3 cm) in acetone, 0.1M hydrochloric acid and absolute ethyl alcohol in sequence, ultrasonically cleaning to remove oil stains and oxide layers on the surface of the foamy copper, and drying in vacuum for later use;
(2) Adding 0.4g of nafion membrane solution with the mass fraction of 5wt% into 9.6g of absolute ethyl alcohol to prepare nafion solution with the mass fraction of 0.2 wt%; then 0.063g of carboxylated carbon nano tube is added into the nafion solution with the mass fraction of 0.2wt%, and ultrasonic treatment is carried out for 30min to obtain uniform carbon nano tube dispersion liquid;
(3) Soaking the foamy copper obtained in the step (1) in the carbon nano tube dispersion liquid obtained in the step (2), pulling out the dispersion liquid at a constant speed of 1cm/s, repeatedly pulling for many times, putting the dispersion liquid into a blast drying oven to dry at 60 ℃, and weighing the mass difference between the front and the back of the electrode, wherein when the mass difference is 0.024g, the loading capacity of the carboxylated carbon nano tube is 2mg/cm 2 The foamed copper cathode of (1), denoted as CNTs/CF;
the electrode is used as a cathode, a platinum sheet is used as an anode, a sodium sulfate solution with the anode-cathode spacing of 3cm and 0.05M is used as an electrolyte, the pH is =5.7, the I =72mA, the aeration amount is 0.6L/min, and 200mL sulfamethoxazole wastewater with the concentration of 10mg/L is degraded.
Comparative example 1 differs from example 1 in that carboxylated carbon nanotubes are only impregnated on copper foam, followed by no electrodeposition of cuprous oxide. At 120min, the degradation rate of sulfamethoxazole was 95%, as shown by curve b in FIG. 2.
Comparative example 2
The specific preparation process is the same as that of comparative example 1 except that steps (2) and (3) are omitted in order to pre-treat only the copper foam without impregnating the carboxylated carbon nanotubes and electrodepositing cuprous oxide. When the electrode is used as a cathode, a platinum sheet is used as an anode, a sodium sulfate solution with the anode-cathode spacing of 3cm and 0.05M is used as an electrolyte, the pH is =5.7, I =72mA, the aeration rate is 0.6L/min, 200mL sulfamethoxazole wastewater with the concentration of 10mg/L is degraded, and the degradation rate of sulfamethoxazole reaches 59.5% at 120min as shown by a curve a in FIG. 2.
Claims (4)
1. An application of a cuprous oxide/carbon nanotube/copper foam composite electrode for a heterogeneous electro-Fenton system is used as a cathode in the heterogeneous electro-Fenton system, and is used for removing organic wastewater by in-situ catalytic oxidation under a near-neutral condition, wherein the preparation method of the cuprous oxide/carbon nanotube/copper foam composite electrode comprises the following specific steps:
(1) Soaking and ultrasonically cleaning the foamy copper by using acetone, hydrochloric acid and absolute ethyl alcohol in sequence to remove oil stains and an oxidation layer on the surface of the foamy copper, and drying in vacuum for later use;
(2) Adding the nafion membrane solution into absolute ethyl alcohol to prepare nafion solution with the mass fraction of 0.1-0.3 wt%; then adding a certain mass of carbon nano tubes into the nafion solution, and carrying out ultrasonic treatment for 30min to obtain a uniform carbon nano tube dispersion liquid;
(3) Soaking the foamy copper obtained in the step (1) in the carbon nano tube dispersion liquid obtained in the step (2), uniformly pulling out the dispersion liquid at a speed of 1cm/s, repeatedly pulling for multiple times, putting the dispersion liquid into a blast drying oven to dry at the temperature of 40-60 ℃, obtaining a foamy copper cathode loaded with the carbon nano tube, which is marked as CNTs/CF, wherein the loading capacity of the carbon nano tube on the foamy copper is 1mg/cm 2 ～3mg/cm 2 ；
(4) Preparing 0.1-0.3M CuSO 4 Adding triethanolamine with a certain concentration into the solution, wherein the concentration is 0 g/L-4 g/L and is not 0, and uniformly stirring and mixing to obtain an electrodeposition solution;
(5) The CNTs/CF electrode in the step (3) is used as a cathode, a Pt sheet is used as an anode, the distance between the electrodes is 1-5cm, the CNTs/CF electrode is placed in the electrolyte solution prepared in the step (4), a two-electrode system is adopted at room temperature, the constant current is 360-800 mA, the deposition time is 1-5 min, the electrodes are washed three times by deionized water after deposition, and the electrodes are dried at room temperature;
(6) Placing the electrode obtained in the step (5) in a muffle furnace, heating to 150-250 ℃ at the speed of 4 ℃/min under the condition of continuously introducing air, calcining at constant temperature for 1-3h, and cooling to room temperature to obtain Cu 2 O/CNTs/CF electrode.
2. The use according to claim 1, wherein the concentration of the nafion membrane solution of step (2) is 5wt%.
3. The use of claim 1, wherein the carbon nanotubes of step (2) are original carbon nanotubes or different functionalized carbon nanotubes, and the functionalized carbon nanotubes are selected from one or more of carboxylated carbon nanotubes, hydroxylated carbon nanotubes and aminated carbon nanotubes.
4. The use according to claim 1, wherein the concentration of the carbon nanotubes in the dispersion of step (2) is 4 to 6g/L.
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| CN113968602B (en) * | 2021-10-25 | 2023-11-24 | 中国科学院合肥物质科学研究院 | Method for removing nitrified nitrogen in water by electrocatalytic treatment |
| CN113998760B (en) * | 2021-10-30 | 2023-09-19 | 北京工业大学 | Copper-cobalt oxide/carbon nano tube/foam nickel composite electrode for heterogeneous electro-Fenton system and application |
| CN113830863B (en) * | 2021-11-01 | 2023-01-20 | 北京工业大学 | Copper-cerium layered double metal hydroxide/carboxylated carbon nanotube/copper foam composite electrode and application |
| CN116874033A (en) * | 2023-06-09 | 2023-10-13 | 华北电力大学（保定） | Preparation method and application of three-dimensional structure electric cathode based on cuprous oxide |
| CN117342658A (en) * | 2023-10-24 | 2024-01-05 | 河海大学 | Fenton-like electro-catalysis coupling device for deep treatment of landfill leachate and application thereof |
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