CN110668438A - Novel porous carbon electrode material for capacitive deionization technology and application thereof - Google Patents
Novel porous carbon electrode material for capacitive deionization technology and application thereof Download PDFInfo
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Abstract
The invention discloses a novel porous carbon electrode material for a capacitive deionization technology and application thereof. The prepared porous carbon material has a fixed frame, a three-level pore structure morphology and nitrogen element doping, so that the porous carbon material has a large specific surface area and good electrochemical performance, and the distance between a solution and an electrode material can be effectively shortened by adopting a flow-through electrode type mode, so that the contact resistance is reduced, and the desalting performance is improved. The method has the advantages of simple process, convenient operation, rich raw material resources, low production cost, good application prospect and good economic benefit.
Description
Technical Field
The invention relates to the technical field of capacitive deionization, in particular to a novel porous carbon electrode material for capacitive deionization technology and application thereof.
Background
Capacitive Deionization (CDI) is a novel desalination technology based on the theory of electric double layers, and the basic principle is that an electric field is applied to two ends of two parallel and opposite porous electrodes, negative and positive ions in a solution move towards the two electrodes under the action of the electric field, an electric double layer is formed at the interface of the electrodes and an electrolyte and is stored in the electrodes, and the purpose of removing charged ions in the solution is achieved. When the adsorption reaches saturation, the electrodes are short-circuited or reverse voltage is applied, and the ions return to the solution again to realize the regeneration of the electrodes. Based on the principle of CDI, its adsorption capacity depends on the total capacitance after the inner layer capacitance between the electrode and the solution and the diffusion layer capacitance are connected in series. As a new water treatment technology, the technology has attracted much attention because of its advantages of environmental friendliness, easy operation, and simple design.
In general, the electrode material should have good electrical conductivity, high specific surface area, narrow pore size distribution, and good hydrophilicity. Good conductivity facilitates electron transport, high specific surface area can provide more active sites, narrower pore size distribution and good hydrophilicity can rapidly transport electrolyte. Currently, commonly used electrode materials include activated carbon, carbon nanotubes, graphene, carbon nanofibers, mesoporous carbon, carbon aerogel and the like. For example, patent CN201610511908.8 discloses a method for preparing a capacitive deionization selective adsorption electrode, which comprises dissolving sodium polyacrylate under acidic conditions, esterifying with polyvinyl alcohol at high temperature, mixing the prepared selective material with activated carbon, carbon black and polyvinyl alcohol in a certain proportion to obtain a slurry, coating the slurry on graphite paper, and drying to obtain the capacitive deionization selective adsorption electrode. The invention patent CN201910387152.4 discloses a porous carbon electrode based on high-temperature pyrolysis of chitosan and a preparation method thereof, wherein the porous carbon electrode is prepared by firstly carbonizing chitosan, mixing with potassium hydroxide, calcining at high temperature in a nitrogen atmosphere to obtain porous carbon, uniformly mixing the porous carbon, an adhesive and a conductive agent, and pressing on a titanium mesh. The invention patent CN201910709680.7 discloses a charcoal-based capacitive electrode material, a capacitive electrode prepared by using the charcoal-based capacitive electrode material and application of the charcoal-based capacitive electrode material. The electrode material comprises biochar, conductive black and polyvinylidene fluoride, the biochar-based capacitive electrode material and an organic solvent are uniformly mixed to obtain electrode slurry, the electrode slurry is adopted to soak a current collector, and the drying is carried out to obtain the biochar-based capacitive electrode material. However, when the electrode is made of activated carbon powder or particles, the activated carbon generally needs to be bonded together by a polymer adhesive, and the polymer adhesive is often adsorbed on the surface of a part of the activated carbon, so that the electrode has high current transfer and mass transfer resistance. In addition, in a CDI electrode obtained from a powdery electrode material, CDI treatment is generally performed by a flow-through type between electrodes, and a solution is in contact with the electrode material and is electrostatically adsorbed for a certain distance, which tends to increase the resistance. Even if adjacent carbon particles are in contact with each other, the electrical contact therebetween is not very tight, resulting in a high electrical resistance. The invention patent CN201210523040.5 discloses a green nanometer carbon-based film capacitor water treatment device, which adopts a low-temperature low-pressure chemical vapor deposition device to directly grow a carbon nanotube-carbon nanofiber composite film with high specific surface area on a conductive substrate, and further uses acid and plasma for activation treatment to introduce an ion exchange film into a CDI technology. However, the carbon nano-tubes are easy to agglomerate, so that the specific surface area and the ion transmission rate of the carbon nano-tubes are reduced, and the specific surface area of the carbon nano-tubes is far smaller than that of other carbon materials, so that the capacitance deionization performance of the carbon nano-tubes is also smaller than that of other carbon materials, and the adsorption capacity of the carbon nano-tubes is lower. The invention patent CN201710194620.7 discloses a preparation method of a graphene/ferrite nano-composite electrode material, which comprises the following steps: (1) preparing a nano composite material precursor by a hydrothermal method; drying the precursor to obtain black powder, calcining, and grinding to obtain a uniform graphene/ferrite nanocomposite; (2) dispersing active carbon, carbon nano tubes, carbon black, graphene/ferrite nano composite materials and polytetrafluoroethylene in ethanol or deionized water, heating and stirring to obtain slurry in a semi-solid state, and rolling for multiple times by using a roll-to-roll machine. However, the graphene electrode has high preparation cost and a complex process. From the viewpoint of cost and practical desalting effect, conventional materials are difficult to be further applied in the CDI field, and thus research and development of new carbon materials are urgently needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a novel porous carbon electrode material for a capacitive deionization technology and application thereof, and solves the problems of large current transfer and mass transfer resistance, poor adsorption effect, high cost, complex process flow and the like of the conventional carbon material.
In order to solve the technical problems, the invention adopts the following technical scheme: a novel porous carbon electrode material for a capacitive deionization technology is characterized in that a biomass material with a frame structure is immersed in a pore-forming agent solution, washed and dried, then calcined at high temperature in an inert atmosphere to obtain porous carbon, then the porous carbon is placed in a concentrated nitric acid solution for activation, and then washed and dried to obtain the porous carbon electrode material.
Further, the biomass material having a frame structure refers to various biomaterials produced by photosynthesis using the atmosphere, water, land, or the like, such as bamboo, wood, or plant stems. Biomass is one of the most abundant renewable resources on earth, mainly composed of carbon element, oxygen element and trace elements such as nitrogen and sulfur, and structurally, biomass has a unique macro/micro pore structure.
Further, the pore-forming agent is potassium hydroxide, sodium hydroxide, potassium carbonate, potassium bicarbonate, sodium chloride, calcium carbonate or phosphoric acid, and preferably potassium bicarbonate.
Further, the immersion time was 1 ~ 3 h.
Further, the high-temperature calcination is carried out by heating to 600-800 ℃ at the speed of 10 ℃/min and preserving the heat for 2 ~ 4 h.
Furthermore, the concentration of the concentrated nitric acid is 18mol/L, and the activation time is 2 ~ 4 h.
The invention also provides application of the novel porous carbon electrode material for the capacitive deionization technology in wastewater treatment, and further, the novel porous carbon electrode material is used for removing heavy metal ions in the wastewater. The novel porous carbon electrode material for the capacitive deionization technology is applied to desalting brine.
Compared with the prior art, the invention has the following beneficial effects:
1. the novel porous carbon electrode material provided by the invention takes a biomass material with a fixed frame structure as a raw material, is prepared into a biomass-derived porous carbon material with the fixed frame structure through high-temperature calcination with the aid of a pore-forming agent solution, and is then soaked in concentrated nitric acid to enhance the wettability of the biomass-derived porous carbon material. The prepared porous carbon electrode material has a stable structure, has the structural appearances of a fixed framework and a three-level pore channel, the pore size is between several nanometers and hundreds of nanometers, and the larger micropores and the specific surface area are favorable for the storage and the transfer of ions, so that the porous carbon electrode material has better electrochemical performance and excellent desalting performance, and can be used as a CDI electrode material to be applied to water for desalting or removing heavy metal ions.
2. The biomass material adopted by the invention not only contains abundant carbon elements, but also contains trace nitrogen elements, so that the biomass-derived porous carbon material with the fixed framework structure prepared by the invention is doped with the nitrogen elements, and the electrochemical performance of the obtained carbon material is favorably improved.
3. The biomass-derived porous carbon material with the fixed frame structure provided by the invention is directly used as a CDI electrode material by utilizing the fixed frame structure, a binder is not required to be adhered to a collector plate like a powdery sample, and the CDI operation is carried out by adopting a flow-through electrode type mode, so that the distance between a solution and the electrode material can be effectively shortened, the contact resistance is further reduced, and the desalting efficiency is finally improved, thereby solving the problems of large current transfer and mass transfer resistance of a powder or granular carbon material.
4. The method takes cheap and abundant biomass as raw materials, has low production cost, is green and economic, has simple process, convenient operation and easy industrial production, is beneficial to the further research of the capacitive deionization technology, and provides a new choice and a new idea for electrode materials for CDI.
Drawings
FIG. 1 is an electron microscope image of a porous carbon electrode material prepared in example 1 of the present invention; a is a digital photograph, b is a scanning electron microscope photograph, c is a partially magnified scanning electron microscope photograph, and d is a transmission electron microscope photograph.
FIG. 2 is a microstructure analysis diagram of the porous carbon electrode material prepared in example 1 of the present invention; a is an X-ray diffraction pattern, and b is a Raman test pattern.
FIG. 3 is a characteristic diagram of the surface structure of the porous carbon electrode material prepared in example 1 of the present invention; a is a nitrogen adsorption-desorption curve chart, and b is a pore diameter distribution chart.
FIG. 4 is a graph showing the electrochemical performance of the porous carbon electrode material prepared in example 1 of the present invention; a is a cyclic voltammogram, and b is a corresponding specific capacitance diagram at a current density of 0.5A/g.
FIG. 5 is a graph showing the desalting performance of the porous carbon electrode material prepared in example 1 of the present invention as a CDI electrode material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A preparation method of a novel porous carbon electrode material for capacitive deionization technology comprises the following steps:
1) cutting bamboo chips into blocks with fixed sizes, cleaning, drying, soaking in a saturated potassium bicarbonate solution for 3 hours, drying, then placing in a tubular furnace for high-temperature calcination under the nitrogen atmosphere, wherein the heating rate is 10 ℃/min, keeping the temperature for 3 hours when the calcination temperature reaches 800 ℃, then cooling the calcined product to room temperature, washing with a hydrochloric acid solution (the hydrochloric acid solution is formed by mixing 37% by mass of concentrated hydrochloric acid and deionized water with the same volume), performing suction filtration, washing with deionized water until the solution is neutral, and drying at 60 ℃, thereby preparing the biomass-derived porous carbon material with a fixed frame structure.
2) Soaking the porous carbon material prepared in the step 1) in concentrated nitric acid for 2h, enhancing the surface wettability of the carbon material, taking out, washing with deionized water to be neutral, and drying to obtain the novel porous carbon electrode material.
1. The porous carbon electrode material prepared in this example was observed with a digital camera, a Quanta 200 FEG Field Emission Scanning Electron Microscope (FESEM), and a JEOL 2010 high-resolution Transmission Electron Microscope (TEM), and the results are shown in fig. 1.
As can be seen from figure 1, the porous carbon electrode material prepared by the method disclosed by the invention reserves the porous carbon structure of the original fixed framework of the biomass material, and the original pore structure has abundant micropores, so that a three-level pore structure is formed, the specific surface area of the carbon material is greatly increased, the pore size is from several nanometers to hundreds of nanometers, and the larger micropores and the specific surface area are favorable for storage and transmission of ions.
2. The porous carbon electrode material prepared in this example was tested by using a Philips X' Pert X-ray diffractometer and a Renishaw inVia Reflex raman spectrometer, and the results are shown in fig. 2.
As can be seen from fig. 2, after the biomass is calcined at a high temperature, the XRD peak is relatively sharp, and a more intense graphite carbon peak is exhibited in the raman spectrum, which indicates that the graphitization degree of the obtained porous carbon material is relatively high after the high-temperature calcination.
3. The porous carbon electrode material prepared in this example was tested with a Tristar3020M specific surface area and pore size distribution testing instrument, respectively, and the results are shown in fig. 3.
As can be seen from the figure, the porous carbon material of the present invention has a surface area of 1636.2 m2The nitrogen adsorption-desorption curve is a typical type IV curve, and an obvious hysteresis band exists between the pressure range of 0.2 ~ 0.9.9, which indicates that a large number of mesopores exist in a sample, the pore structure mainly comprises mesopores, and by combining scanning diagrams of fig. 1b and fig. 1c, the porous carbon also contains rich macroporous structures, which means that more penetrating mesopores can be utilized, and the application of the sample in the aspect of high-performance electrochemistry is facilitated.
4. The porous carbon material prepared by the present invention was tested using a CHI 660E electrochemical workstation, and the results are shown in FIG. 4.
As can be seen from the figure, when the sweep rate is 5 ~ 20 mV s-1When the electrochemical double layer behavior is small, the CV curve is almost rectangular, and excellent electrochemical double layer behavior is shown; as the sweep rate increases, the rectangular CV curve deforms due to the pseudocapacitance effect caused by the nitrogen doping. When the current density is 0.5A g-1The specific capacitance of the porous carbon electrode material was 330.2F g-1It is well known that high specific capacitance is very advantageous for the electrochemically related electrosorption of materialsIn (1).
5. The porous carbon electrode material prepared in this example was assembled as a CDI electrode material into a CDI unit for desalting performance test at a desalting test voltage of 1.2V, and a NaCl solution having a concentration of 50mg/L was desalted, and the results are shown in FIG. 5.
As can be seen from the graph, the desalting rate in a NaCl solution having a concentration of 50mg/L was 1.13mg/g/min and the desalting capacity was 18 mg/g.
Example 2
A preparation method of a novel porous carbon electrode material for capacitive deionization technology comprises the following steps:
1) cutting bamboo chips into blocks with fixed sizes, cleaning, drying, soaking in a saturated potassium bicarbonate solution for 3 hours, drying, then placing in a tubular furnace for high-temperature calcination under the nitrogen atmosphere, wherein the heating rate is 10 ℃/min, keeping the temperature for 3 hours when the calcination temperature reaches 700 ℃, then cooling the calcined product to room temperature, washing with a hydrochloric acid solution (the hydrochloric acid solution is formed by mixing 37% by mass of concentrated hydrochloric acid and deionized water with the same volume), performing suction filtration, washing with deionized water until the solution is neutral, and drying at 60 ℃, thereby preparing the biomass-derived porous carbon material with a fixed frame structure.
2) Soaking the porous carbon material prepared in the step 1) in concentrated nitric acid for 2h, enhancing the surface wettability of the carbon material, taking out deionized water, washing to be neutral, and drying to obtain the novel porous carbon electrode material.
Through tests, the specific surface area of the porous carbon electrode material obtained in the embodiment is 1534.2 m2The specific capacitance was 298.3F/g, the desalting rate in a NaCl solution at a concentration of 50mg/L was 1.03mg/g/min and the desalting capacitance was 16.5 mg/g.
Example 3
A preparation method of a novel porous carbon electrode material for capacitive deionization technology comprises the following steps:
1) cutting bamboo chips into blocks with fixed sizes, cleaning, drying, soaking in saturated potassium hydroxide solution for 3 hours, drying, then placing in a tubular furnace for high-temperature calcination under nitrogen atmosphere, wherein the heating rate is 10 ℃/min, keeping the temperature for 3 hours when the calcination temperature reaches 600 ℃, then cooling the calcined product to room temperature, washing with hydrochloric acid solution (the hydrochloric acid solution is formed by mixing 37% by mass of concentrated hydrochloric acid and deionized water in equal volume) for three times, performing suction filtration, washing with deionized water until the solution is neutral, and drying at 60 ℃, thereby preparing the biomass-derived porous carbon material with a fixed frame structure.
2) Soaking the porous carbon material prepared in the step 1) in concentrated nitric acid for 2h, enhancing the surface wettability of the carbon material, taking out deionized water, washing to be neutral, and drying to obtain the novel porous carbon electrode material.
Through tests, the specific surface area of the porous carbon electrode material obtained in the embodiment is 1316.3 m2The specific capacitance was 301.2F/g, the desalting rate in a NaCl solution at a concentration of 50mg/L was 1.08mg/g/min and the desalting capacitance was 17.3 mg/g.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A novel porous carbon electrode material for a capacitive deionization technology is characterized in that a biomass material with a frame structure is immersed in a pore-forming agent solution, washed and dried, then calcined at high temperature in an inert atmosphere to obtain porous carbon, then the porous carbon is placed in a concentrated nitric acid solution for activation, and washed and dried to obtain the porous carbon electrode material.
2. The novel porous carbon electrode material for capacitive deionization technology as claimed in claim 1, wherein said biomass material is bamboo, wood or plant straw.
3. The novel porous carbon electrode material for capacitive deionization technology as claimed in claim 1, wherein said pore-forming agent is potassium hydroxide, sodium hydroxide, potassium carbonate, potassium bicarbonate, sodium chloride, calcium carbonate or phosphoric acid, preferably potassium bicarbonate.
4. The novel porous carbon electrode material for capacitive deionization technology as claimed in claim 1, wherein said immersion time is 1 ~ 3 h.
5. The novel porous carbon electrode material for capacitive deionization according to claim 1, wherein the high temperature calcination is carried out at a temperature rise rate of 10 ℃/min to 600-800 ℃ for 2 ~ 4 hours.
6. The novel porous carbon electrode material for the capacitive deionization technology as claimed in claim 1, wherein the concentration of the concentrated nitric acid is 18mol/L and the activation time is 2 ~ 4 h.
7. Use of a novel porous carbon electrode material as claimed in any one of claims 1 ~ 6 for capacitive deionization techniques in the treatment of wastewater.
8. The use according to claim 7, wherein the heavy metal ions in the wastewater are removed.
9. Use of a novel porous carbon electrode material as claimed in any one of claims 1 ~ 6 for capacitive deionization techniques in desalinating brine.
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| CN111204733A (en) * | 2020-01-16 | 2020-05-29 | 兰州交通大学 | Method for preparing active porous carbon electrode through 3D printing and application thereof |
| CN112516964A (en) * | 2020-11-16 | 2021-03-19 | 湖南大学 | Nitrogen-doped biochar and preparation method and application thereof |
| CN112678821A (en) * | 2020-12-25 | 2021-04-20 | 兰州大学 | Self-supporting carbon material and preparation method and application thereof |
| CN115259307A (en) * | 2022-09-01 | 2022-11-01 | 沈阳工业大学 | Preparation method of ion exchange gel electrode for capacitive deionization technology |
| CN117976423A (en) * | 2024-03-15 | 2024-05-03 | 江苏科技大学 | Prussian blue analogue-porous carbon composite material and preparation method and application thereof |
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| CN111204733A (en) * | 2020-01-16 | 2020-05-29 | 兰州交通大学 | Method for preparing active porous carbon electrode through 3D printing and application thereof |
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| CN115259307A (en) * | 2022-09-01 | 2022-11-01 | 沈阳工业大学 | Preparation method of ion exchange gel electrode for capacitive deionization technology |
| CN115259307B (en) * | 2022-09-01 | 2023-10-31 | 沈阳工业大学 | Preparation method of ion exchange gel electrode for capacitive deionization technology |
| CN117976423A (en) * | 2024-03-15 | 2024-05-03 | 江苏科技大学 | Prussian blue analogue-porous carbon composite material and preparation method and application thereof |
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Application publication date: 20200110 |