CN115504544A - Cu-Bi/TiO 2 Preparation method and application of nano electro-catalytic denitrification electrode - Google Patents
Cu-Bi/TiO 2 Preparation method and application of nano electro-catalytic denitrification electrode Download PDFInfo
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Abstract
The invention belongs to the technical field of electrocatalysis water treatment, and particularly relates to Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode comprises the step of carrying out electro-deposition treatment on copper-bismuth metal on the surface of a titanium dioxide nano electrode to obtain Cu-Bi/TiO 2 Nano-electrode and illustrates the use of the nano-electrode in the electrocatalytic reduction removal of nitrate nitrogen from water. The prepared Cu-Bi/TiO 2 In water by nano electro-catalytic electrodeThe nitrate nitrogen has high reaction activity and high removal efficiency, and has great application prospect.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis water treatment, and particularly relates to Cu-Bi/TiO 2 A preparation method and application of a nano electro-catalytic denitrification electrode.
Background
Nitrate is an oxyanion which does not form a ligand, has high mobility, and is soluble in water. However, nitrate pollution in surface and ground water is caused by artificial activities, including chemical fertilizer runoff in agricultural land, rain water runoff from urban surfaces, and discharge of sewage or treated wastewater. The world health organization and the U.S. environmental protection agency limit the maximum contaminant levels in drinking water to 50mg/L (NO 3-) and 10mg/L (NO 3-N). Therefore, the removal of nitrate from environmental sources such as surface waters and groundwater is critical to preventing such problems. Electrochemical techniques are considered to be the most promising industrial popularization technique due to their environmental suitability, stability and ease of operation.
The electrode material influences dynamics and product selectivity in the electrochemical nitrate reduction process, so the key of the electrocatalytic reduction technology lies in the selection of the electrode material and the catalyst, and the material with good performance has the characteristics of good electrocatalytic performance, higher conductivity and stability. The noble metals such as Pt, pd and Ru are expensive in cost although having good electrocatalytic activity, and Cu has high reaction kinetics speed, but the main product taking the copper plate as the cathode is ammonia nitrogen and lacks stability, so that the copper plate is easy to corrode. Therefore, the search for electrodes with excellent performance is significant for researching water treatment.
Disclosure of Invention
In response to the problems of the prior art, the present invention provides a Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode solves the problem of low wastewater treatment efficiency in the past, and can be used for electro-catalytic reduction of nitrate nitrogen in water.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode comprises the following steps:
step 1, pretreatment of a titanium substrate: respectively polishing a titanium plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh abrasive paper until the surface is free of scratches, washing the surface by using deionized water, sequentially putting the titanium plate into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic treatment for 10min, and finally taking out and drying the titanium plate for later use;
step 2, preparing the titanium dioxide nano electrode: taking a graphite electrode as a cathode, a pretreated titanium sheet as an anode, ammonium fluoride with the mass fraction of 0.28% and ethylene glycol solution with the mass fraction of 9.0% as electrolyte, anodizing for 3 hours at room temperature under the condition of constant voltage of 25V, washing the surface of the electrode after the reaction is finished, naturally airing, putting the electrode into a muffle furnace, calcining for 2 hours at 500 ℃, and naturally cooling; the titanium sheet and the graphite electrode have the same area;
step 3, preparing the electrodeposition solution: (1) Preparing copper electrodeposition liquid, taking 0.01mol/L copper sulfate as main salt and 0.01mol/L disodium ethylene diamine tetraacetate as complexing agent, adding water, and fully stirring until the copper-containing electrodeposition liquid is completely dissolved to obtain copper-containing electrodeposition liquid; preparing an electrodeposition solution of bismuth: taking 0.01mol/L bismuth nitrate pentahydrate as a main salt, taking 0.01mol/L disodium ethylene diamine tetraacetate as a complexing agent, taking 1g/L potassium chloride as an electrolyte, adding water, and fully stirring until the bismuth nitrate pentahydrate and the disodium ethylene diamine tetraacetate are dissolved to obtain an electro-deposition solution containing bismuth; (3) preparing mixed electrodeposition liquid: mixing copper-containing electrodeposition liquid and bismuth-containing electrodeposition liquid to obtain mixed electrodeposition liquid; the molar concentration ratio of copper ions to bismuth ions in the mixed deposition solution is 1-4;
step 4, electrodeposition: electroplating at room temperature with the titanium dioxide nano-electrode as cathode and graphite electrode with equal area as anode at current density of 2mA/cm2 for 20s to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
The Cu-Bi/TiO 2 The nano electrode is used for removing nitrate nitrogen in water through electrocatalytic reduction.
The invention selects two non-noble metals (Cu and Bi) as catalysts, the Cu metal has good promotion effect on the speed limiting step in the nitrate reduction process, the electrolysis product of the Bi electrode is mainly nitrogen, and the selectivity is between 58% and 65%, therefore, the invention takes the titanium dioxide nano electrode as a carrier, and the Cu and Bi are doped in the titanium dioxide nano electrode, thereby effectively improving the electrode performance.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention takes the titanium dioxide nano electrode as the substrate, has good stability, multiple reaction points, good corrosion resistance and higher specific surface area, provides a good carrier for metal copper bismuth, and utilizes and improves the efficiency of electro-catalytic reduction of nitrate nitrogen.
2. The invention adopts a simple formula of frontal electrodeposition, has good stability and long storage time. 3. The invention adopts an electrodeposition method to prepare Cu-Bi/TiO 2 The nano electrode is simple to operate and easy to scale.
4. Cu-Bi/TiO prepared by the invention 2 In the nano electrode, the size of copper and bismuth belongs to the nano level, the distribution is uniform, and the specific surface is large.
5. Cu-Bi/TiO prepared by the invention 2 The nano-electrode has more excellent removal efficiency than a conventional electrode.
Drawings
FIG. 1 shows Cu-Bi/TiO prepared in example 1 of the present invention 2 Scanning electron microscope images of the nanoelectrodes;
FIGS. 2 to 4 show Cu-Bi/TiO compounds prepared in example 1 of the present invention 2 Analyzing an image of the energy spectrum of the nano electrode;
FIG. 5 shows Cu-Bi/TiO prepared in example 1 of the present invention 2 A time-varying rule graph of the removal effect of the nano-electrode on nitrate nitrogen, wherein: the molar concentration ratio of Cu2+ and Bi3+ is 1;
FIG. 6 shows Cu-Bi/TiO prepared in example 2 of the present invention 2 A time-varying rule graph of the removal effect of the nano-electrode on nitrate nitrogen, wherein: the molar concentration ratio of Cu2+ and Bi3+ is 4.
Detailed Description
The embodiments of the present invention will be described in detail with reference to fig. 1 to 6, but the present invention is not limited to the claims.
Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode comprises the following steps:
step 1, pretreatment of a titanium substrate: respectively polishing a titanium plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh abrasive paper until the surface is free of scratches, washing the surface by using deionized water, sequentially putting the titanium plate into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic treatment for 10min, and finally taking out and drying the titanium plate for later use;
step 2, preparing the titanium dioxide nano electrode: taking a graphite electrode as a cathode, a pretreated titanium sheet as an anode, ammonium fluoride with the mass fraction of 0.28% and ethylene glycol solution with the mass fraction of 9.0% as electrolyte, anodizing for 3 hours at room temperature under the condition of constant voltage of 25V, washing the surface of the electrode after the reaction is finished, naturally airing, putting the electrode into a muffle furnace, calcining for 2 hours at 500 ℃, and naturally cooling; the titanium sheet and the graphite electrode have the same area;
step 3, preparing the electrodeposition solution: (1) Preparing copper electrodeposition liquid, adding water into 0.01mol/L copper sulfate serving as a main salt and 0.01mol/L disodium ethylene diamine tetraacetate serving as a complexing agent, and fully stirring until the copper electrodeposition liquid is completely dissolved to obtain copper-containing electrodeposition liquid; preparing an electrodeposition solution of bismuth: taking 0.01mol/L bismuth nitrate pentahydrate as a main salt, taking 0.01mol/L disodium ethylene diamine tetraacetate as a complexing agent, taking 1g/L potassium chloride as an electrolyte, adding water, and fully stirring until the bismuth nitrate, the disodium ethylene diamine tetraacetate and the potassium chloride are dissolved to obtain an electrodeposition solution containing bismuth; (3) preparing mixed electrodeposition liquid: mixing copper-containing electrodeposition liquid and bismuth-containing electrodeposition liquid to obtain mixed electrodeposition liquid; the molar concentration ratio of copper ions to bismuth ions in the mixed deposition solution is 1-4;
step 4, electrodeposition: electroplating at room temperature with the titanium dioxide nano electrode as cathode and graphite electrode with equal area as anode at current density of 2mA/cm2 for 20s to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
The scanning electron microscope image of the nano electrode is shown in figure 1, the GIA nano electrode has a porous structure and a large specific surface area; the energy level analysis images of the nano-electrode are shown in fig. 2, fig. 3 and fig. 4, and it can be clearly seen that copper and bismuth are uniformly distributed on the titanium dioxide nano-electrode, and the nano-electrode has the characteristic of large specific surface area.
Example 1
Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode comprises the following steps:
step 1, pretreatment of a titanium substrate: respectively polishing a titanium plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh abrasive paper until the surface is free of scratches, washing the surface by using deionized water, sequentially putting the titanium plate into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic treatment for 10min, and finally taking out and drying the titanium plate for later use;
step 2, preparing the titanium dioxide nano electrode: taking a graphite electrode as a cathode, taking a pretreated titanium sheet as an anode, taking ammonium fluoride with the mass fraction of 0.28% and ethylene glycol solution with the mass fraction of 9.0% as electrolyte, carrying out anodic oxidation for 3 hours at room temperature under the condition of constant voltage of 25V, washing the surface of the electrode after the reaction is finished, naturally airing, putting the electrode into a muffle furnace, calcining for 2 hours at 500 ℃, and naturally cooling; the titanium sheet and the graphite electrode have the same area;
step 3, preparing the electrodeposition solution: (1) Preparing copper electrodeposition liquid, taking 0.01mol/L copper sulfate as main salt and 0.01mol/L disodium ethylene diamine tetraacetate as complexing agent, adding water, and fully stirring until the copper-containing electrodeposition liquid is completely dissolved to obtain copper-containing electrodeposition liquid; preparing an electrodeposition solution of bismuth: taking 0.01mol/L bismuth nitrate pentahydrate as a main salt, taking 0.01mol/L disodium ethylene diamine tetraacetate as a complexing agent, taking 1g/L potassium chloride as an electrolyte, adding water, and fully stirring until the bismuth nitrate pentahydrate and the disodium ethylene diamine tetraacetate are dissolved to obtain an electro-deposition solution containing bismuth; (3) preparing mixed electrodeposition liquid: mixing copper-containing electrodeposition liquid and bismuth-containing electrodeposition liquid to obtain mixed electrodeposition liquid; the molar concentration ratio of copper ions to bismuth ions in the mixed deposition solution is 1;
step 4, electrodeposition: electroplating at room temperature with the titanium dioxide nano electrode as cathode and graphite electrode with equal area as anode at current density of 2mA/cm2 for 20s to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
Example 2
Cu-Bi/TiO 2 The preparation method of the nano electro-catalytic denitrification electrode comprises the following steps:
step 1, pretreatment of a titanium substrate: polishing a titanium plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh abrasive paper respectively until the surface is free from scratches, washing the surface by using deionized water, then sequentially putting the titanium plate into acetone, absolute ethyl alcohol and deionized water for ultrasonic treatment for 10min, finally taking out the titanium plate, and drying the titanium plate for later use;
step 2, preparing the titanium dioxide nano electrode: taking a graphite electrode as a cathode, taking a pretreated titanium sheet as an anode, taking ammonium fluoride with the mass fraction of 0.28% and ethylene glycol solution with the mass fraction of 9.0% as electrolyte, carrying out anodic oxidation for 3 hours at room temperature under the condition of constant voltage of 25V, washing the surface of the electrode after the reaction is finished, naturally airing, putting the electrode into a muffle furnace, calcining for 2 hours at 500 ℃, and naturally cooling; the titanium sheet and the graphite electrode have the same area;
step 3, preparing the electrodeposition solution: (1) Preparing copper electrodeposition liquid, adding water into 0.01mol/L copper sulfate serving as a main salt and 0.01mol/L disodium ethylene diamine tetraacetate serving as a complexing agent, and fully stirring until the copper electrodeposition liquid is completely dissolved to obtain copper-containing electrodeposition liquid; preparing an electrodeposition solution of bismuth: taking 0.01mol/L bismuth nitrate pentahydrate as a main salt, taking 0.01mol/L disodium ethylene diamine tetraacetate as a complexing agent, taking 1g/L potassium chloride as an electrolyte, adding water, and fully stirring until the bismuth nitrate pentahydrate and the disodium ethylene diamine tetraacetate are dissolved to obtain an electro-deposition solution containing bismuth; (3) preparing mixed electrodeposition liquid: mixing copper-containing electrodeposition liquid and bismuth-containing electrodeposition liquid to obtain mixed electrodeposition liquid; the molar concentration ratio of copper ions to bismuth ions in the mixed deposition solution is 4;
step 4, electrodeposition: electroplating at room temperature with the titanium dioxide nano electrode as cathode and graphite electrode with equal area as anode at current density of 2mA/cm2 for 20s to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
Test experiment
Cu-Bi/TiO prepared in example 1 2 Nano-electrode electrocatalytic reduction simulation wastewater
Reduction conditions are as follows: 490mL of simulated wastewater, 0.5g/L of sodium sulfate as electrolyte, 20mA/cm2 of current density, 3cm of distance, 40cm2 of electrode effective area, 100mg/L of initial concentration of nitrate nitrogen for electrocatalytic reduction for 2h, removal effect of nitrate nitrogen and timeThe relationship is shown in FIG. 5, cu-Bi/TiO prepared in example 1 2 The nano electrode has high catalytic efficiency, and the removal rate of nitrate nitrogen is 75% after 2h of electrocatalysis.
Cu-Bi/TiO prepared in example 2 2 Nano-electrode electrocatalytic reduction simulation wastewater
Reduction conditions are as follows: 490mL of simulated wastewater, 0.5g/L of sodium sulfate as electrolyte, 20mA/cm2 of current density, 3cm of spacing, 40cm2 of effective electrode area, 100mg/L of initial nitrate nitrogen concentration for 2h of electrocatalytic reduction, the relationship between the nitrate nitrogen removal effect and time is shown in FIG. 6, the Cu-Bi/TiO prepared in example 2 2 The nano electrode has high catalytic efficiency, and the removal rate of nitrate nitrogen is 82% after 2h of electrocatalysis.
The invention utilizes an electrodeposition method to prepare Cu-Bi/TiO 2 The nano electrode is applied to reduction of nitrate nitrogen in water, and compared with the traditional electrode, the prepared nano electrode has the advantages of good corrosion resistance, high stability and high reaction efficiency.
It should be understood that the detailed description of the invention is only for illustrating the invention and is not limited to the technical solutions described in the embodiments of the invention. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (7)
1. Cu-Bi/TiO 2 The preparation method of the nano electrocatalytic denitrification electrode is characterized by comprising the following steps: the method comprises the step of carrying out electrodeposition treatment on copper-bismuth metal on the surface of a titanium dioxide nano electrode to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
2. The Cu-Bi/TiO of claim 1 2 The preparation method of the nano electro-catalytic denitrification electrode is characterized by comprising the following steps: preparing the titanium dioxide nano electrode: taking a graphite electrode as a cathode, a pretreated titanium sheet as an anode, 0.28 mass percent of ammonium fluoride and 9.0 mass percent of ethylene glycol solution as electrolysisAnodizing the solution for 3 hours at room temperature under the condition of constant voltage of 25V, washing the surface of the electrode after the reaction is finished, naturally drying the electrode, calcining the electrode for 2 hours at 500 ℃ in a muffle furnace, and naturally cooling the electrode; the titanium sheet and the graphite electrode have the same area.
3. The Cu-Bi/TiO of claim 2 2 The preparation method of the nano electro-catalytic denitrification electrode is characterized by comprising the following steps: the specific steps of the pretreated titanium sheet comprise: polishing a titanium plate with the purity of 99.9% and the thickness of 0.2mm by using 300-mesh and 600-mesh abrasive paper respectively until the surface is free from scratches, washing the surface by using deionized water, then sequentially putting the titanium plate into acetone, absolute ethyl alcohol and deionized water for ultrasonic treatment for 10min, finally taking out the titanium plate, and drying the titanium plate for later use.
4. The Cu-Bi/TiO of claim 1 2 The preparation method of the nano electrocatalytic denitrification electrode is characterized by comprising the following steps: the electrodeposition process includes: soaking a titanium dioxide nano electrode serving as a cathode and a graphite electrode with the same area serving as an anode into the copper-bismuth mixed electrodeposition liquid at room temperature for electroplating, wherein the current density is 2mA/cm & lt 2 & gt, and the electrodeposition time is 20s to obtain Cu-Bi/TiO 2 And (4) a nano electrode.
5. The Cu-Bi/TiO of claim 4 2 The preparation method of the nano electro-catalytic denitrification electrode is characterized by comprising the following steps: the molar concentration ratio of copper ions to bismuth ions in the copper-bismuth mixed electrodeposition liquid is 1-4.
6. The Cu-Bi/TiO of claim 4 2 The preparation method of the nano electrocatalytic denitrification electrode is characterized by comprising the following steps: the preparation method of the copper-bismuth mixed electrodeposition solution comprises the following steps: (1) Preparing copper electrodeposition liquid, adding water into 0.01mol/L copper sulfate serving as a main salt and 0.01mol/L disodium ethylene diamine tetraacetate serving as a complexing agent, and fully stirring until the copper electrodeposition liquid is completely dissolved to obtain copper-containing electrodeposition liquid; preparing an electrodeposition solution of bismuth: 0.01mol/L bismuth nitrate pentahydrate is taken as main salt, 0.01mol/L disodium ethylene diamine tetraacetate is taken as complexing agent, and 1g/L potassium chloride is taken as complexing agentAdding water into the electrolyte, and fully stirring until the electrolyte is dissolved to obtain electrodeposition liquid containing bismuth; preparing a mixed electrodeposition liquid: and mixing the copper-containing electrodeposition liquid and the bismuth-containing electrodeposition liquid to obtain mixed electrodeposition liquid.
7. The Cu-Bi/TiO of claim 1 2 The preparation method of the nano electro-catalytic denitrification electrode is characterized by comprising the following steps: the Cu-Bi/TiO 2 The nano electrode is used for removing nitrate nitrogen in water through electrocatalytic reduction.
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