CN114538578A - Silicon sphere poly-dopamine-cobalt composite derived defect-rich carbon electrode and preparation and application thereof - Google Patents
Silicon sphere poly-dopamine-cobalt composite derived defect-rich carbon electrode and preparation and application thereof Download PDFInfo
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- CN114538578A CN114538578A CN202210267051.5A CN202210267051A CN114538578A CN 114538578 A CN114538578 A CN 114538578A CN 202210267051 A CN202210267051 A CN 202210267051A CN 114538578 A CN114538578 A CN 114538578A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- 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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Abstract
The invention discloses a method for preparing a defect-rich carbon-based electrode material based on a polydopamine and cobalt nitrate compound coated with silicon spheres, and the method is applied to the field of efficient capacitive deionization and desalination. The preparation method specifically comprises the steps of firstly synthesizing polydopamine and cobalt nitrate compound coated with silicon spheres, then calcining at high temperature in an argon environment, washing to obtain a porous carbon material rich in defects, mixing the porous carbon with a conductive agent carbon black and a binder PTFE, pressing and covering on graphite paper, drying, preparing into a porous carbon electrode, and forming the symmetrical capacitance desalting device. In the process of capacitive deionization, the desalting capacity of porous carbon derived from polydopamine and cobalt nitrate mixture coated with silicon spheres is as high as 32.9mg g‑1Is 1.3-2.0 times of other comparative carbon electrodes, and the electrode adsorption is stable. The defect-rich porous carbon material prepared by the method can be used as an electrode material to greatly improve the electric adsorption capacity of a capacitance desalting device, and can be used for desalting salt waterThe field has good development prospect.
Description
Technical Field
The invention relates to preparation of an electrode material in the technical field of environmental engineering, is mainly used for a capacitive deionization desalination process, belongs to the application field of water treatment technology, and particularly belongs to the technical field of salt water desalination.
Background
China is a country with serious water shortage and faces the situation of serious shortage of fresh water resources, and more than 97 percent of water resources in the world are seawater and brackish water which cannot be directly drunk or utilized, so that the desalination of the seawater and the brackish water becomes the best means for fundamentally solving the world water crisis. In response to this situation, many desalination technologies such as reverse osmosis technology, electrodialysis technology, multi-stage flash evaporation technology, ion exchange technology, etc. have been developed worldwide. However, most conventional desalination techniques suffer from the drawback that the principle is to extract a relatively large number of water molecules out of solution, which necessarily consumes a large amount of energy. The reverse osmosis technology needs high pressure to realize water-salt separation through high driving energy, and a concentrated water chamber of the reverse osmosis technology can bring secondary pollution; the multi-stage flash technology needs to consume a large amount of heat energy to realize vaporization and separation of water; the ion exchange method requires a complicated and expensive regeneration process, and the regeneration requires strong acid and strong base, so the environment is damaged; electrodialysis techniques must use extremely large voltages to force ions to move directionally to achieve separation, which results in extremely high energy consumption and can result in water breakdown. In conclusion, the conventional desalination technology generally has the problems of high energy consumption, low efficiency, low water utilization rate, secondary pollution and the like, so that the seawater desalination is difficult to really realize large-scale industrialization. The basic principle of the Capacitive Deionization (CDI) is based on the principle of electric double layer capacitance, an external electric field is applied between a pair of parallel electrodes, one electrode is positively charged, the other electrode is negatively charged, a solution containing ions flows between the electrodes, the ions in the solution move to the electrodes with reversed charges under the action of static electricity, cations in the solution are adsorbed on the surface of a negative electrode, anions are adsorbed on the surface of a positive electrode, and the concentration of the solution is gradually reduced along with the continuous adsorption of the ions, so that the ions in the solution are removed. When the adsorption is saturated, the electrodes are reversely connected, ions adsorbed on the surfaces of the electrodes are released into the solution under the action of repulsive force and flow out along the solution to realize electrode regeneration, along with the processes of desalination and electrode regeneration, energy is stored and released, the desalination process is an energy storage process, and the electrode regeneration process is an energy release process. Because the capacitive deionization technology and the super capacitor are based on the principle of an electric double layer, the higher the electric double layer capacitance value of the electrode is, the more ions are adsorbed by the electrode, and the higher the ion removal rate is. No chemical agent is needed in the process of capacitance desalination, the strong brine discharged by regeneration comes from raw water, new emissions are not generated by the system, and the problem of secondary pollution is avoided. Therefore, compared with the traditional desalination technology, the technology not only saves troubles in transportation, storage and operation of concentrated acid and concentrated alkali, but also has low energy consumption, small investment and no secondary pollution, is an economic, effective and environment-friendly desalination technology, and has potential application prospects in various water treatment fields, such as seawater and brackish water desalination, industrial and household hard water softening, medical high-purity water and special ion removal and extraction, and the like.
The electrode material is the most important factor affecting the desalting effect of the capacitor, and must have a sufficiently large surface area and good conductivity, so the electrode material used is often a carbon material with a high specific surface area, such as activated carbon, activated carbon fiber, carbon nanotube, carbon aerogel, etc. However, no literature report exists on the defect-rich carbon-based electrode material prepared by calcining the polydopamine and cobalt nitrate compound coated with the silicon spheres. The polydopamine and cobalt nitrate compound coated with the silicon spheres has comprehensive characteristics of inorganic and organic functional materials, a novel porous carbon material can be obtained after calcination in an argon environment, and the porous carbon material has the advantages of large specific surface area and pore volume, high yield, low resistance and the like, wherein a large amount of doping and external defects can be generated in the carbon material through cobalt doped impurities introduced by cobalt nitrate. The defects can generate better conductivity and wettability, charge accumulation can be caused by charge imbalance, charge transmission is facilitated, and the electrode doped material can be used as an excellent electrode doped material. Therefore, the poly-dopamine and cobalt nitrate compound coated with the silicon spheres is calcined under argon flow at 800 ℃ to prepare the novel porous carbon electrode material, and the capacitive deionization and desalting performance of the electrode is researched.
Disclosure of Invention
The porous hollow carbon electrode material derived from the poly-dopamine and cobalt nitrate compound coated with the silicon spheres, which is provided by the invention, has the advantages of simple preparation, rich defects, high desalting capability and good cycle performance, and a preparation method and application thereof.
The invention relates to a preparation method of a defect-rich carbon electrode derived from a silicon-sphere poly-dopamine-cobalt compound, which is characterized in that graphite paper is used as a current collector and coated on a composite material of silicon-removed poly-dopamine hydrochloride and cobalt nitrate which is burnt in an argon environment to prepare a corresponding electrode;
the method comprises the following steps:
(1) dissolving 400-600mg of dopamine hydrochloride, 5-10mg of cobalt nitrate and 5-8mL of tetraethoxysilane in 160mL of solution containing ammonia water, ethanol and deionized water, and stirring for 30-40 minutes at room temperature;
(2) then, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain a compound of silicon-containing polymeric dopamine hydrochloride and cobalt nitrate;
(3) calcining the product obtained in the step (2) in a nitrogen environment to obtain a carbon-silicon compound;
(4) soaking the product obtained in the step (3) into 10-20% hydrofluoric acid solution, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain porous hollow cobalt-doped carbon spheres;
(5) and (4) mixing the product obtained in the step (4), carbon black and Polytetrafluoroethylene (PTFE) in alcohol, and coating graphite paper to obtain the electrode.
The invention comprises an electrode material prepared by the preparation method of the silicon sphere poly dopamine cobalt compound derived defect-rich carbon electrode.
The temperature for burning under the argon atmosphere in the step (3) is 750-950 ℃.
The ratio of the materials in the step (5) is 6:1:1-9:1: 1.
In the step (1), the ratio of ammonia water, ethanol and deionized water is 3:80:180-7:80: 180.
The electrode is applied to an electrode of a capacitive desalination device.
According to the invention, the poly-dopamine cobalt composite material coated with silicon spheres is calcined at high temperature in argon atmosphere to prepare the carbon material as the electrode material, and the carbon material has the characteristics of spherical appearance, rich porous configuration, structural defects, large specific surface area, high pore volume and the like, and is used as the electrode material to prepare the novel capacitive deionization electrode, so that the novel capacitive deionization electrode shows good capacitive deionization performance. Compared with the traditional activated carbon electrode, the invention has the advantages and effects that:
1. the porous carbon derived from the poly-dopamine cobalt composite material coated with the silicon spheres has the advantages of much higher mass specific capacitance compared with other comparative carbon samples, good conductivity, small hydrophilicity and small equivalent series resistance, and is beneficial to charge transmission, and the electrochemical properties can fully prove that the porous carbon material prepared by the invention has good capacitance desalting capability.
2. In the porous carbon electrode rich in defects and derived from the poly-dopamine cobalt composite material coated with silicon spheres, the desalting capacity is as high as 32.9mg g in the capacitive deionization process-11.3-2.0 times of other comparative carbon electrodes (the desalting capacity of the polydopamine-derived porous carbon electrode only coated with silicon spheres is only 25.7mg g-1(ii) a The desalting capacity of a porous carbon electrode derived from the polydopamine cobalt composite material is 16.4mg g-1) And the porous carbon electrode derived from the poly-dopamine cobalt composite material coated with the silicon spheres is stable in adsorption.
3. The preparation method is simple in preparation process, is beneficial to generating defects, adjusts the doping and type of the cobalt element and promotes the desalting performance of the capacitor.
4. The porous carbon electrode material prepared by the invention has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high desalination amount and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a porous carbon electrode derived from poly-dopamine cobalt composite material coated with silicon spheres
FIG. 2 is an elemental X-ray photoelectron spectroscopy analysis chart of porous carbon electrode derived from poly-dopamine cobalt composite material coated with silicon spheres
FIG. 3 is a cyclic voltammogram of porous carbon electrode derived from poly-dopamine cobalt composite material coated with silicon spheres
FIG. 4 is a graph of unit electro-adsorption desalination capacity of porous carbon electrode derived from poly-dopamine cobalt composite material coated with silicon spheres
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto. Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
the preparation of porous carbon electrodes derived from polydopamine material with only silicon spheres coated on the carbon electrodes was compared.
In order to facilitate comparison of products of the invention, comparative carbon electrodes are prepared and respectively used as electrodes of a capacitance desalination device, and the specific preparation method is as follows:
(1) first, 500mg of dopamine hydrochloride and 7mL of ethyl orthosilicate were dissolved in 160mL of a solution containing ammonia, ethanol and deionized water, and stirred at room temperature for thirty minutes.
(2) And then centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain the silicon-containing polymerized dopamine hydrochloride compound.
(1) And calcining the product in an argon environment to obtain the carbon-silicon composite.
(2) Soaking the materials in 10% hydrofluoric acid solution, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, washing with water for 3 times, and drying to obtain porous hollow carbon spheres.
(3) The above product was mixed with carbon black, PTFE in a ratio of 8:1:1 with alcohol.
(6) Repeatedly and uniformly compacting the uniformly stirred mixture in the step (5) on a tablet press, and then pressing and covering the mixture on the dried graphite paper;
(7) drying in an oven at 80 deg.C for 2h, naturally cooling to room temperature, taking out, and weighing respectively.
(8) Electrochemical testing of electrode materials
Cyclic Voltammetry (CV) test
And analyzing the mass specific capacitance of the prepared porous carbon electrode and the reference carbon electrode by adopting a three-electrode system, wherein the porous carbon electrode and the activated carbon electrode are working electrodes, a platinum electrode is a counter electrode, and a saturated calomel electrode is a reference electrode. The test conditions were: the electrolyte is 1.0M NaCl solution, and the scanning frequency is 0.05V s-1Scanning ofThe voltage range is-0.5V-0.5V, and the electrode sheet size is 1 multiplied by 1 cm.
Electrochemical Impedance (EIS) testing
The resistances of the prepared porous carbon electrode and a comparative carbon electrode are analyzed in a three-electrode system, wherein the porous carbon electrode and the active carbon electrode are working electrodes, a platinum electrode is a counter electrode, and a saturated calomel electrode is a reference electrode. The test conditions were: the electrolyte is 1.0M NaCl solution, the frequency range is 0.1-100000Hz, and the size of the electrode sheet is 1 multiplied by 1 cm.
(9) 500mg L under 1.2V external voltage by adopting a symmetrical deionization device structure-1In the sodium chloride solution (2), the desalting capacity was 25.7mg g-1。
Example 2:
preparation of porous carbon electrode derived from only polydopamine cobalt nitrate composite material compared with carbon electrode
(1) First, 500mg of dopamine hydrochloride and 8mg of cobalt nitrate were dissolved in 160mL of a solution containing ammonia, ethanol and deionized water, and stirred at room temperature for thirty minutes.
(2) And then centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain the polymerized dopamine hydrochloride and cobalt nitrate compound.
(4) And calcining the product in an argon environment to obtain the carbon-cobalt composite.
(4) Soaking the materials in 10% hydrofluoric acid solution, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, washing with water for 3 times, and drying to obtain porous hollow cobalt-doped carbon spheres.
(5) The above product was mixed with carbon black, PTFE in a ratio of 8:1:1 with alcohol.
(6) Repeatedly and uniformly compacting the uniformly stirred mixture in the step (5) on a tablet press, and then pressing and covering the mixture on the dried graphite paper;
(5) drying in an oven at 80 deg.C for 2h, naturally cooling to room temperature, taking out, and weighing respectively.
(8) Electrochemical testing of electrode materials
Cyclic Voltammetry (CV) test
And analyzing the mass specific capacitance of the prepared porous carbon electrode and the comparative carbon electrode by adopting a three-electrode system, wherein the porous carbon electrode and the activated carbon electrode are working electrodes, the platinum electrode is a counter electrode, and the saturated calomel electrode is a reference electrode. The test conditions were: the electrolyte is 1.0M NaCl solution, and the scanning frequency is 0.05V s-1The scanning voltage range is-0.5V-0.5V, and the size of the electrode sheet is 1 multiplied by 1 cm.
Electrochemical Impedance (EIS) testing
The resistances of the prepared porous carbon electrode and a comparative carbon electrode are analyzed in a three-electrode system, wherein the porous carbon electrode and the active carbon electrode are working electrodes, a platinum electrode is a counter electrode, and a saturated calomel electrode is a reference electrode. The test conditions were: the electrolyte is 1.0M NaCl solution, the frequency range is 0.1-100000Hz, and the size of the electrode sheet is 1 multiplied by 1 cm.
(9) Adopts a symmetrical deionization device structure, and 500mg L of the deionization device is under the external voltage of 1.2V-1In the sodium chloride solution (2), the desalting capacity was 16.4mg g-1。
Claims (6)
1. A preparation method of a silicon-ball poly dopamine cobalt compound derived defect-rich carbon electrode is characterized in that graphite paper is used as a current collector and coated on a composite material of desiliconized poly dopamine hydrochloride and cobalt nitrate which is burnt in an argon environment to prepare a corresponding electrode;
the method comprises the following steps:
(1) dissolving 400-600mg of dopamine hydrochloride, 5-10mg of cobalt nitrate and 5-8mL of tetraethoxysilane in 160mL of solution containing ammonia water, ethanol and deionized water, and stirring for 30-40 minutes at room temperature;
(2) then, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain a compound of silicon-containing polymeric dopamine hydrochloride and cobalt nitrate;
(3) calcining the product obtained in the step (2) in a nitrogen environment to obtain a carbon-silicon compound;
(4) soaking the product obtained in the step (3) into 10-20% hydrofluoric acid solution, centrifuging and washing at room temperature, washing the product with ethanol for 3 times, then washing with water for 3 times, and drying to obtain porous hollow cobalt-doped carbon spheres;
(5) and (4) mixing the product obtained in the step (4), carbon black and Polytetrafluoroethylene (PTFE) in alcohol, and coating graphite paper to obtain the electrode.
2. An electrode material prepared by the preparation method of the silicon sphere poly dopamine cobalt compound derived defect-rich carbon electrode as claimed in claim 1.
3. The method for preparing the silicon ball poly dopamine cobalt composite derived defect-rich carbon electrode as claimed in claim 1, wherein the temperature for firing under argon atmosphere in the step (3) is 750-950 ℃.
4. The method for preparing the silicon sphere poly dopamine cobalt composite derived defect-rich carbon electrode according to claim 1, wherein the ratio of the materials in the step (5) is 6:1:1-9:1: 1.
5. The method for preparing the silicon sphere poly dopamine cobalt composite derived defect-rich carbon electrode according to claim 1, wherein the ratio of ammonia water, ethanol and deionized water in the step (1) is 3:80:180-7:80: 180.
6. The method for applying the silicon sphere poly dopamine cobalt compound derived defect-rich carbon electrode according to claim 1, wherein the electrode is applied to an electrode of a capacitive desalination device.
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| CN112403501A (en) * | 2020-10-20 | 2021-02-26 | 上海大学 | Porous nitrogen-doped carbon sphere material with ultralow cobalt atom content, and preparation method and application thereof |
| JP2022013012A (en) * | 2020-07-03 | 2022-01-18 | 国立研究開発法人物質・材料研究機構 | Composite, and manufacturing method thereof, and anode electrode material using the same, and lithium ion secondary battery using the same |
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Patent Citations (8)
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| US20140118884A1 (en) * | 2012-10-30 | 2014-05-01 | Industrial Technology Research Institute | Porous carbon material and manufacturing method thereof and supercapacitor |
| CN104817144A (en) * | 2015-04-13 | 2015-08-05 | 东华大学 | Preparation method of polydopamine modified porous carbon electrode for capacitive deionization |
| CN106825553A (en) * | 2017-02-07 | 2017-06-13 | 合肥工业大学 | A kind of preparation method of cobalt nitrogen carbon nucleocapsid hybrid hollow porous carbon ball |
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