CN115072845A - Nano porous carbon modified graphite felt cathode material and preparation method and application thereof - Google Patents
Nano porous carbon modified graphite felt cathode material and preparation method and application thereof Download PDFInfo
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- CN115072845A CN115072845A CN202210540308.XA CN202210540308A CN115072845A CN 115072845 A CN115072845 A CN 115072845A CN 202210540308 A CN202210540308 A CN 202210540308A CN 115072845 A CN115072845 A CN 115072845A
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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
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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
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention relates to a nano porous carbon modified graphite felt cathode material and a preparation method and application thereof, wherein the preparation method comprises the following steps: adding a carboxylated multi-walled carbon nanotube into deionized water to form a suspension; adding the suspension and Zn (NO) into methanol 3 ) 2 ·6H 2 Reacting O with 2-methylimidazole to obtain ZIF-8@ MWCNTs; drying ZIF-8@ MWCNTs in vacuum, calcining, soaking in hydrochloric acid, centrifugally washing to be neutral, and drying in vacuum to obtain nano porous carbon; mixing nano porous carbon, isopropanol, polytetrafluoroethylene emulsion and deionized water, performing ultrasonic treatment, immersing a graphite felt, and performing ultrasonic treatment to obtain a primarily modified cathode material; will be provided withAnd drying the preliminarily modified cathode material, annealing, and cooling to room temperature to obtain the nano porous carbon modified graphite felt cathode material. The cathode material can be applied to an electro-Fenton system or organic pollutant removal, and compared with the prior art, the cathode material has important significance for perfecting and optimizing the electro-Fenton system and applying and popularizing the cathode material in organic wastewater treatment.
Description
Technical Field
The invention relates to the technical field of electrocatalysis electrode materials, in particular to a nano porous carbon modified graphite felt cathode material and a preparation method and application thereof.
Background
electro-Fenton as a novel water treatment process has been shown to be effective in fading and degrading azo dyes in water and is mainly characterized by the ability to generate H in situ at the cathode 2 O 2 Further, hydroxyl radicals OH, which are second to fluorine in oxidizing property, are generated, and pollutants are degraded into water and carbon dioxide. Compared with other EF cathode materials, graphite felt has the advantages of relatively good mechanical strength and electrocatalytic activity, easy manufacture, low price and the like, and is a typical three-dimensional carbon-based material. The cathode material is H in an electro-Fenton system 2 O 2 The key factor in yield. H of graphite felt cathode material 2 O 2 The yield is limited by the low specific surface area and the active site.
Disclosure of Invention
The invention aims to provide a nano porous carbon modified graphite felt cathode material, a preparation method and application thereof, and the nano porous carbon modified graphite felt cathode material has higher porosity and larger specific surface area.
The purpose of the invention can be realized by the following technical scheme: a preparation method of a nano porous carbon modified graphite felt cathode material comprises the following steps:
step 1, adding a carboxylated multi-walled carbon nanotube into deionized water, and performing ultrasonic treatment to form a suspension;
Step 3, drying ZIF-8@ MWCNTs in vacuum, calcining under the protection of inert gas, then soaking in hydrochloric acid, centrifugally washing to neutrality, and drying in vacuum to obtain nanoporous carbon;
step 4, mixing nano porous carbon, isopropanol, polytetrafluoroethylene emulsion and deionized water, performing ultrasonic treatment, immersing a graphite felt, and performing ultrasonic treatment to obtain a preliminarily modified cathode material;
and 5, drying the preliminarily modified cathode material, annealing, and cooling to room temperature to obtain the nano porous carbon modified graphite felt cathode material.
Preferably, the concentration of the carboxylated multi-wall carbon nanotube suspension in the step 1 is 4-6 mg/mL, and the ultrasonic treatment is carried out for 20-30 min.
Further preferably, the concentration of the carboxylated multi-walled carbon nanotube suspension in the step 1 is 5 mg/mL.
Preferably, Zn (NO) as described in step 2 3 ) 2 ·6H 2 The molar ratio of O to 2-methylimidazole is 1: 2; 1mmol Zn (NO) 3 ) 2 ·6H 2 O is dissolved by using 12mL of methanol; the volume ratio of the carboxylated multi-wall carbon nanotube suspension to the methanol is 1: 48.
Preferably, the calcining temperature in the step 3 is 600-1000 ℃, and the calcining time is 3-5 h.
Preferably, the vacuum drying temperature in step 3 is below 80 ℃.
Preferably, the soaking time in step 3 is 24 h.
Preferably, the centrifugal washing in the step 2 and the step 3 is carried out for 10-20 min at 8000-10000 rpm.
Preferably, the mass-to-volume ratio of the nanoporous carbon, the isopropanol, the polytetrafluoroethylene emulsion and the deionized water in the step 4 is (5-30 mg): 3mL of: (0.3-0.8 mL): 7 mL.
Preferably, the mixing ultrasonic time of the nanoporous carbon, the isopropanol, the polytetrafluoroethylene emulsion and the deionized water in the step 4 is 20-30 min, the graphite felt is immersed, and the ultrasonic treatment is carried out for 30min, so as to obtain the preliminarily modified cathode material.
Preferably, in step 5, the preliminarily modified cathode material is dried at 80 ℃ or lower and then annealed.
Preferably, in the step 5, the annealing temperature is 300-400 ℃ and the time is 1-2 h.
The nano porous carbon modified graphite felt cathode material is prepared by the preparation method.
The application of the nano porous carbon modified graphite felt cathode material is to apply the nano porous carbon modified graphite felt cathode material to an electro-Fenton system or remove organic pollutants.
When the nano porous carbon modified graphite felt cathode material is applied to an electro-Fenton system, H is increased 2 O 2 The yield of (2).
When the nano porous carbon modified graphite felt cathode material is applied to removal of organic pollutants, the decolorization rate of acid red 18 is improved.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the nano porous carbon taking ZIF-8@ MWCNTs as a precursor has higher porosity and larger specific surface area than other carbon materials, and the prepared nano porous carbon modified graphite felt cathode material can improve H content when applied to an electro-Fenton system 2 O 2 The yield of (2) can improve the decolorization rate of acid red 18 when applied to the removal of organic pollutants;
2. the electrode material has the advantages of simple preparation method, large specific surface area, high electrocatalytic activity and lower cost;
3. the method is simple to operate, has wide applicability and good application prospect;
4. the invention has important significance for perfecting and optimizing the electro-Fenton system and application and popularization in organic wastewater treatment;
5. the invention is realized by adding Zn (NO) into suspension 3 ) 2 ·6H 2 The design of the addition sequence and addition amount of O and 2-methylimidazole can fully utilize the added materials and make the size of the prepared ZIF-8@ MWCNT particles more uniform.
Drawings
FIG. 1 is an electron microscope image of nanoporous carbon obtained in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of the surface of the nanoporous carbon modified graphite felt cathode material obtained in example 1 of the present invention.
FIG. 3 is a scanning electron microscope image of the surface of the graphite felt material before modification.
Fig. 4 is a flowchart and an application diagram of embodiment 1 of the present invention.
FIG. 5 shows H in the electro-Fenton system of the graphite felt material before and after modification in example 1 of the present invention 2 O 2 And (4) a yield graph.
Fig. 6 is a graph showing the recycling effect of the modified graphite felt material of example 1 of the present invention in the electro-fenton system for treating acid red 18.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments. The following examples are carried out on the premise of the technical scheme of the invention, and detailed embodiments and specific operation processes are given, but the scope of the invention is not limited to the following examples.
Example 1
Preparing carboxylated carbon nano-tubes into 5 mg.L -1 And (3) suspension. 5mg/mL according to the volume ratio of 1:48 -1 The MWCNTs suspension was mixed with 48mL of methanol, and 4mmol of Zn (NO) was added 3 ) 2 ·6H 2 O to obtain a black solution a. Simultaneously, 8mmol of 2-methylimidazole were dissolved in 48mL of methanol to form a clear solution B. Adding the solution B into the solution A at a constant speed, continuously stirring for 4h, and standing for 24 h. And (3) centrifugally washing the product with methanol for more than 3 times, and performing vacuum drying at 80 ℃ for 12 hours to obtain the ZIF8@ MWCNTs compound. At 5 ℃ for min -1 At a temperature rise rate of N 2 Carbonizing at 800 ℃ for 5h in the atmosphere, collecting the obtained black powder, soaking in 35% HCl for 24h to remove residual impurities such as Zn, washing with deionized water until the pH value is neutral, and vacuum drying at 80 ℃ for 12h to obtain the nano porous carbon.
And (3) ultrasonically treating the graphite felt (2 multiplied by 2cm) in acetone for 30min to remove grease, washing with deionized water, and drying at 60 ℃ to constant weight to obtain the original graphite felt. A certain amount of nanoporous carbon 20mg, isopropanol 3mL, deionized water 7mL and PTFE emulsion 0.3mL are mixed and subjected to ultrasonic treatment for 20min to obtain a uniformly dispersed mixture. Immersing the pretreated GF, carrying out ultrasonic treatment for 30min, drying for 24h at 60 ℃ to form a catalytic layer, and finally carrying out carbonization treatment for 1 h at 360 ℃ by using a muffle furnace to obtain the nano porous carbon modified graphite felt cathode material.
The electron microscope image of the nanoporous carbon obtained in this example is shown in fig. 1, and it can be seen that the intertwined multi-walled carbon nanotubes are combined with the zernillium salt framework-8. As shown in fig. 2, a scanning electron microscope image of the surface of the nanoporous carbon modified graphite felt cathode material is compared with a scanning electron microscope image of the graphite felt material before treatment shown in fig. 3, and as is apparent from fig. 2, porous carbon particles are tightly adhered to the surface of the graphite felt substrate material, so that the specific surface area of the carbonaceous cathode material is increased.
As shown in FIG. 4, in the electro-Fenton system of this example, Ti/RuO is used 2 -IrO 2 (2×2cm 2 ) The sheet electrode is an anode, and the cathode is graphite felt (2 multiplied by 2cm) 2 ) Flake electrode or nano porous carbon modified graphite felt (2 x 2cm) 2 ) And a sheet electrode. The electrolyte used in the experiment is 0.05 mol.L -1 Na 2 SO 4 pH of 7 and working current density of 17.5mA cm -2 The aeration rate is 0.6 L.min -1 . As shown in FIG. 5, the nanoporous carbon modified graphite felt electrode H 2 O 2 The yield is improved by about 17 times compared with the original graphite felt. The concentration of acid red 18 in the degradation experiment is 100 mg.L -1 ，Fe 2+ The concentration is 0.36 mmol.L -1 . After eight cycles, the degradation rate still reached 96.13% within 120min, as shown in fig. 6. Therefore, the NPC-GF electrode has good stability, which would be a useful characteristic in practical applications.
Example 2
Preparing carboxylated carbon nano-tubes into 5 mg.L -1 And (3) suspension. 5mg/mL according to the volume ratio of 1:48 -1 The MWCNTs suspension was mixed with 48mL of methanol, and 4mmol of Zn (NO) was added 3 ) 2 ·6H 2 O to obtain a black solution a. Simultaneously, 8mmol of 2-methylimidazole are dissolved inClear solution B was formed in 48mL methanol. Adding the solution B into the solution A at a constant speed, continuously stirring for 4h, and standing for 24 h. And (3) centrifugally washing the product with methanol for more than 3 times, and performing vacuum drying at 80 ℃ for 12 hours to obtain the ZIF8@ MWCNTs compound. At 5 ℃ for min -1 At a temperature rise rate of N 2 Carbonizing at 1000 ℃ for 3h in the atmosphere, collecting the obtained black powder, soaking in 35% HCl for 24h to remove residual impurities such as Zn, washing with deionized water until the pH value is neutral, and vacuum drying at 80 ℃ for 12h to obtain the nano porous carbon.
And (3) ultrasonically treating a graphite felt (2 multiplied by 2cm) in acetone for 30min to remove grease, washing with deionized water, and drying at 60 ℃ to constant weight to obtain the original graphite felt. A certain amount of nanoporous carbon 5mg, isopropanol 3mL, deionized water 7mL and PTFE emulsion 0.6mL are mixed and ultrasonically treated for 20min to obtain a uniformly dispersed mixture. Immersing the pretreated GF, carrying out ultrasonic treatment for 30min, drying for 24h at 60 ℃ to form a catalytic layer, and finally carrying out carbonization treatment for 1 h at 380 ℃ by using a muffle furnace to obtain the nano porous carbon modified graphite felt cathode material.
Comparative example 1
Preparing carboxylated carbon nano-tubes into 5 mg.L -1 And (3) suspension. 5mg/mL according to the volume ratio of 1:48 -1 The MWCNTs suspension was mixed with 48mL of methanol, and 4mmol of Zn (NO) was added 3 ) 2 ·6H 2 O to obtain a black solution a. Simultaneously, 8mmol of 2-methylimidazole were dissolved in 48mL of methanol to form a clear solution B. Adding the solution B into the solution A at a constant speed, continuously stirring for 4h, and standing for 24 h. And (3) centrifugally washing the product with methanol for more than 3 times, and performing vacuum drying at 80 ℃ for 12 hours to obtain the ZIF8@ MWCNTs compound. At 5 ℃ for min -1 At a temperature rise rate of N 2 Carbonizing at 800 ℃ for 5h in the atmosphere, collecting the obtained black powder, soaking in 35% HCl for 24h to remove residual impurities such as Zn, washing with deionized water until the pH value is neutral, and vacuum drying at 80 ℃ for 12h to obtain the nano porous carbon.
And (3) ultrasonically treating the graphite felt (2 multiplied by 2cm) in acetone for 30min to remove grease, washing with deionized water, and drying at 60 ℃ to constant weight to obtain the original graphite felt. A certain amount of nanoporous carbon 20mg, isopropanol 3mL, deionized water 7mL and PTFE emulsion 0.1mL are mixed and ultrasonically treated for 20min to obtain a uniformly dispersed mixture. Immersing the pretreated GF, carrying out ultrasonic treatment for 30min, drying for 24h at 60 ℃ to form a catalytic layer, and finally carrying out carbonization treatment for 1 h at 360 ℃ by using a muffle furnace to obtain the nano porous carbon modified graphite felt cathode material.
In the electro-Fenton system, the nano porous carbon on the surface of the prepared cathode material is easy to fall off, so that the performance of the electrode is rapidly reduced.
Comparative example 2
Preparing carboxylated carbon nano-tubes into 5 mg.L -1 And (3) suspension. 5mg/mL according to the volume ratio of 1:48 -1 The MWCNTs suspension was mixed with 48mL of methanol, and 4mmol of Zn (NO) was added 3 ) 2 ·6H 2 O to obtain a black solution a. Simultaneously, 8mmol of 2-methylimidazole were dissolved in 48mL of methanol to form a clear solution B. Adding the solution B into the solution A at a constant speed, continuously stirring for 4h, and standing for 24 h. And (3) centrifugally washing the product with methanol for more than 3 times, and performing vacuum drying at 80 ℃ for 12 hours to obtain the ZIF8@ MWCNTs compound. At 5 ℃ for min -1 At a temperature rise rate of N 2 Carbonizing at 800 ℃ for 5h in the atmosphere, collecting the obtained black powder, soaking in 35% HCl for 24h to remove residual impurities such as Zn, washing with deionized water until the pH value is neutral, and vacuum drying at 80 ℃ for 12h to obtain the nano porous carbon.
And (3) ultrasonically treating a graphite felt (2 multiplied by 2cm) in acetone for 30min to remove grease, washing with deionized water, and drying at 60 ℃ to constant weight to obtain the original graphite felt. A certain amount of nanoporous carbon 20mg, isopropanol 3mL, deionized water 7mL and PTFE emulsion 1mL are mixed and subjected to ultrasonic treatment for 20min to obtain a uniformly dispersed mixture. And (3) immersing the pretreated GF, carrying out ultrasonic treatment for 30min, drying for 24h at 60 ℃ to form a catalytic layer, and finally carrying out carbonization treatment for 1 h at 360 ℃ by using a muffle furnace to obtain the nano porous carbon modified graphite felt cathode material.
A compact PTFE film is formed on the surface of the prepared cathode material, so that the conductivity of the electrode material is poor, and the electrocatalytic reaction cannot be effectively carried out.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a nano porous carbon modified graphite felt cathode material is characterized by comprising the following steps:
step 1, adding a carboxylated multi-walled carbon nanotube into deionized water, and performing ultrasonic treatment to form a suspension;
step 2, adding the suspension obtained in the step 1 and Zn (NO) into methanol 3 ) 2 ·6H 2 After the reaction between O and 2-methylimidazole, centrifugally washing a reaction product to obtain a zeolite imidazole framework-8 and a multi-walled carbon nanotube polymer ZIF-8@ MWCNTs;
step 3, drying ZIF-8@ MWCNTs in vacuum, calcining under the protection of inert gas, then soaking in hydrochloric acid, centrifugally washing to neutrality, and drying in vacuum to obtain nanoporous carbon;
step 4, mixing nano porous carbon, isopropanol, polytetrafluoroethylene emulsion and deionized water, performing ultrasonic treatment, immersing a graphite felt, and performing ultrasonic treatment to obtain a preliminarily modified cathode material;
and 5, drying the preliminarily modified cathode material, annealing, and cooling to room temperature to obtain the nano porous carbon modified graphite felt cathode material.
2. The preparation method of the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein the concentration of the carboxylated multiwalled carbon nanotube suspension in the step 1 is 4-6 mg/mL, and the ultrasound treatment is performed for 20-30 min.
3. The method for preparing the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein Zn (NO) in the step 2 3 ) 2 ·6H 2 The molar ratio of O to 2-methylimidazole is 1: 2; 1mmol Zn (NO) 3 ) 2 ·6H 2 O is dissolved by using 12mL of methanol; the volume ratio of the carboxylated multi-wall carbon nanotube suspension to the methanol is 1: 48.
4. The preparation method of the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein the calcination temperature in the step 3 is 600-1000 ℃ and the calcination time is 3-5 h.
5. The method for preparing the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein the vacuum drying temperature in the step 3 is below 80 ℃.
6. The preparation method of the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein the centrifugal washing in the steps 2 and 3 is carried out at 8000-10000 rpm for 10-20 min.
7. The preparation method of the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein the mass-to-volume ratio of the nanoporous carbon, the isopropanol, the polytetrafluoroethylene emulsion and the deionized water in the step 4 is (5-30 mg): 3mL of: (0.3-0.8 mL): 7 mL.
8. The preparation method of the nanoporous carbon modified graphite felt cathode material according to claim 1, wherein in the step 5, the annealing temperature is 300-400 ℃ and the annealing time is 1-2 h.
9. A nanoporous carbon modified graphite felt cathode material is characterized by being prepared by the preparation method of any one of claims 1-8.
10. The use of the nanoporous carbon-modified graphite felt cathode material of claim 9, wherein the nanoporous carbon-modified graphite felt cathode material is used in an electro-Fenton system or for removal of organic contaminants.
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| CN116043531A (en) * | 2023-03-06 | 2023-05-02 | 杭州德海艾科能源科技有限公司 | Modified graphite felt for high density of vanadium battery and preparation method and application thereof |
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