CN109205743B - Preparation method and application of carbon nanotube composite titanium oxide porous carbon material - Google Patents
Preparation method and application of carbon nanotube composite titanium oxide porous carbon material Download PDFInfo
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- CN109205743B CN109205743B CN201811301539.5A CN201811301539A CN109205743B CN 109205743 B CN109205743 B CN 109205743B CN 201811301539 A CN201811301539 A CN 201811301539A CN 109205743 B CN109205743 B CN 109205743B
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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
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a preparation method of a carbon nano tube composite titanium oxide porous carbon material, which comprises the following steps: adding N, N-dimethylformamide and methanol into a centrifuge tube, and then adding terephthalic acid or a related ligand thereof; adding carbon nanotubes after complete dissolution, adding a titanic acid precursor, carrying out heating reaction on the solution, cooling to room temperature after the reaction is finished, washing for multiple times by using a first organic solvent, and drying at 60-120 ℃ to obtain a CNT-Ti-MOF material; putting the prepared CNT-Ti-MOF into a porcelain boat, and carbonizing in a tube furnace, wherein the carbonization temperature is 400-1000 ℃, the heating rate is 2-10 ℃/min, the heat preservation is 2-5h, and the carbonization gas is N2Or Ar, cooling to room temperature to obtain the carbon nano tube composite titanium oxide porous carbon material. Compared with the traditional carbon-based electrode material, the material obtained by the method has better wettability to water and higher desalting efficiency.
Description
Technical Field
The invention relates to the technical field of capacitive deionization materials, in particular to a preparation method and application of a carbon nanotube composite titanium oxide porous carbon material.
Background
Fresh water resources are an indispensable part for human survival and development, and human life activities, social activities and industrial and agricultural development cannot be separated from fresh water. Although 70% of the earth's surface is covered by seawater, the freshwater resource available to mankind is only 0.27%. And because of the pollution of the daily life of industrial, agricultural and urban residents to natural fresh water resources, the crisis of fresh water and drinking water resources is becoming more and more serious. Therefore, how to convert seawater into fresh water that can be utilized by human beings and how to purify drinking water are problems that need to be solved urgently. The traditional desalination and purification technology comprises thermal separation and membrane separation, which have the defects of high cost, obvious energy consumption, low water yield and the like. Since the sixties of the twentieth century, the academic world began to develop a capacitive deionization technology, which is a novel water treatment technology and has the advantages of low operation energy consumption, high water utilization rate, electrode regeneration, no secondary pollution and the like. At present, active carbon, mesoporous carbon, carbon nano tubes, graphene and the like are generally adopted as electrode materials in a capacitive deionization technology, and the main problems of the materials are poor wettability of the materials to water and low desalting efficiency.
Disclosure of Invention
The invention aims to provide a preparation method and application of a carbon nanotube composite titanium oxide porous carbon material, which solves one or more of the problems in the prior art.
The invention provides a preparation method of a carbon nano tube composite titanium oxide porous carbon material, which comprises the following steps:
alpha 1, synthesis: adding N, N-Dimethylformamide (DMF) and methanol (MeOH) into a centrifuge tube according to the molar ratio of 12:1-7:1, and then adding terephthalic acid or related ligands thereof;
adding 0.01-0.2g of carbon nano tube after complete dissolution, performing ultrasonic treatment for 30-60min, then adding a titanic acid precursor, wherein the molar ratio of the titanic acid precursor to terephthalic acid or related ligands thereof is 1:8-1:1, stirring, adding the solution into a reaction kettle for heating reaction, cooling to room temperature after the reaction is finished, washing for multiple times by using a first organic solvent, and drying at 60-120 ℃ to obtain the carbon nano tube composite metal organic framework material CNT-Ti-MOF with the particle size of 0.2-5 mu m;
alpha 2, carbonization: putting the CNT-Ti-MOF prepared in the step alpha 1 into a porcelain boat, and carbonizing in a tube furnace, wherein the carbonization temperature is 400-1000 ℃, the heating rate is 2-10 ℃/min, the heat preservation is 2-5h, and the carbonization gas is N2Or Ar, cooling to room temperature to obtain the carbon nano tube composite titanium oxide porous carbon material.
Wherein, N, N-dimethylformamide is abbreviated as DMF, methanol is abbreviated as MeOH, and the carbon nanotube composite metal organic framework material is abbreviated as CNT-Ti-MOF.
In some embodiments, the salts of terephthalic acid or other related ligands can be one or more of 2-aminoterephthalic acid, 2, 5-diaminoterephthalic acid, or 2, 6-diaminoterephthalic acid.
In some embodiments, the titanic acid precursor is tetra-n-butyl titanate or tetra-isobutyl titanate.
In some embodiments, the stirring rate is 400-1000r/min and the stirring time is 10-60 min.
In some embodiments, the reaction temperature is 120-.
In some embodiments, the first organic solvent is one or more of N, N-dimethylformamide, methanol, or ethanol.
A preparation method of an electrode for capacitive deionization comprises the following steps:
mixing 10-200mg of the carbon nanotube composite titanium oxide porous carbon material with a conductive agent, adding an adhesive and a second organic solvent, stirring for 6-12h, coating the stirred material on a current collector, and drying to obtain the electrode.
In some embodiments, the conductive agent is one or more of graphite powder, carbon black, or graphene; the adhesive can be one or more of PVDF, PTFE or Nafion, and the second organic solvent is one or more of DMAC, methanol or ethanol; the current collector is one or more of graphite paper, graphite foil, carbon paper, nickel mesh or copper mesh.
The carbon nanotube composite titanium oxide porous carbon material is applied to capacitive deionization.
The application of the electrode for capacitive deionization in capacitive deionization.
The use of the electrode for capacitive deionization in capacitive deionization comprises the steps of:
the prepared electrode slice is cut into two pieces with certain size and weighed. Then the mixture is put into a self-made module, a voltage of 0.8-1.6V is applied, sodium chloride solution with the initial concentration of 40-1000mg/l is injected at the flow rate of 10-40ml/min, and data are recorded at regular intervals.
The invention has the beneficial effects that: the material prepared by the preparation method of the carbon nanotube composite titanium oxide porous carbon material provided by the embodiment of the invention has communicated pores, good hydrophilicity and excellent conductivity, can adsorb more hydrated ions, and improves the adsorption capacity. Meanwhile, the pore passages are communicated, so that the adsorption rate of the material is high. The capacitive deionization test shows that the material has better water wettability and higher desalting efficiency than the traditional carbon-based electrode material.
Drawings
FIG. 1 is an SEM image of CNT-Ti-MOF prepared in example 1;
FIG. 2 is a TEM image of CNT-Ti-MOF prepared in example 1;
FIG. 3 is a diagram of a capacitive deionization entity apparatus prepared in example 1;
FIG. 4 is a schematic view of the self-made capacitive deionization apparatus (i.e., seawater desalination module) in example 1;
fig. 5 is test data of the home-made capacitive deionization apparatus in example 1 and comparative example 1.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1
A1, measuring 30ml of N, N-Dimethylformamide (DMF) and 3.33ml of methanol (MeOH), sequentially adding into a centrifuge tube, then adding 1.67g of terephthalic acid, after completely dissolving by ultrasonic waves, adding 0.1g of carbon nano tube, after ultrasonic waves are carried out for 1h at normal temperature, adding 0.87ml of tetrabutyl titanate, adding a stirrer, stirring for 30min at the speed of 600r/min, transferring the solution into a 50ml of inner liner of a reaction kettle, filling into an iron box of the reaction kettle, and then putting into an oven at the temperature of 150 ℃ for reaction for 24 h. Cooling to room temperature, washing with DMF and methanol for three times respectively, and placing in a 110 deg.C oven overnight to obtain carbon nanotube composite metal organic framework material CNT-Ti-MOF, the morphology of which is shown in FIGS. 1 and 2.
And A2, putting the synthesized CNT-Ti-MOF material into a clean porcelain boat, heating to 600 ℃ at the speed of 5 ℃/min in a tubular furnace in the atmosphere of high-purity nitrogen gas, preserving heat for 3h, and cooling to room temperature to obtain the carbon nano tube composite titanium oxide/porous carbon material.
And A3, dissolving 0.24g of the carbonized material, 0.03g of conductive carbon black and 0.03g of emulsion in 2ml of ethanol, stirring for 8 hours, coating the solution on carbon paper according to the area of 3 x 3cm, and drying the electrode plate in an oven at 80 ℃ to obtain the electrode plate for later use.
A4, assembling of capacitive deionization device
The capacitive deionization device (i.e. the seawater desalination module) is self-made, and the structure of the capacitive deionization device is shown in figure 3.
The prepared electrode plate is put into a self-made module, 1.2V voltage is applied to the module, 50ml of 125mg/L sodium chloride solution is injected at the rate of 10ml/min, and data is recorded every 60 s.
Wherein the principle refers to the attached figure 4: after low voltage is applied to the electrodes, the salt solution enters a seawater desalination module (CDI module), cations, anions or charged particles in the solution migrate to the two electrodes under the action of electric field force and concentration gradient respectively, and are adsorbed on the surfaces of the electrodes to form a double electric layer, so that the effluent water achieves the aim of desalination or purification. When the voltage is removed, the adsorbed ions are released into the solution, thereby achieving the purpose of electrode regeneration.
Example 2
B1, weighing 30ml of N, N-Dimethylformamide (DMF) and 3.33ml of methanol (MeOH), sequentially adding into a centrifuge tube, then adding 1.81g of 2-aminoterephthalic acid, after completely dissolving by ultrasonic waves, adding 0.8g of carbon nano tube, after ultrasonic waves are carried out for 1h at normal temperature, adding 0.87ml of tetrabutyl titanate, adding a stirrer, stirring for 1h at the speed of 800r/min, transferring the solution into a 50ml of reaction kettle lining, filling into a reaction kettle iron box, and then putting into an oven at 150 ℃ for reaction for 24 h. Cooling to room temperature, washing twice with DMF and methanol respectively, and placing in an oven at 80 deg.C overnight to obtain the carbon nanotube composite metal organic framework material CNT-Ti-MOF.
And B2, putting the synthesized CNT-Ti-MOF material into a clean porcelain boat, heating to 600 ℃ at the speed of 3 ℃/min in a tube furnace in the atmosphere of high-purity nitrogen gas, preserving the heat for 2h, and cooling to room temperature to obtain the carbon nano tube composite titanium oxide/porous carbon material.
B3, 0.48g of the carbonized material, 0.06g of conductive carbon black, and 0.06g of pvdf were dissolved in DMAC, and after stirring for 10 hours, the solution was applied to carbon in an area of 4 × 4 cm. And drying the electrode slice in an oven at 80 ℃ and reserving for later use.
B4 Assembly of capacitive deionization device
The capacitance deionization device (namely the seawater desalination module) is made by self. The prepared electrode plate is put into a self-made module, 1.0V voltage is applied to the module, 60ml of 200mg/L sodium chloride solution is injected at the rate of 16ml/min, and data is recorded every 30 s.
Comparative example 1:
c1, dissolving 0.24g of activated carbon, 0.03g of conductive carbon black and 0.03g of emulsion in 2ml of ethanol, stirring for 8 hours, coating the solution on carbon paper according to the area of 3 x 3cm, and drying the electrode slice in an oven at 80 ℃ for later use;
c2, Assembly of capacitive deionization device
The capacitance deionization device (namely the seawater desalination module) is made by self. The prepared electrode sheet was tested according to the parameters shown in example 1, and data was recorded every 60 seconds.
Example 1 and comparative exampleFIG. 5 shows experimental data of the capacitive deionization apparatus prepared in 1, in which TiO is abbreviated as carbon nanotube composite titanium oxide/porous carbon material2@ C/CNT, activated carbon AC for short.
As can be seen from fig. 5: after the voltage is applied, the conductivity decreases, which indicates that the concentration of the solution decreases and salt ions are adsorbed; after the voltage is removed, the conductivity rises again, which indicates that the solution concentration rises, and the adsorbed ions are desorbed into the solution again, thereby realizing the electrode regeneration. From the graph, the adsorption capacity of the carbon nanotube composite titanium oxide porous carbon material is obviously improved for the activated carbon, and the adsorption rate is faster.
The embodiment of the invention provides a preparation method and application of a carbon nano tube composite titanium oxide porous carbon material.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these should also be construed as being within the scope of the present invention.
Claims (10)
1. A preparation method of a carbon nanotube composite titanium oxide porous carbon material is characterized by comprising the following steps:
alpha 1, synthesis: adding N, N-dimethylformamide and methanol into a centrifugal tube according to the molar ratio of 12:1-1:1, and then adding terephthalic acid or related ligands thereof;
adding 0.02-0.2g of carbon nano tube after complete dissolution, performing ultrasonic treatment for 30-60min, then adding a titanic acid precursor, wherein the molar ratio of the titanic acid precursor to terephthalic acid or other related ligands is 1:8-1:1, stirring, adding the solution into a reaction kettle for heating reaction, cooling to room temperature after the reaction is finished, washing for multiple times by using a first organic solvent, and drying at 60-120 ℃ to obtain the carbon nano tube composite metal organic framework material CNT-Ti-MOF with the particle size of 0.2-5 mu m;
alpha 2, carbonization: mixing the CNT-Ti-M prepared in the step alpha 1OF is put into a porcelain boat and carbonized in a tube furnace, wherein the carbonization temperature is 400-1000 ℃, the heating rate is 2-10 ℃/min, the temperature is kept for 2-5h, and the carbonized gas is N2Or Ar, cooling to room temperature to obtain the carbon nano tube composite titanium oxide porous carbon material.
2. The method for preparing a carbon nanotube composite titanium oxide porous carbon material according to claim 1, wherein the related ligand is one or more of p-aminobenzoic acid, 2-aminoterephthalic acid, 2, 5-diaminoterephthalic acid, or 2, 6-diaminoterephthalic acid.
3. The method for preparing a carbon nanotube composite titanium oxide porous carbon material according to claim 1, wherein the titanic acid precursor is tetra-n-butyl titanate or tetra-isobutyl titanate.
4. The method for preparing a carbon nanotube composite titanium oxide porous carbon material as claimed in claim 1, wherein the stirring speed is 400-1000r/min and the stirring time is 10-60 min.
5. The method for preparing a carbon nanotube composite titanium oxide porous carbon material as claimed in claim 1, wherein the reaction temperature is 120-180 ℃ and the reaction time is 16-48 h.
6. The method for preparing a carbon nanotube composite titanium oxide porous carbon material according to claim 1, wherein the first organic solvent is one or more of N, N-dimethylformamide, methanol or ethanol.
7. A preparation method of an electrode for capacitive deionization is characterized by comprising the following steps:
mixing 40-2000mg of the carbon nanotube composite titanium oxide porous carbon material according to any one of claims 1-6 with a conductive agent, adding an adhesive and a second organic solvent, stirring for 6-12h, coating the material obtained after stirring on a current collector, and drying to obtain an electrode.
8. The method for preparing an electrode for capacitive deionization according to claim 7, wherein the conductive agent is one or more of graphite powder, carbon black or graphene; the adhesive is one or more of PVDF, PTFE or Nafion, and the second organic solvent is one or more of DMAC, methanol or ethanol; the current collector is one or more of graphite paper, graphite foil, carbon paper, nickel mesh or copper mesh.
9. Use of a carbon nanotube composite titania porous carbon material prepared by the method of any one of claims 1 to 6 in capacitive deionization.
10. Use of an electrode for capacitive deionization prepared by the method of any one of claims 7 to 8 in capacitive deionization.
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| CN111410274B (en) * | 2020-04-17 | 2022-09-27 | 清华大学深圳国际研究生院 | Titanium-based material, preparation method thereof and application thereof in flow electrode |
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