CN107522266B - Preparation method of hierarchical porous carbon material capacitive desalination electrode material - Google Patents
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 38
- 238000010612 desalination reaction Methods 0.000 title claims abstract description 27
- 239000007772 electrode material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 55
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000006230 acetylene black Substances 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 14
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims description 13
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 5
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 17
- 238000002156 mixing Methods 0.000 abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000011033 desalting Methods 0.000 description 21
- 238000005265 energy consumption Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- 239000013153 zeolitic imidazolate framework Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229940079865 intestinal antiinfectives imidazole derivative Drugs 0.000 description 1
- 239000013337 mesoporous metal-organic framework Substances 0.000 description 1
- 239000012924 metal-organic framework composite Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
- C02F1/46114—Electrodes in particulate form or with conductive and/or non conductive particles between them
-
- 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
-
- 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
- C02F2001/46152—Electrodes characterised by the shape or form
- C02F2001/46157—Perforated or foraminous electrodes
- C02F2001/46161—Porous electrodes
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明涉及一种分级多孔碳材料电容型脱盐电极材料的制备方法。该方法选用水为溶剂合成金属有机框架，在合成过程中引入表面活性剂为模板改变金属有机框架独有的微孔结构，得到均匀混合溶液；一定温度下洗去多余的活性组分得到分级多孔结构金属有机框架复合物。这种复合物具有与纯的金属有机框架化合物晶体相类似的几何外形，经过高温煅烧、盐酸溶液反应除去其内部金属，即可得到高含氮量的分级多孔碳材料；将复合材料、乙炔黑及聚四氟乙烯乳液混合均匀后涂覆在石墨纸上，烘干即制得电容型脱盐电极。本发明操作简单、条件易控，可大批量合成，所得的电极具有高含氮量、高比表面和良好导电性、润湿性，在电容型脱盐方面拥有潜在应用前景。The invention relates to a preparation method of a graded porous carbon material capacitive desalination electrode material. In this method, water is used as solvent to synthesize metal-organic frameworks, and surfactants are introduced as templates in the synthesis process to change the unique microporous structure of metal-organic frameworks to obtain a uniform mixed solution; wash off excess active components at a certain temperature to obtain hierarchical porous Structural metal organic framework complexes. This composite has a geometric shape similar to that of pure metal organic framework compound crystals. After high temperature calcination and hydrochloric acid solution reaction to remove its internal metal, a hierarchical porous carbon material with high nitrogen content can be obtained; the composite material, acetylene black After mixing evenly with polytetrafluoroethylene emulsion, it is coated on graphite paper and dried to obtain capacitive desalination electrode. The invention has simple operation, easy controllable conditions, and can be synthesized in large quantities. The obtained electrode has high nitrogen content, high specific surface, good conductivity and wettability, and has potential application prospects in capacitive desalination.
Description
Technical Field
The invention relates to a preparation method of a hierarchical porous carbon material capacitive desalination electrode material.
Background
With the development of human society, the existence and development of human beings are seriously affected by energy shortage and environmental pollution, wherein the water resource crisis is particularly prominent. The seawater and brackish water desalination technology has attracted extensive social attention as an important way to effectively solve the crisis. At present, the existing desalination and desalination technical methods mainly comprise a distillation method and a membrane method. However, the traditional desalination technologies have some inevitable problems, namely the cost of the selective semipermeable membrane used by the membrane method is high, the equipment investment is large, membrane parts are easy to block, and secondary pollution is easily caused; the distillation method has high requirements on heat energy, high operation temperature, large energy consumption and serious boiler scale damage and corrosion. Efforts have been made to reduce the cost and energy consumption of these conventional desalination techniques by using renewable resources such as solar, tidal and wind energy as the driving energy for the desalination system, but still not to achieve the low cost and low energy consumption requirements. Therefore, the development of new desalination technology with low cost, high efficiency, low energy consumption and environmental friendliness is urgent. Capacitive desalination is a brand new desalination technology based on the principle of double electric layers and capacitors. The method has low energy consumption and high desalting efficiency, and is environment-friendly. Can be applied to the desalination of seawater and brackish water, the softening of industrial and agricultural production and domestic water and the like, and has wide development space and application prospect.
Based on the principle of capacitive desalination, an electrode material with large specific surface area, developed gaps and good conductivity becomes the key for obtaining high capacitive desalination performance. The porous carbon material has the characteristics of high specific surface area, good conductivity, unique chemical stability, easily controlled pore structure, good conductivity and the like, and is always the first choice of the electrode material of the capacitive type desalting device. Metal-organic frameworks (MOFs) compounds have high specific surface area, large pore volume and tunable pore structure, and have recently been demonstrated to be useful as carbon precursors or templates for the preparation of porous carbon materials (Chaikitisil W, Hu M, Wang H, Huang H S, Fujita T, Wu K C W, Chen L C, Yamauchi Y, Ariga K, Nanopous carbon through direct carbon synthesis of a zeolitic adsorbent framework for supercritical electrolytes, M. Commun. 2012, 48(58): 7259) 7261). The porous carbon material has the characteristics of simple preparation method, excellent electrochemical performance and the like, and the material is endowed with unique properties of machinery, electronics, optics, semiconductors, energy storage and the like, so that the porous carbon material is widely applied to the fields of electrode materials of supercapacitors, adsorbents, hydrogen storage, catalysis and the like.
Zeolitic Imidazolate framework materials (ZIFs) are a branch of metal organic framework materials, which are three-dimensional tetrahedral Frameworks similar to zeolite structures formed from transition metal and imidazole ligands. The high thermal stability and chemical stability of ZIFs and the rich nitrogen source in the imidazole ligand make the ZIFs an ideal precursor for preparing nitrogen-doped porous carbon with excellent performance. However, it should be noted that the precursors of the currently prepared ZIF-based porous carbon materials are generally selected from organic solvents (e.g., N-dimethylformamide, methanol, etc.) which not only pollute the environment, but also are difficult to degrade. And the pore structure of the ZIF-based porous carbon material is mainly microporous, which is not beneficial to the diffusion and transmission of ions in the solution. Increasing the length of imidazole derivatives increases the cage diameter and pore size of ZIFs, but long organic ligands cause poor stability of the material framework structure, resulting in collapse of the mesoporous structure when fired. Therefore, the search for green and environmentally friendly synthetic methods, high porosity carbon materials remain challenging.
The surfactant is an effective structure directing agent of the mesoporous material, and can be effectively cooperatively assembled at an organic-inorganic interface to obtain the mesoporous material. The surfactant is used as a template and is successfully applied to the synthesis of mesoporous silica and metal oxide materials (Soler-Illia G J d A, Sanchez C, Lebeau B, Pataring J, chem. Rev. 2002, 102 (11), 4093-4138). However, to date, ordered mesoporous MOFs and their carbon materials have been reported less as capacitive desalination electrodes. In order to overcome the performance defect of a ZIF-based porous carbon material as a capacitive desalting electrode, the invention adopts a green solvent synthesis method, combines the template effect of a surfactant, and changes the pore structure of carbon by regulating and controlling the different ratios of the surfactant and a carbon precursor, so as to prepare a novel high-nitrogen-content hierarchical porous carbon capacitive desalting electrode material with high surface area, high conductivity and developed pores, thereby providing a new way for desalting with high performance, high efficiency and low energy consumption.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a preparation method of a hierarchical porous carbon material capacitive desalination electrode material.
According to the invention, green, environment-friendly and pollution-free water is selected as a solvent to synthesize a metal organic framework, a surfactant is introduced as a template in the synthesis process to change the unique microporous structure of the metal organic framework, a mesoporous and microporous composite hierarchical pore channel structure is formed to promote the diffusion and transmission of ions in a solution, and redundant active agent components are washed away at a certain temperature to obtain the hierarchical porous structure metal organic framework composite. The composite has a geometric appearance similar to that of a pure metal organic framework compound crystal, and internal metal of the composite is removed through high-temperature calcination and hydrochloric acid solution reaction, so that the high-nitrogen-content hierarchical porous carbon capacitive desalination electrode material with high surface area, high conductivity and developed pores can be obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a hierarchical porous carbon material capacitive desalination electrode material is characterized by comprising the following specific steps:
a. dissolving 2-methylimidazole in a deionized water solution to prepare a solution with the concentration of 2-4 wt%, adjusting the pH value of the solution to 9-11, and uniformly mixing to obtain a solution A;
b. dissolving zinc nitrate hexahydrate and a surfactant in deionized water according to the mass ratio of 1: 1-1: 3 to prepare a solution with the concentration of 1-2 wt% of zinc nitrate, and uniformly mixing to obtain a solution B;
c. dropwise adding the solution B obtained in the step B into the reverse solution A obtained in the step a at a stirring speed of 350-500 rpm/min, stirring for reacting for 10-24 h, and then centrifuging, washing and drying to obtain a precursor, namely the porous metal organic framework ZIF-8; the volume ratio of the solution A to the solution B is 1: 1-1: 2;
d. c, carbonizing the porous metal organic framework ZIF-8 obtained in the step c in an inert atmosphere, adding 2 mol of hydrochloric acid solution to react to remove metal oxides, and fully washing and drying to obtain a hierarchical porous carbon material;
e. d, mixing the graded porous carbon material obtained in the step d, acetylene black and polytetrafluoroethylene emulsion according to the mass ratio of 80:10: 10-90: 5:5, uniformly stirring and mixing, coating the mixture on conductive substrate graphite paper, and drying at 100-120 ℃; finally, the hierarchical porous carbon material capacitive type desalting electrode material is prepared.
The preparation method of the hierarchical porous carbon material capacitive desalination electrode material is characterized in that the surfactant is at least one of cetyl trimethyl ammonium bromide and polyethylene oxide-polypropylene oxide-polyethylene oxide.
The preparation method of the high-nitrogen-content hierarchical porous carbon material capacitive desalination electrode is characterized in that the composite material prepared by the method takes water as a solvent to synthesize a metal organic framework ZIF-8, takes a surfactant as a template to change a unique microporous structure of the metal organic framework ZIF-8, and the metal organic framework ZIF-8 is used as a carbon source and a nitrogen source to form a three-dimensional hierarchical porous structure through high-temperature calcination. The material has the characteristics of high surface area, high conductivity, developed gaps and the like, has high efficiency and low energy consumption when being applied to desalting, can be applied to desalting seawater and brackish water, and provides a new way for desalting with low energy consumption, low cost and high performance.
Detailed Description
Specific embodiments of the present invention will now be described.
Example 1
Dissolving 2-methylimidazole in a deionized water solution to prepare a solution with the concentration of 2 wt%, adjusting the pH value of the solution to 9, and uniformly mixing to obtain a solution A; dissolving zinc nitrate hexahydrate and a surfactant in deionized water according to the mass ratio of 1:1 to prepare a solution with the concentration of 1 wt% of zinc nitrate, and uniformly mixing to obtain a solution B; and dropwise adding the obtained solution B into the solution A at a stirring speed of 350rpm/min, stirring for reacting for 12 hours, centrifuging, washing for 2-3 times by using deionized water, and drying at 80 ℃ to obtain the porous metal organic framework ZIF-8.
And (3) placing the obtained porous metal organic framework ZIF-8 in a tubular furnace, controlling the heating rate to be 2 ℃/min under the protection of nitrogen with the gas flow rate of 90 mL/min, heating to 900 ℃, preserving the heat for 3 h at 900 ℃, adding 2M hydrochloric acid solution after cooling to room temperature, stirring overnight to remove metal oxides, fully washing and drying to obtain the high-nitrogen-content hierarchical porous carbon material. The obtained high-nitrogen-content hierarchical porous carbon material is uniformly mixed with acetylene black and polytetrafluoroethylene emulsion according to the mass ratio of 80:10:10, then the mixture is coated on graphite paper, and then the graphite paper is dried at 100-120 ℃. Finally, the high-nitrogen-content hierarchical porous carbon material capacitive type desalting electrode is prepared.
And testing the specific capacitance of the high-nitrogen hierarchical porous carbon material capacitive type desalting electrode. Using a CHI-660D type electrochemical workstation, wherein the electrolyte is 0.5M sodium chloride solution, the scanning speed is 5mV/s, and the voltage range is-0.5V; the specific capacitance of the electrode was measured to be greater than 100F/g. The electrode prepared above was tested for desalting performance, and the desalting efficiency was more than 80% in 100ppm of brine.
Example 2
Dissolving 2-methylimidazole in a deionized water solution to prepare a solution with the concentration of 3 wt%, adjusting the pH value of the solution to 10, and uniformly mixing to obtain a solution A; dissolving zinc nitrate hexahydrate and a surfactant in deionized water according to the mass ratio of 1:2 to prepare a solution with the concentration of 1.5 wt% of zinc nitrate, and uniformly mixing to obtain a solution B; and dropwise adding the obtained solution B into the solution A at a stirring speed of 400rpm/min, stirring for reacting for 16 hours, centrifuging, washing for 2-3 times by using deionized water, and drying at 80 ℃ to obtain the porous metal organic framework ZIF-8.
And (3) placing the obtained porous metal organic framework ZIF-8 in a tubular furnace, controlling the heating rate to be 3 ℃/min under the protection of nitrogen with the gas flow rate of 100 mL/min, heating to 800 ℃, preserving the heat for 4 h at 800 ℃, adding 2M hydrochloric acid solution after cooling to room temperature, stirring overnight to remove metal oxides, fully washing and drying to obtain the high-nitrogen-content hierarchical porous carbon material. The obtained high-nitrogen-content hierarchical porous carbon material is uniformly mixed with acetylene black and polytetrafluoroethylene emulsion according to the mass ratio of 85:10:5, then the mixture is coated on graphite paper, and then the graphite paper is dried at 100-120 ℃. Finally, the high-nitrogen-content hierarchical porous carbon material capacitive type desalting electrode is prepared.
And testing the specific capacitance of the high-nitrogen hierarchical porous carbon material capacitive type desalting electrode. Using a CHI-660D type electrochemical workstation, wherein the electrolyte is 0.5M sodium chloride solution, the scanning speed is 5mV/s, and the voltage range is-0.5V; the specific capacitance of the electrode was measured to be greater than 95F/g. The electrode prepared above was tested for desalting performance and had desalting efficiency of greater than 75% in 300ppm saline.
Example 3
Dissolving 2-methylimidazole in a deionized water solution to prepare a solution with the concentration of 3 wt%, adjusting the pH value of the solution to 11, and uniformly mixing to obtain a solution A; dissolving zinc nitrate hexahydrate and a surfactant in deionized water according to the mass ratio of 1:3 to prepare a solution with the concentration of zinc nitrate being 2 wt%, and uniformly mixing to obtain a solution B; and dropwise adding the obtained solution B into the solution A at a stirring speed of 450rpm/min, stirring for reacting for 20 hours, centrifuging, washing with deionized water for 2-3 times, and drying at 80 ℃ to obtain the porous metal organic framework ZIF-8.
And (3) placing the obtained porous metal organic framework ZIF-8 in a tubular furnace, controlling the heating rate to be 4 ℃/min under the protection of nitrogen with the gas flow rate of 130 mL/min, heating to 700 ℃, preserving the heat for 5 h at 700 ℃, adding 2M hydrochloric acid solution after cooling to room temperature, stirring overnight to remove metal oxides, fully washing and drying to obtain the high-nitrogen-content hierarchical porous carbon material. The obtained high-nitrogen-content hierarchical porous carbon material is uniformly mixed with acetylene black and polytetrafluoroethylene emulsion according to the mass ratio of 90:5:5, then the mixture is coated on graphite paper, and then the graphite paper is dried at 100-120 ℃. Finally, the high-nitrogen-content hierarchical porous carbon material capacitive type desalting electrode is prepared.
And testing the specific capacitance of the high-nitrogen hierarchical porous carbon material capacitive type desalting electrode. Using a CHI-660D type electrochemical workstation, wherein the electrolyte is 0.5M sodium chloride solution, the scanning speed is 5mV/s, and the voltage range is-0.5V; the specific capacitance of the electrode was measured to be greater than 100F/g. The electrode prepared above was tested for desalting performance, and the desalting efficiency was more than 70% in 50ppm of brine.
Claims (2)
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| CN201710166993.3A CN107522266B (en) | 2017-03-20 | 2017-03-20 | Preparation method of hierarchical porous carbon material capacitive desalination electrode material |
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