CN111573789A - Preparation method and application of photo-anode material - Google Patents
Preparation method and application of photo-anode material Download PDFInfo
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- CN111573789A CN111573789A CN202010472459.7A CN202010472459A CN111573789A CN 111573789 A CN111573789 A CN 111573789A CN 202010472459 A CN202010472459 A CN 202010472459A CN 111573789 A CN111573789 A CN 111573789A
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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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4618—Supplying or removing reactants or electrolyte
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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
- C02F2305/10—Photocatalysts
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Abstract
The invention particularly relates to a preparation method of a photo-anode material, which is characterized by comprising the following steps: 1) cutting the titanium plate into titanium sheets; 2) etching the titanium sheet; 3) ultrasonically removing impurities from the etched titanium sheet and drying; 4) preparation C3N4Grinding into powder for later use; 5) 1 to 5g/L of C3N4Adding Pb (NO)3)2In solution, make C3N4Present in suspension in solution; 6) adopting a double-electrode system, respectively taking two treated titanium sheets as a cathode and an anode, taking the solution prepared in the step 5) as a supporting electrolyte, and preparing PbO by adopting an electrodeposition method2/C3N4And an anode electrode. The application of the photoanode material is characterized in that PbO is added2/C3N4The anode electrode and the titanium sheet are respectively used as an anode and a cathode, and the concentration of Na is 0.1-0.2mol/L2SO4The solution is used as supporting electrolyte until the printing and dyeing wastewater is degraded to nothingThe color is transparent. The PbO2/C3N4 nanowire in the photoanode material prepared by the invention is firmly combined with the substrate, is uniformly distributed, has low cost and good effect of degrading printing and dyeing wastewater.
Description
Technical Field
The invention belongs to the field of material chemistry, and particularly relates to a preparation method and application of a photo-anode material.
Background
In the modern society, with the increasing types of printed matters and packaging products, the types and the amount of dyes are increasing day by day, and high-chroma printing and dyeing wastewater is the harmful wastewater accepted by the industry at present, wherein the harmful wastewater mainly contains organic matters which are difficult to biodegrade, such as dyes, pigments and the like, has large influence on the environment and high treatment cost, so that the degradation and decoloration treatment is needed, the pollution is reduced, and the ecological balance is protected. In order to solve the pollution problem, many materials are used as materials for degrading printing and dyeing wastewater, such as graphite, platinum, RuO2, SnO2, PbO2, and boron-doped diamond (BDD). Among them, PbO2 is attractive because of its high electrical conductivity, high overpotential for Oxygen Evolution Reaction (OER), chemical inertness, and low cost. In recent years, the skilled person has focused on modifying the catalytic activity and stability of PbO2 electrodes. For example, patent CN106222717 provides a method for preparing an iodine-containing lead dioxide electrode, which has the characteristics of low cost, high activity and long service life, and has a good removing effect on 4-chlorophenol; patent CN106868509 provides a preparation method of a graphene-modified fluorine-containing lead dioxide electrode, and the electrode prepared by the method has higher electrocatalytic activity and longer service life than a common fluorine-containing lead dioxide electrode.
Disclosure of Invention
The invention aims to provide a preparation method and application of a photoanode material, which is used for preparing an electrode of carbon nitride modified lead dioxide for treating printing and dyeing wastewater generated by manufacturing printed matters and packaging products and prepared PbO2/C3N4The nanowires are firmly combined with the matrix and are uniformly distributed, the cost is low, and the effect of degrading printing and dyeing wastewater is good.
The invention is realized by the following technical scheme:
namely, the preparation method of the photo-anode material is characterized by comprising the following steps:
1) cutting a titanium plate with the purity of 99.7% and the thickness of 0.5-2 mm into a rectangular titanium sheet with the length of 60-80 mm, the width of 5-15 mm and the thickness of 0.5-2 mm by using an aviation shear, using the rectangular titanium sheet as a matrix, and then washing with deionized water for 3-5 times;
2) etching the titanium sheet cleaned in the step 1) for 1-3 hours in an oxalic acid solution with the water bath temperature of 75-85 ℃ and the concentration of 7-15%, stirring once every 15-25 min, and then repeatedly cleaning for 3-5 times by using deionized water;
3) respectively carrying out ultrasonic treatment on the titanium sheet etched in the step 2) in an acetone solution and an ethanol solution for 15-30 min, carrying out ultrasonic treatment in deionized water for 25-40 min, taking out the titanium sheet after ultrasonic treatment, and drying the titanium sheet in a drying oven at 50-70 ℃ for 7-9 h;
4) uniformly mixing 4-6 g of urea and melamine, placing the mixture in a muffle furnace, wherein the urea content is 35% -45%, the calcination temperature is 520-600 ℃, the calcination time is 3-4 h, after the calcination is finished, cooling the mixture to room temperature, and taking out a sample, namely C3N4Grinding into powder for later use;
5) preparing 80-100 mL (1mmol/L) of Pb (NO)3)2The solution is slowly mixed with 1-5 g/L of C3N4Adding Pb (NO)3)2In solution, make C3N4Present in suspension in solution;
6) adopting a double-electrode system, respectively taking two processed titanium sheets as a cathode and an anode, taking the solution prepared in the step 5) as a supporting electrolyte, and applying 3-6 mA/cm to the electrodes through an adjustable direct current voltage-stabilizing power supply2The constant current density is 25-35 min, the deposition time is 65-70 ℃, and after the deposition is finished, the anode is washed by deionized water for 3-5 times to obtain PbO2/C3N4And an anode electrode.
Further, the substrate in step 1) of the present invention may also be a nickel foil or a zinc or tin sheet.
Further, the shape of the substrate in step 1) of the present invention may be square or triangular or circular.
Further, PbO in step 6) of the present invention2The electrodes can also be made using a pulsed current process or a thermal oxidation process or a hydrolysis process.
Further, PbO in step 6) of the present invention2/C3N4The electrodes can also be produced using a hydrothermal method or a vapor deposition method or a coating method.
Use of a photoanode material according to claim 1, wherein PbO is added2/C3N4The anode electrode and the titanium sheet are respectively used as an anode and a cathode, and the concentration of Na is 0.1-0.2mol/L2SO4The solution is used as a supporting electrolyte until the printing and dyeing wastewater is degraded to be colorless and transparent.
And after the printing and dyeing wastewater is degraded, sampling by using an ultraviolet spectrophotometer to test the degradation degree of the wastewater.
PbO in the photoanode material prepared by the invention2/C3N4The nanowires are firmly combined with the matrix and are uniformly distributed, the cost is low, and the effect of degrading printing and dyeing wastewater is good. The invention is in PbO2Introduction of C into the coating3N4Changes the appearance, surface hydrophilicity and hydrophobicity of the electrode, promotes an electrochemical active region and generates efficient hydroxyl radicals. In addition, in PbO2Introduction of C into the coating3N4Can improve PbO2The oxygen evolution capacity and the carrier density of the PbO2 are further improved, and an obvious photoelectric synergistic effect exists in the photoelectrocatalysis process, namely the PbO with surface hydrophobicity combined with photoelectrocatalysis2/C3N4The photo-anode material has good effect of degrading printing and dyeing wastewater.
Drawings
FIG. 1 is PbO2A Scanning Electron Microscope (SEM) image of the electrode;
FIG. 2 is C3N4A Scanning Electron Microscope (SEM) image of the electrode;
FIG. 3 is PbO2/C3N4Scanning electron of electrodeMicroscope (SEM) images;
FIG. 4 shows different ratios of PbO2/C3N4Degradation rate profile of the electrode.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In order to make the objects, schemes, procedures and advantages of the present invention more clear, the present invention is further described in detail with reference to the embodiments, it should be noted that the specific embodiments are only used for explaining the present invention and not for limiting the present invention. For example, PbO2The preparation process of the electrode also comprises a pulse current method, a heating oxidation method, a hydrolysis method and PbO2/C3N4The preparation process of the electrode also comprises a hydrothermal method, a vapor deposition method and a coating method.
In the following examples, unless otherwise specified, the experimental procedures used were all conventional, the titanium sheets were obtained from titanium processing factory of Baoji, and the reagents were obtained from chemical reagents of Kemiou, Tianjin.
Example 1
A preparation method of carbon nitride modified lead dioxide as a photo-anode material comprises the following steps:
s1: cutting a titanium plate (with the purity of 99.7%) with the thickness of 1mm into a rectangular titanium sheet with the size of 70mm multiplied by 10mm multiplied by 1mm by using an aviation shear, using the rectangular titanium sheet as a substrate, and then washing the rectangular titanium sheet with deionized water for 5 times;
s2: etching the titanium sheet cleaned in the step S1 for 2h under the conditions of water bath 80 ℃ and 10% oxalic acid solution, stirring once every 20min, and then repeatedly cleaning for 5 times by using deionized water;
s3: carrying out ultrasonic treatment on the titanium sheet etched in the step S2 in acetone solution, ethanol solution and deionized water for 30min, taking out the titanium sheet after ultrasonic treatment, and drying the titanium sheet in a 60 ℃ drying oven for 8 h;
s4: uniformly mixing 5g of urea and melamine, placing the mixture in a muffle furnace, wherein the urea content is 40%, the calcination temperature is 520 ℃, the calcination time is 4h, and after the calcination is finished, cooling the mixture to room temperatureTaking out the sample, namely C3N4Grinding into powder for later use;
s5: 100mL (1mmol/L) of Pb (NO) was prepared3)2Then slowly adding 1g/L of C3N4Adding Pb (NO)3)2In solution, make C3N4Present in suspension in solution;
s6: adopting a double-electrode system, respectively using two processed titanium sheets as a cathode and an anode, using the solution described in S5 as a supporting electrolyte, and applying 5mA/cm to the electrodes by an adjustable DC voltage-stabilizing power supply2Constant current density of (2). The deposition time was 30min and the temperature 65 ℃. Washing the anode with deionized water for 5 times after deposition to obtain PbO2/C3N4An anode material.
Example 2
A preparation method of carbon nitride modified lead dioxide as a photo-anode material comprises the following steps:
s1: cutting a titanium plate (with the purity of 99.7%) with the thickness of 1mm into a rectangular titanium sheet with the size of 70mm multiplied by 10mm multiplied by 1mm by using an aviation shear, using the rectangular titanium sheet as a substrate, and then washing the rectangular titanium sheet with deionized water for 5 times;
s2: etching the titanium sheet cleaned in the step S1 for 2h under the conditions of water bath 80 ℃ and 10% oxalic acid solution, stirring once every 20min, and then repeatedly cleaning for 5 times by using deionized water;
s3: carrying out ultrasonic treatment on the titanium sheet etched in the step S2 in acetone solution, ethanol solution and deionized water for 30min, taking out the titanium sheet after ultrasonic treatment, and drying the titanium sheet in a 60 ℃ drying oven for 8 h;
s4: uniformly mixing 5g of urea and melamine, placing the mixture in a muffle furnace, wherein the urea content is 40%, the calcination temperature is 520 ℃, the calcination time is 4 hours, after the calcination is finished, cooling the mixture to room temperature, and taking out a sample, namely C3N4Grinding into powder for later use;
s5: 100mL (1mmol/L) of Pb (NO) was prepared3)2Then slowly adding 5g/L of C3N4Adding Pb (NO)3)2In solution, make C3N4Present in suspension in solution;
s6: adopting a double-electrode system, respectively using two processed titanium sheets as a cathode and an anode, using the solution described in S5 as a supporting electrolyte, and applying 5mA/cm to the electrodes by an adjustable DC voltage-stabilizing power supply2Constant current density of (2). The deposition time was 30min and the temperature 65 ℃. Washing the anode with deionized water for 5 times after deposition to obtain PbO2/C3N4An anode material.
Experimental example 1
The carbon nitride modified lead dioxide prepared in example 2 was used as a photoanode material and observed by a Scanning Electron Microscope (SEM):
firstly, cutting a sample into a size of 5 multiplied by 5mm, pasting the sample on a test disc by using a conductive adhesive tape, spraying a layer of gold, putting the sample into a test groove, vacuumizing, and starting testing. The electrode surface was observed using a scanning electron microscope (Hitachi, Japan) of type Hitachi-1510.
As shown in FIG. 1, the observation result by a Scanning Electron Microscope (SEM) showed C3N4In a lamellar form, PbO2The electrodes present a massive and uneven rock structure. PbO2/C3N4The electrodes exhibit a rock-like structure similar to that of PbO2Electrode phase comparison, PbO2/C3N4Tend to be smaller and more compact and therefore have a greater specific surface area, the adsorption effect being better for the same mass.
Experimental example 2
Experiments of the carbon nitride modified lead dioxide prepared in example 1 and example 2 as the photoanode material to degrade reactive brilliant blue (KN-R):
the PEC activity of the electrodes was evaluated by removing the anthraquinone dye (reactive Brilliant blue KN-R) solution at a concentration of 60mg/L in a quartz reactor. 250mL of a solution containing 0.1mol/LNa2SO4The solution of (a) serves as a supporting electrolyte. Preparation of C3N4Modified PbO2The electrode sample and the titanium sheet were used as an anode and a cathode, respectively. The anode and cathode were placed vertically and parallel to each other at a distance of 30 mm. Before the experiment, the reaction solution was kept in blackStirring for 30min using a magnetic stirrer in the dark until an adsorption-desorption equilibrium is established between the dye and the finished electrode. Using a DC power supply (constant current density of 30mA cm)-2) PEC oxidation experiments were performed. A175W xenon lamp (used to simulate sunlight) was used for illumination, and the reaction vessel was cooled with a circulating water jacket (the xenon lamp was placed in the jacket). During the experiment, samples were withdrawn from the reactor every 20min for detection and analysis.
The results of the experiment are shown in FIG. 2. Lead dioxide-carbon nitrides-1 to-5 are each C in step S5 of example 13N4The concentration of (A) is 1g/L to 5g/L, and C can be clearly seen in the figure3N4The adsorption rate and the degradation rate are the best when the concentration of the compound is 4g/L, and the degradation rate after 2 hours of illumination can reach 84.3 percent. And it can be seen from the curves that the degradation continues with the increase of time, compared with the PbO alone2The degradation rate of the electrode 2h is much higher than 61.3%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (6)
1. A preparation method of a photo-anode material is characterized by comprising the following steps:
1) cutting a titanium plate with the purity of 99.7% and the thickness of 0.5-2 mm into a rectangular titanium sheet with the length of 60-80 mm, the width of 5-15 mm and the thickness of 0.5-2 mm by using an aviation shear, using the rectangular titanium sheet as a matrix, and then washing with deionized water for 3-5 times;
2) etching the titanium sheet cleaned in the step 1) for 1-3 hours in an oxalic acid solution with the water bath temperature of 75-85 ℃ and the concentration of 7-15%, stirring once every 15-25 min, and then repeatedly cleaning for 3-5 times by using deionized water;
3) respectively carrying out ultrasonic treatment on the titanium sheet etched in the step 2) in an acetone solution and an ethanol solution for 15-30 min, carrying out ultrasonic treatment in deionized water for 25-40 min, taking out the titanium sheet after ultrasonic treatment, and drying the titanium sheet in a drying oven at 50-70 ℃ for 7-9 h;
4) uniformly mixing 4-6 g of urea and melamine, placing the mixture in a muffle furnace, wherein the urea content is 35% -45%, the calcination temperature is 520-600 ℃, the calcination time is 3-4 h, after the calcination is finished, cooling the mixture to room temperature, and taking out a sample, namely C3N4Grinding into powder for later use;
5) preparing 80-100 mL (1mmol/L) of Pb (NO)3)2The solution is slowly mixed with 1-5 g/L of C3N4Adding Pb (NO)3)2In solution, make C3N4Present in suspension in solution;
6) adopting a double-electrode system, respectively taking two processed titanium sheets as a cathode and an anode, taking the solution prepared in the step 5) as a supporting electrolyte, and applying 3-6 mA/cm to the electrodes through an adjustable direct current voltage-stabilizing power supply2The constant current density is 25-35 min, the deposition time is 65-70 ℃, and after the deposition is finished, the anode is washed by deionized water for 3-5 times to obtain PbO2/C3N4And an anode electrode.
2. The method of claim 1, wherein the substrate in step 1) is a nickel foil or a zinc or tin sheet.
3. The method of claim 1, wherein the shape of the substrate in step 1) is square, triangular or circular.
4. A method for preparing a photoanode material as claimed in claim 1, wherein the PbO of step 6)2The electrodes can also be made using a pulsed current process or a thermal oxidation process or a hydrolysis process.
5. A method for preparing a photoanode material as claimed in claim 1, wherein the PbO of step 6)2/C3N4The electrodes can also be applied by hydrothermal or vapor depositionPrepared by a method or a coating method.
6. Use of a photoanode material according to claim 1, wherein PbO is added2/C3N4The anode electrode and the titanium sheet are respectively used as an anode and a cathode, and the concentration of Na is 0.1-0.2mol/L2SO4The solution is used as a supporting electrolyte until the printing and dyeing wastewater is degraded to be colorless and transparent.
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Citations (5)
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US20090263647A1 (en) * | 2008-03-25 | 2009-10-22 | The Curators Of The University Of Missouri | Nanocomposite dielectric coatings |
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CN110902777A (en) * | 2019-11-26 | 2020-03-24 | 大连工业大学 | Preparation method of anion-doped cobalt-based photo-anode material |
CN110898822A (en) * | 2019-11-26 | 2020-03-24 | 大连工业大学 | Preparation method of black titanium dioxide nanowire network photo-anode material |
US20200127279A1 (en) * | 2018-10-18 | 2020-04-23 | UTI Limited Parternship | Electrochemically Exfoliated Phosphated Graphene |
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Patent Citations (5)
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US20090263647A1 (en) * | 2008-03-25 | 2009-10-22 | The Curators Of The University Of Missouri | Nanocomposite dielectric coatings |
CN105668718A (en) * | 2016-04-12 | 2016-06-15 | 上海应用技术学院 | Preparation method of boron carbide/graphite co-doped lead dioxide plastic piece electrode |
US20200127279A1 (en) * | 2018-10-18 | 2020-04-23 | UTI Limited Parternship | Electrochemically Exfoliated Phosphated Graphene |
CN110902777A (en) * | 2019-11-26 | 2020-03-24 | 大连工业大学 | Preparation method of anion-doped cobalt-based photo-anode material |
CN110898822A (en) * | 2019-11-26 | 2020-03-24 | 大连工业大学 | Preparation method of black titanium dioxide nanowire network photo-anode material |
Non-Patent Citations (1)
Title |
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