CN110255697B - Preparation of nitrogen-doped carbon anode and application of nitrogen-doped carbon anode in catalytic wet air oxidation - Google Patents
Preparation of nitrogen-doped carbon anode and application of nitrogen-doped carbon anode in catalytic wet air oxidation Download PDFInfo
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Abstract
The invention discloses a preparation method of a nitrogen-doped carbon anode and application thereof in catalytic wet air oxidation, wherein a common three-dimensional carbon material is used as a substrate, EDTA is used as a nitrogen source, and hydrothermal nitrogen doping reaction is carried out at a certain temperature; and (3) cooling, taking out the carbon material, cleaning, drying, placing in a tubular furnace, and performing heat treatment in a nitrogen atmosphere to obtain the nitrogen-doped carbon material. Under normal temperature and normal pressure, in a single-chamber three-electrode system, the prepared nitrogen-doped carbon material is used as the anode of a battery, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and 0.05 mol.L is applied under the voltage of 1.0V‑1Na2SO4Is electrolyte, and can catalyze air to oxidize dye wastewater under a certain pH condition, so that a plurality of dyes with certain concentration can be completely removed within 2 h.
Description
Technical Field
The invention relates to preparation and application of an electrically-assisted catalytic wet air oxidation catalyst, in particular to preparation of a nitrogen-doped carbon anode and application of the nitrogen-doped carbon anode in catalytic wet air oxidation.
Background
The nitrogen atoms have similar radiuses to the carbon atoms, so that the carbon material has good compatibility with the nitrogen atoms, is easy to dope into carbon lattices, and has higher stability and durability. In addition, the generated N-C bond can enable the carbon atoms adjacent to the nitrogen atoms to have more positive charges, the enhancement of electron adsorption can create better conditions for catalytic oxidation-reduction reaction, and the characteristics also enable the nitrogen doping to be widely applied to various catalytic fields. The solvothermal or hydrothermal method has the advantages of mild conditions, easy operation, suitability for large-scale preparation and the like, and is a common method for carrying out nitrogen doping modification on carbon materials at present, wherein more nitrogen sources are reported to be ammonia water, urea, ammonium salt, hydrazine hydrate, melamine, triethanolamine and the like.
Wet air oxidation is an advanced oxidation technology that can effectively treat organic pollutants in wastewater. The technology was first proposed by U.S. f.j.zimmermann in the 50 th 20 th century, which is an oxidation process of oxidizing organic pollutants in a liquid phase into simple small molecules such as carbon dioxide, water and organic acids using air or oxygen as an oxidant under conditions of high temperature (125-. The wet air oxidation technology has stable treatment efficiency on various organic pollutants in water, does not depend on additional chemical agents and is environment-friendly. However, in order to achieve deep degradation of organic pollutants in a short time, the wet air oxidation reaction needs to be performed under high temperature and high pressure conditions, which not only puts severe requirements on equipment materials, but also consumes very high energy. The temperature and pressure of the wet air oxidation reaction can be reduced to some extent by selecting an appropriate catalyst. However, to date, they still require operating temperatures above 80 ℃ and operating pressures above 0.5MPa (Zhang et al, sci. rep.2014,4, 6797). In the case of heterogeneous catalysts, the higher the reaction temperature, the more severe the deactivation caused by sintering or metal ion leaching of the catalyst, etc. (Keav et al, cat. sci. technol.2011,1, 342-. The development of a normal-temperature normal-pressure catalytic wet air oxidation system with strong oxidation capacity, high stability and no metal ion leaching has important significance for promoting the industrial application of a wet air oxidation technology.
According to the method, a cheap and easily-obtained carbon material is selected as a substrate, a simple hydrothermal method is combined with a heat treatment process, nitrogen is doped on the surface of the carbon material, the nitrogen-doped carbon material electrode material is prepared, and organic dye wastewater is oxidized at normal temperature and normal pressure by catalyzing air under the drive of lower external voltage.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-doped carbon material anode and application of the nitrogen-doped carbon material anode in catalytic wet air oxidation. And then the nitrogen-doped carbon material is used as an anode to catalyze air to oxidize organic dye wastewater with a certain concentration, and the degradation rate reaches 100% within 2 hours.
The preparation method of the nitrogen-doped carbon anode comprises the following steps:
carrying out hydrothermal nitrogen doping reaction at a certain temperature by using a common three-dimensional carbon material as a substrate and using ethylene diamine tetraacetic acid disodium salt as a nitrogen source; and (3) cooling, taking out the carbon material, cleaning, drying, placing in a tubular furnace, and performing heat treatment in a nitrogen atmosphere to obtain the nitrogen-doped carbon material.
The three-dimensional carbon material is selected from carbon fiber, carbon felt, foam carbon or carbon cloth. Cleaning with acetone, and passing through 1% H2O2The aqueous solution is hydrothermally treated at 120 ℃ for 12 h.
The nitrogen source is ethylene diamine tetraacetic acid disodium salt, and the dosage of the nitrogen source is 2.5-12.5 times of the mass of the carbon material.
The reaction temperature of the hydrothermal nitrogen doping reaction is 120-200 ℃, and the reaction time is 8-24 h.
The heat treatment temperature is 300-900 ℃, and the heat treatment time is 1-5 h.
The application of the nitrogen-doped carbon anode prepared by the invention is that under the drive of an external voltage, the nitrogen-doped carbon is used as a catalyst to catalyze wet air oxidation reaction, and the degradation of organic dye is realized at normal temperature and normal pressure. Specifically, in a single-chamber three-electrode system, under normal temperature and normal pressure, the nitrogen-doped carbon material prepared by the method is used as the anode of a battery, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and 0.05 mol.L is carried out under the voltage of 1.0V-1Na2SO4Is electrolyte, and can catalyze air to oxidize dye wastewater under a certain pH condition, so that a plurality of dyes with certain concentration can be completely removed within 2 h.
The organic dye is one of neutral fuchsin, methylene blue, crystal violet and rhodamine B, and the concentration of the organic dye is 0-50 mg.L-1。
The pH value is 3 to 9, preferably 3 to 7.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts ethylene diamine tetraacetic acid disodium salt as a nitrogen source, and can obtain the nitrogen-doped carbon material with high nitrogen content by combining simple hydrothermal reaction with a heat treatment process.
2. The nitrogen-doped carbon material obtained by the invention has high catalytic activity on the oxidation of oxygen under the drive of normal temperature and normal pressure and lower external voltage, and can quickly degrade organic pollutants.
3. The invention adopts the non-metal modified carbon material as the anode material to be applied to the degradation of organic dye wastewater, and avoids the possibility of secondary pollution to the environment due to no leaching phenomenon of metal ions.
Drawings
Fig. 1 shows XPS total spectrum (a) and N1s high resolution XPS spectrum (b) of the nitrogen-doped carbon material prepared in example 1, and it can be seen that the nitrogen doping amount after heat treatment at 700 ℃ is 5.73%, wherein the ratio of pyrrole nitrogen to pyridine nitrogen is 85: 15;
fig. 2 shows XPS total spectrum (a) and N1s high resolution XPS spectrum (b) of the nitrogen-doped carbon material prepared in example 2, and it can be seen that the nitrogen doping amount is 10.1% after the heat treatment at 300 ℃, wherein the ratio of pyrrole nitrogen to pyridine nitrogen is 68: 32, a first step of removing the first layer;
fig. 3 shows XPS total spectrum (a) and N1s high resolution XPS spectrum (b) of the nitrogen-doped carbon material prepared in example 3, and it can be seen that the nitrogen doping amount is 3.36% after the heat treatment at 900 ℃, wherein the ratio of pyrrole nitrogen to pyridine nitrogen is 87: 13;
fig. 4 is an ultraviolet-visible spectrum of the solution of the nitrogen-doped carbon anode prepared in example 1 in the process of catalyzing air oxidation degradation of rhodamine B, and it can be seen that the characteristic absorption peak of rhodamine B completely disappears within 2 hours;
fig. 5 is a graph showing the relationship between the degradation rate and the time of the nitrogen-doped carbon anodes prepared in examples 1 to 4 in the process of catalyzing the oxidative degradation of organic pollutants in air, and it can be seen that the removal rates of several dyes within 2 hours all reach 100%.
Detailed Description
The following detailed description of the embodiments of the present invention is provided in conjunction with some technical solutions:
example 1:
adding 2.0g of disodium ethylene diamine tetraacetate into 30mL of deionized water, dissolving to form a transparent solution, transferring the transparent solution to a 50mL hydrothermal reaction kettle, immersing 0.4g of carbon felt subjected to hydrogen oxide treatment in the solution, and reacting for 14h at 160 ℃; cooling, taking out the carbon felt, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying in an oven at 80 ℃ for 12 hours; and then putting the dried carbon felt into a tubular furnace, and carrying out heat treatment for 1h at 700 ℃ under the protection of nitrogen to obtain the nitrogen-doped carbon felt material.
In a single-chamber three-electrode system, under normal temperature and pressure, the prepared nitrogen-doped carbon felt material is used as an anode, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and the concentration of the nitrogen-doped carbon felt material is 0.05 mol.L-1Na2SO4As an electrolyte, pH 7.0, 30mL · s-1The flow rate of (2) was adjusted by blowing air from the bottom of the reactor, and oxidizing 130mL of the catalytic air at an external voltage of 1.0V to a concentration of 25 mg. L-1The degradation rate of rhodamine B in 2h reaches 100 percent.
Example 2:
adding 5.0g of disodium ethylene diamine tetraacetate into 30mL of deionized water, dissolving to form a transparent solution, transferring the transparent solution to a 50mL hydrothermal reaction kettle, immersing 0.4g of carbon felt subjected to hydrogen oxide treatment in the solution, and reacting for 8 hours at 200 ℃; cooling, taking out the carbon felt, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying in an oven at 80 ℃ for 12 hours; and then putting the dried carbon felt into a tubular furnace, and carrying out heat treatment for 5 hours at 300 ℃ under the protection of nitrogen to obtain the nitrogen-doped carbon felt material.
In a single-chamber three-electrode system, under normal temperature and pressure, the prepared nitrogen-doped carbon felt material is used as an anode, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and the concentration of the nitrogen-doped carbon felt material is 0.05 mol.L-1Na2SO4As an electrolyte, pH 3.0, 30mL · s-1The flow rate of (2) was adjusted by blowing air from the bottom of the reactor, and oxidizing 130mL of the catalytic air at an external voltage of 1.0V to a concentration of 25 mg. L-1The degradation rate of rhodamine B in 2h reaches 100 percent.
Example 3:
adding 1.0g of ethylene diamine tetraacetic acid disodium salt into 30mL of deionized water, dissolving to form a transparent solution, transferring the transparent solution to a 50mL hydrothermal reaction kettle, immersing 0.4g of carbon fiber subjected to hydrogen oxide treatment in the solution, and reacting for 24h at 120 ℃; after cooling, taking out the carbon fiber, alternately washing the carbon fiber with deionized water and absolute ethyl alcohol for three times, and drying the carbon fiber in an oven at the temperature of 80 ℃ for 12 hours; and then putting the dried carbon felt into a tubular furnace, and carrying out heat treatment for 1h at 900 ℃ under the protection of nitrogen to obtain the nitrogen-doped carbon fiber material.
In a single-chamber three-electrode system, under normal temperature and pressure, the prepared nitrogen-doped carbon fiber material is used as an anode, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and the concentration of the nitrogen-doped carbon fiber material is 0.05 mol.L-1Na2SO4As an electrolyte, pH 5.0, 30mL · s-1The flow rate of (2) was adjusted by blowing air from the bottom of the reactor, and oxidizing 130mL of the catalytic air at an external voltage of 1.0V to a concentration of 25 mg. L-1The degradation rate of the crystal violet reaches 100 percent within 2 hours.
Example 4:
adding 4.0g of disodium ethylene diamine tetraacetate into 30mL of deionized water, dissolving to form a transparent solution, transferring the transparent solution to a 50mL hydrothermal reaction kettle, immersing 0.4g of carbon cloth subjected to hydrogen oxide treatment in the solution, and reacting for 16h at 140 ℃; cooling, taking out the carbon cloth, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying in an oven at 80 ℃ for 12 hours; and then putting the dried carbon cloth into a tubular furnace, and carrying out heat treatment for 2h at 700 ℃ under the protection of nitrogen to obtain the nitrogen-doped carbon cloth material.
In a single-chamber three-electrode system, under normal temperature and pressure, the prepared nitrogen-doped carbon cloth material is used as an anode, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and the concentration of the nitrogen-doped carbon cloth material is 0.05 mol.L-1Na2SO430mL · s as an electrolyte-1The flow rate of (2) was adjusted by blowing air from the bottom of the reactor, and oxidizing 130mL of the catalytic air at an external voltage of 1.0V to a concentration of 25 mg. L-1The degradation rate of the neutral fuchsin within 2h reaches 100 percent.
Example 5:
adding 3.0g of disodium ethylene diamine tetraacetate into 30mL of deionized water, dissolving to form a transparent solution, transferring the transparent solution to a 50mL hydrothermal reaction kettle, immersing 0.4g of hydrogen oxide-treated carbon foam into the solution, and reacting for 12 hours at 160 ℃; cooling, taking out the foam carbon, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying in an oven at 80 ℃ for 12 hours; and then putting the dried foamy carbon into a tubular furnace, and carrying out heat treatment for 1h at 700 ℃ under the protection of nitrogen to obtain the nitrogen-doped foamy carbon material.
In a single-chamber three-electrode system, at normal temperature and normal pressure, the prepared nitrogen-doped foamy carbon material is used as an anode, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and the concentration of the nitrogen-doped foamy carbon material is 0.05 mol.L-1Na2SO430mL · s as an electrolyte-1Blowing air from the bottom of the reactor at a flow rate of 50 mg.L in 130mL under an external voltage of 1.0V-1The degradation rate of the methylene blue within 2h reaches 100 percent.
Claims (7)
1. The application of the nitrogen-doped carbon anode is characterized in that:
under the drive of an external voltage, a nitrogen-doped carbon material is used as a catalyst to catalyze a wet air oxidation reaction, so that the degradation of organic dye is realized at normal temperature and normal pressure;
the nitrogen-doped carbon anode takes a common three-dimensional carbon material as a substrate and ethylene diamine tetraacetic acid disodium salt as a nitrogen source, and performs hydrothermal nitrogen doping reaction at a certain temperature; cooling, taking out the carbon material, cleaning, drying, placing in a tubular furnace, and performing heat treatment in a nitrogen atmosphere to obtain a nitrogen-doped carbon material;
the adding mass of the nitrogen source is 2.5-12.5 times of the mass of the carbon material;
the organic dye is one of neutral fuchsin, methylene blue, crystal violet and rhodamine B, and the concentration of the organic dye is 0-50 mg.L-1。
2. Use according to claim 1, characterized in that:
the three-dimensional carbon material is selected from carbon fiber, carbon felt, foam carbon or carbon cloth; the three-dimensional carbon material is cleaned by acetone before use and then passes through 1% H2O2The aqueous solution is hydrothermally treated at 120 ℃ for 12 h.
3. Use according to claim 1, characterized in that:
the reaction temperature of the hydrothermal nitrogen doping reaction is 120-200 ℃, and the reaction time is 8-24 h.
4. Use according to claim 1, characterized in that:
the heat treatment temperature is 300-900 ℃, and the heat treatment time is 1-5 h.
5. Use according to claim 1, characterized in that:
in a single-chamber three-electrode system, under normal temperature and normal pressure, the prepared nitrogen-doped carbon material is used as the anode of a battery, a platinum wire is used as a counter electrode, a calomel electrode is used as a reference electrode, and under the voltage of 1.0V, 0.05 mol.L-1Na2SO4Is an electrolyte and catalyzes air to oxidize dye wastewater under a certain pH condition.
6. Use according to claim 5, characterized in that:
the pH value is 3-9.
7. Use according to claim 6, characterized in that:
the pH value is 3-7.
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| CN114392747B (en) * | 2022-01-20 | 2023-11-03 | 合肥工业大学 | Preparation method and application of nickel-doped sludge substrate block electrode anode |
| CN115467159B (en) * | 2022-09-06 | 2024-04-09 | 昆明云大新能源有限公司 | In-situ etching nitrogen-doped modified carbon cloth and preparation method and application thereof |
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| CN104689857A (en) * | 2015-03-26 | 2015-06-10 | 中国科学院青岛生物能源与过程研究所 | Preparing method for nitrogen-doped porous carbon material, catalyst comprising material and application of material |
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