CN112551650B - Preparation method and application of foamed nickel loaded carbon nanotube/copper electrode for water treatment - Google Patents
Preparation method and application of foamed nickel loaded carbon nanotube/copper electrode for water treatment Download PDFInfo
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- CN112551650B CN112551650B CN202011113042.8A CN202011113042A CN112551650B CN 112551650 B CN112551650 B CN 112551650B CN 202011113042 A CN202011113042 A CN 202011113042A CN 112551650 B CN112551650 B CN 112551650B
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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
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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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
- C02F1/46104—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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
Abstract
A preparation and application of a foamed nickel loaded carbon nanotube and a copper metal electrode for water treatment belong to the cross field of materials science, chemistry and environmental engineering. The invention uses electrophoretic deposition method to load carbon nano tube on the pretreated foam nickel matrix. The introduction of the carbon nano tube can provide a larger specific surface area and more nucleation sites for the active metal component Cu in the process of preparing the electrode by electrodeposition, promote the high dispersion of metal particles and improve the catalytic activity of the electrode. The cathode prepared by the method has the advantages of excellent electro-catalytic reduction performance, easy operation control, low cost and easy realization of industrialization, is applied to the electro-catalytic reduction method for treating nitrate wastewater difficult to degrade, and has good catalytic reduction effect.
Description
Technical Field
The invention provides a preparation and application method of a nickel foam-based loaded carbon nanotube/copper electrode. The method belongs to the crossed field of materials science, chemistry and environmental engineering.
Background
The electrocatalytic reduction method is one of reduction treatment technologies, has the advantages of high treatment efficiency, safety, environmental protection, easy control of operation and the like, is widely concerned by scholars in research on the method, and is applied to the field of treatment of various kinds of wastewater difficult to degrade. In conventional chemical catalytic reactions, electron transfer between the reactants and the catalyst is carried out in a confined area, and the transfer of electrons cannot be controlled from the outside. In addition, the catalytic hydrogenation method needs to continuously add hydrogen required by the reaction, and the flammable and explosive properties of the hydrogen cause great danger to the process. The electrocatalysis method can control the potential of the electrode by an external power supply, so that the reaction speed is easier to control. Various intermediates and products (NO) are produced during the electrocatalytic reduction of nitrate nitrogen in water 2 - /HNO 2 ，NH 3 /NH 4 + ，N 2 O and N 2 ) The nitrogen is the final ideal product after the nitrate nitrogen wastewater is treated. The application of the electrocatalytic reduction technology in the aspect of treating nitrate nitrogen in wastewater still lacks of a cathode material with high reduction efficiency, low cost and high nitrogen selectivity, which is also a key point and a difficulty point for limiting the application of the technology.
The foamed nickel is a three-dimensional mesh material prepared by adopting open-cell foamed plastic, preparing a conductive layer by chemical nickel plating, vacuum nickel plating and other methods, electroplating thick nickel in a general sulfate nickel plating electrolyte, and finally performing the working procedures of burning, reducing and annealing. The foam nickel has the characteristics of good electric and heat conducting properties, large specific surface area, low price and the like, and is widely applied to the aspects of fuel cells, catalyst carriers and the like.
The foamed nickel material with three-dimensional structure is different from the common electrode matrix, and provides a large surface area for a load material. Promoter copper metal, with a highly occupied d-orbital and an unclosed d-orbital shell, converts nitrate to nitrite, contributing to the electrocatalytic reduction of nitrate. The carbon nano tubes are electrophoretically deposited on the foam nickel substrate, and the introduction of the carbon nano tubes can provide more nucleation sites for an active metal component Cu in the process of preparing the electrode by electrodeposition, promote the high dispersion of metal particles and improve the conductivity and catalytic activity of the electrode. And then, electroplating a proper amount of Cu on the foamed nickel/carbon nanotube electrode to prepare the foamed nickel/carbon nanotube/copper electrode. The synergistic effect of different materials can improve the reaction rate and the nitrogen selectivity of the nitrate in the electrocatalytic reduction wastewater.
At present, researches on development of a nitrate electrolysis wastewater cathode material based on the characteristics of nickel foam are rarely reported, and researches and patents on application of a nickel foam loaded carbon nanotube/copper electrode to a nitrate technology in water treatment, particularly in electrocatalytic reduction wastewater have not been reported.
Disclosure of Invention
The invention provides an electrode based on foamed nickel loaded carbon nano tube/copper, which is applied to the field of water treatment, has the advantages of excellent material performance, simple preparation steps, low cost, good catalytic reduction effect and nitrogen selectivity, and is easy to realize industrial application.
The preparation process of the electrode comprises the following steps:
(1) Pretreatment of a foamed nickel matrix: and (3) putting the foamed nickel into acetone for ultrasonic oil removal for 20min, then putting the foamed nickel into a 0.5mol/L sulfuric acid solution for acid cleaning for 5-10min to remove surface oxides, finally, ultrasonically cleaning the foamed nickel in deionized water for 10min, and drying the foamed nickel for later use.
(2) Electrophoretic deposition of carbon nanotubes: stainless steel electrodes of the same area were used as anodes. The two electrodes were placed vertically, parallel to each other, at a distance of 10 mm. Preparing 250mL of 4g/L polyethylene glycol solution, adding 20mg of Carbon Nanotubes (CNTs), ultrasonically dispersing for 15min under the condition that the power is 400w, and adding 0.4g of Al into 80.0mg/L carbon nanotube suspension 2 (SO 4 ) 3 Since CNTs in the deposition solution will be at negative potential, surrounding Al 3 + Around Al 3 + Driven and deposited on the surface of the cathode under the action of the electric field force. After 10 minutes electrophoretic deposition (EPD) at 4-12V, the prepared Ni foam/CNTs electrode was dried in air at room temperature for 12 hours and stored in a vacuum desiccator.
(3) Ni foam/CNTs is taken as a cathode, ti/RuO 2 -Ir 2 O 3 Is an anode. And performing a cathodic electrodeposition experiment by using an intelligent double-pulse power supply. The Cu electrodeposition solution contains 20mmol/L CuSO 4 ·5H 2 O，0.05mol/LNa 2 SO 4 15g/L sodium citrate dihydrate (C) 6 H 5 Na 3 O 7 ) And 0.4g/L sodium lauryl sulfate (C) 12 H 25 SO 4 Na). Adopting constant current of 7mA/cm 2 After electrodeposition for 10-30 min, washing with deionized water. The prepared Ni foam/CNTs/Cu electrode is placed in a constant-temperature drying oven to be dried for 12 hours and then can be used.
The electrode prepared by the method is applied as a cathode in an electrocatalytic reduction system to treat nitrate nitrogen wastewater, and the conditions are as follows: the anode adopts Ti/RuO 2 -Ir 2 O 3 The electrode and the cathode adopt a Ni foam/CNTs/Cu electrode, the pH value is 3-9, and the current density is 4-8 mA/cm 2 The reaction time is 90-150 min, and the electrode distance is 5mm.
The nitrate nitrogen wastewater refers to inorganic nitrogen simulation wastewater containing nitrate ions, and the pollutants are relatively stable and difficult to treat.
In the invention, based on foam nickel loaded carbonThe nanotube electrode provides a larger specific surface area and more loading sites, divalent Cu ions are reduced to zero-valent metal by an electrodeposition method and loaded on the Ni foam/CNTs electrode to be used as a catalytic active center, the Ni foam/CNTs/Cu electrode adsorbs pollutants on the surface of the Ni foam/CNTs/Cu electrode, and the catalytic active sites loaded on the surface of the cathode firstly adsorb NO 3 - Reduction to NO 2 - Thereby degrading and reducing the pollutants into nitrogen for removal. The whole system is simple to operate and high in current efficiency. The electrode has stable property, high electrocatalytic reduction activity and good nitrogen selectivity. Has good effect of removing nitrate nitrogen under wide pH value and pollutant concentration range, and is an excellent electrode with industrial application prospect.
Drawings
FIG. 1a is a first SEM representation of the cathode used in example 1, and FIG. 1b is a second SEM representation of the cathode used in example 1.
FIG. 2 is an EDS characterization of the cathode used in example 1.
Figure 3 is an XRD characterization pattern of the cathode used in example 1.
FIG. 4 is a graph showing the time-dependent change in the concentration of waste water from the cathodic electrocatalytic reduction of nitrate nitrogen in example 1.
FIG. 5 is a graph showing the time-dependent change in the concentration of waste water from the cathodic electrocatalytic reduction of nitrate nitrogen in example 2.
FIG. 6 is a graph showing the time-dependent change in the concentration of waste water from the cathodic electrocatalytic reduction of nitrate nitrogen in example 3.
Fig. 7 is a graph showing the effect of stability of the cathode in example 1 after 6 times of repeated use.
Detailed Description
In order to better explain the spirit and content of the invention and to further illustrate the use of the invention, the following non-limiting examples of the invention are given, i.e. the content of the invention includes but is not limited to the following embodiments.
Example 1
Firstly, putting foamed nickel into acetone for ultrasonic oil removal for 20min, then putting the foamed nickel into a 0.5mol/L sulfuric acid solution for acid cleaning for 10min, finally, performing ultrasonic cleaning for 10min in deionized water, and drying for later use. In thatThe stainless steel plate with the same area is used as an anode in the process of electrophoretic deposition of the carbon nano tube. The two electrodes were placed vertically, parallel to each other, at a distance of 10 mm. The deposition experiments were performed under quiescent conditions. 250mL of 4g/L polyethylene glycol solution is prepared, 20mgCNTs is added, and ultrasonic dispersion is carried out for 15min under the condition that the power is 400 w. To 80.0mg/L of CNTs suspension was added 0.4gAl 2 (SO 4 ) 3 After 10 minutes electrophoretic deposition (EPD) at 12V, the prepared Ni foam/CNTs electrode was dried in air at room temperature for 12 hours and stored in a vacuum desiccator. Using Ni foam/CNTs as cathode, ti/RuO 2 -Ir 2 O 3 Electrodeposition experiments were performed for the anode. The electrodeposition solution contains 20mmol/L CuSO 4 ·5H 2 O， 0.05mol/LNa 2 SO 4 15g/L sodium citrate dihydrate (C) 6 H 5 Na 3 O 7 ) And 0.4g/L sodium lauryl sulfate (C) 12 H 25 SO 4 Na). Adopting constant current of 7mA/cm 2 After electrodeposition for 30min, rinsing with deionized water. The prepared Ni foam/CNTs/Cu electrode is put in a constant-temperature drying oven to be dried for 12 hours and then can be used.
From FIG. 1, it can be seen that the three-dimensional microscopic structure of the nickel foam has a net shape of pentagons with different sizes, which provides a large amount of space for loading the active components, and the tubular CNTs are uniformly coated on the surface. The foam nickel is loaded with a compact Cu crystal grain plating layer, and is formed by aggregating crystal grains with the average grain diameter of 1-10 mu m. As shown in FIG. 2, the EDS results show that the mass fractions of Cu and C in the active component are 31% and 0.6%, respectively, indicating that Cu and CNTs are successfully supported on the foamed nickel matrix.
In order to further determine the components and the existing forms of the active components, the XRD characterization is carried out on Ni foam/CNTs/Cu, and FIG. 3 is an XRD diffraction pattern of an electrode, and by comparing with a JCPDS standard diffraction pattern, diffraction peaks formed by Ni and Cu are determined, which shows that the Ni and Cu elements exist in the active components and exist in a simple substance state.
The electrode prepared by the method is used as a cathode in an electro-catalytic reduction system to treat simulated nitrate nitrogen wastewater. The specific operation is as follows: in a containerAdding 100mL of the above nitrate nitrogen wastewater into a 126mL electrolytic cell, adopting a commercial ruthenium iridium electrode as an anode and a Ni foam/CNTs/Cu electrode as a cathode, connecting a 0.2A direct current power supply to the anode and the cathode, wherein the electrode spacing is 5mm, and adding Na with the substance amount concentration of 0.05mol/L 2 SO 4 To provide electrolyte, NO 3 - The concentration of N was 100mg/L and the pH was 7. After the reaction is carried out for 150min, the degradation rate of nitrate nitrogen reaches 97.7 percent.
Example 2
Firstly, putting foamed nickel into acetone for ultrasonic oil removal for 20min, then putting the foamed nickel into a 0.5mol/L sulfuric acid solution for acid cleaning for 10min, finally, performing ultrasonic cleaning for 10min in deionized water, and drying for later use. The stainless steel plate with the same area is used as an anode in the process of electrophoretic deposition of the carbon nano tube. The two electrodes were placed vertically, parallel to each other, at a distance of 10 mm. The deposition experiments were performed under quiescent conditions. 250mL of 4g/L polyethylene glycol solution is prepared, 20mgCNTs is added, and ultrasonic dispersion is carried out for 15min under the condition that the power is 400 w. 0.4g/LAl was added to 80.0mg/L of the CNTs suspension 2 (SO 4 ) 3 After 10 minutes of electrophoretic deposition (EPD) at 8V, the prepared Ni foam/CNTs electrode was dried in air at room temperature for 12 hours and stored in a vacuum desiccator. Ni foam/CNTs is taken as a cathode, ti/RuO 2 -Ir 2 O 3 Is an anode. Cathodic electrodeposition experiments. The electrodeposition solution contains 20mmol/L CuSO 4 ·5H 2 O， 0.05mol/LNa 2 SO 4 15g/L sodium citrate dihydrate (C) 6 H 5 Na 3 O 7 ) And 0.4g/L sodium lauryl sulfate (C) 12 H 25 SO 4 Na). Adopting constant current of 7mA/cm 2 After electrodeposition for 20min, rinsing with deionized water. And (3) putting the prepared Ni foam/CNTs/Cu electrode in a constant-temperature drying oven to be dried for 12 hours to obtain the Ni foam/CNTs/Cu electrode.
The electrode prepared by the method is used as a cathode in an electro-catalytic reduction system to treat simulated nitrate nitrogen wastewater. The specific operation is as follows: 100mL of the above nitrate nitrogen wastewater was added to an electrolytic cell having a volume of 126mL, a commercial ruthenium iridium electrode was used as an anode, a Ni foam/CNTs/Cu electrode was used as a cathode,connecting the cathode and the anode with a 0.2A direct current power supply, wherein the electrode distance is 5mm, and adding Na with the substance amount concentration of 0.05mol/L 2 SO 4 To provide electrolyte, NO 3 - The concentration of N was 100mg/L and the pH was 7. After the reaction is carried out for 150min, the degradation rate of nitrate nitrogen reaches 97.5 percent.
Example 3
Firstly, putting foamed nickel into acetone for ultrasonic oil removal for 20min, then putting the foamed nickel into a 0.5mol/L sulfuric acid solution for acid cleaning for 10min, finally, performing ultrasonic cleaning for 10min in deionized water, and drying for later use. The stainless steel plate with the same area is used as an anode in the process of electrophoretic deposition of the carbon nano tube. The two electrodes were placed vertically, parallel to each other, at a distance of 10 mm. The deposition experiments were performed under quiescent conditions. 250mL of 4g/L polyethylene glycol solution is prepared, 20mgCNTs is added, and ultrasonic dispersion is carried out for 15min under the condition that the power is 400 w. To 80.0mg/L suspension of CNTs was added 0.4g/LAl 2 (SO 4 ) 3 After 10 minutes electrophoretic deposition (EPD) at 4V, the prepared Ni foam/CNTs electrode was dried in air at room temperature for 12 hours and stored in a vacuum desiccator. Ni foam/CNTs is taken as a cathode, ti/RuO 2 -Ir 2 O 3 Is an anode. Cathodic electrodeposition experiments. The electrodeposition solution contains 20mmol/L CuSO 4 ·5H 2 O， 0.05mol/LNa 2 SO 4 15g/L sodium citrate dihydrate (C) 6 H 5 Na 3 O 7 ) And 0.4g/L sodium lauryl sulfate (C) 12 H 25 SO 4 Na). Adopting constant current of 7mA/cm 2 After 10min of electrodeposition, rinsing with deionized water. And (3) putting the prepared Ni foam/CNTs/Cu electrode in a constant-temperature drying oven to be dried for 12 hours to obtain the Ni foam/CNTs/Cu electrode.
The electrode prepared by the method is used as a cathode in an electro-catalytic reduction system to treat simulated nitrate nitrogen wastewater. The specific operation is as follows: adding 100mL of the above nitrate nitrogen wastewater into an electrolytic cell with a volume of 126mL, adopting a commercial ruthenium iridium electrode as an anode and a Ni foam/CNTs/Cu electrode as a cathode, connecting a 0.1A direct current power supply to the anode and the cathode, wherein the electrode spacing is 5mm, and adding Na with a substance amount concentration of 0.05mol/L 2 SO 4 To supply electricitySolute, NO 3 - The concentration of N was 100mg/L and the pH was 7. After the reaction is carried out for 150min, the degradation rate of nitrate nitrogen reaches 83.2 percent.
Claims (2)
1. A preparation method of a foam nickel loaded carbon nanotube/copper electrode for water treatment is characterized by comprising the following steps:
(1) Pretreatment of a foamed nickel matrix: ultrasonic degreasing of foamed nickel in acetone for 20min, acid washing in 0.5mol/L sulfuric acid solution for 5-10min to remove surface oxide, ultrasonic washing in deionized water for 10min, and drying for later use;
(2) Electrophoretic deposition of carbon nanotubes: using stainless steel electrodes with the same area as an anode; the two electrodes are vertically arranged and parallel to each other, and the distance is 10 mm; preparing 250mL of 4g/L polyethylene glycol solution, adding 20mg of carbon nano tube CNTs, performing ultrasonic dispersion for 15min under the condition that the power is 400w, and adding 0.4g of Al into 80.0mg/L carbon nano tube suspension 2 (SO 4 ) 3 Because CNTs in the deposition solution will be in negative potential, surrounding Al 3 + Around Al 3 + Driven and deposited to the surface of the cathode under the action of the electric field force; after electrophoretic deposition is carried out for 10 minutes at a voltage of 4-12V, the prepared Ni foam/CNTs electrode is dried in air at room temperature for 12 hours and stored in a vacuum drier;
(3) Ni foam/CNTs is taken as a cathode, ti/RuO 2 -Ir 2 O 3 Is an anode; performing a cathodic electrodeposition experiment by an intelligent double-pulse power supply; the Cu electrodeposition solution contains 20mmol/L CuSO 4˙ 5H 2 O，0.05mol/LNa 2 SO 4 15g/L sodium citrate dihydrate and 0.4g/L sodium lauryl sulfate; constant current of 7mA/cm is adopted 2 After electrodeposition is carried out for 10-30 min, washing with deionized water; the prepared Ni foam/CNTs/Cu electrode is placed in a constant-temperature drying oven to be dried for 12 hours and then can be used.
2. Use of an electrode prepared according to the method of claim 1 as a cathode application in the treatment of nitrate nitrogen waste in an electrocatalytic reduction systemWater, with the conditions: anode adopts Ti/RuO 2 -Ir 2 O 3 The electrode and the cathode adopt a Ni foam/CNTs/Cu electrode, the pH value is 3-9, and the current density is 4-8 mA/cm 2 The reaction time is 90-150 min, and the electrode distance is 5mm.
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| CN115036142B (en) * | 2022-06-16 | 2023-05-02 | 成都信息工程大学 | Manganese dioxide electrode and preparation method and application thereof |
| CN115504544A (en) * | 2022-06-24 | 2022-12-23 | 浙江工业大学 | Cu-Bi/TiO 2 Preparation method and application of nano electro-catalytic denitrification electrode |
| CN115465923B (en) * | 2022-07-28 | 2024-02-13 | 湖南大学 | Method for treating nitrate wastewater by copper-nickel alloy three-dimensional composite electrode loaded with copper hydroxide |
| CN116161768B (en) * | 2023-04-26 | 2023-08-04 | 四川省生态环境科学研究院 | Sewage treatment method, adopted sewage treatment agent and preparation method thereof |
| CN117398983B (en) * | 2023-10-08 | 2024-04-26 | 北方工业大学 | Preparation method of sponge nickel-based heavy metal chromium ion adsorption material |
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