CN104817144A - Preparation method of polydopamine modified porous carbon electrode for capacitive deionization - Google Patents
Preparation method of polydopamine modified porous carbon electrode for capacitive deionization Download PDFInfo
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Abstract
The invention relates to a preparation method of a polydopamine modified porous carbon electrode for capacitive deionization. The preparation method comprises the following steps: (1) carrying out surface polymerization by dispersing a porous carbon material in a dopamine buffer, washing, and drying to obtain a polydopamine modified porous carbon material; and (2) blending the polydopamine modified porous carbon material and a binder in water to form uniform slurry, drying to form a flocculent mixture, and rolling-in the mixture on an inert conductor so as to obtain a polydopamine modified porous carbon electrode. The prepared polydopamine modified porous carbon electrode has good hydrophily and strong mechanical stability. The technology is simple and has high cost performance. Diffusion and transmission of ions on the surface of the electrode can be effectively promoted, and double electrode layer performance can be improved. The electrode provided by the invention is suitable for assembling of a supercapacitor and can raise desalination rate and desalination amount.
Description
Technical field
The invention belongs to the preparation field of capacitive deionization electrode, particularly a kind of capacitive deionization preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL.
Background technology
Under the principle of supercapacitor desalination cell technology is based on the effect of electrostatic field, the anions and canons in solution is adsorbed on positive and negative electrode respectively, thus realizes the desalination of water.In capacitive desalination process, electrode materials is the key factor determining desalting performance.Desirable electrode materials should possess high-specific surface area, suitable pore size distribution and good electroconductibility and wetting ability.
Have specific surface area high, the carbon material that space is enriched is conventional electrode materials, but the wetting ability of porous carbon materials own is poor, limits at capacitive desalination process intermediate ion in the diffusion of electrode surface and transmission, thus reduces desalination speed and desalination amount.Therefore, the wetting ability improving porous carbon materials is a kind of method of effective raising carbon dioxide process carbon electrode desalting performance.W.Li, Z.M.Xie, Z.M.Li, Synthesis, characterization of polyacrylate-g-carbon black and its application tosoap-freewaterborne coating, J.Appl.Polym.Sci.81 (2001) 1100 – 1106. reports one and obtains wetting ability and dispersed modified carbon black preferably at carbon blacksurface graft copolymerization polyacrylic ester, but it exists reaction process complexity and uses the shortcomings such as toxic reagent.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of capacitive deionization with the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, the electrode that the present invention prepares is compared with without the modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL, the modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL of the present invention, utilize in the dopamine solution of alkalescence, the hydrophilic poly-DOPA amine layer of one deck is formed on porous carbon materials surface by the self-polymerization reaction of Dopamine HCL, improve the wetting ability of electrode, due to hydrophilic improvement, can promote that ion is in the diffusion of electrode surface and transmission, improve adsorption rate and the adsorptive capacity of electrode pair ion, the modified porous carbon dioxide process carbon electrode preparation method of poly-Dopamine HCL of the present invention is simple, and cost is low, easy industrial application.
A kind of capacitive deionization of the present invention preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, comprising:
(1) porous carbon materials is scattered in dopamine solution stirs 2-24h and be polymerized, then rinse, dry, obtain the modified porous carbon material of poly-Dopamine HCL;
(2) the modified porous carbon material of Dopamine HCL and the blended formation slurries of binding agent will be gathered, leave standstill, pump supernatant liquor, the throw out obtained is dried, obtain cloud mixture, then mixture being infiltrated also roll-in covers on inert conductor, and obtain the modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL, wherein the poly-modified porous carbon material of Dopamine HCL and the blended mass ratio of binding agent are 12-15:1.
In described step (1), porous carbon materials is one or more in gac, electrically conductive graphite, carbon fiber, carbon nanotube, carbon aerogels.
In described step (1), the solvent of dopamine solution is Tris-HCl damping fluid, pH=7-8; The concentration of dopamine solution is 0.5 ~ 2mg/L.
Stir in described step (1) as mechanical stirring under normal temperature, normal pressure, stir speed (S.S.) is 500r/min.
Rinse in described step (2) as deionized water rinsing.
Blendedly in described step (2) to be specially: the poly-modified porous carbon material of Dopamine HCL is scattered in deionized water and forms dispersion liquid, then in dispersion liquid, drip binding agent emulsion and stir 2 ~ 4h, wherein the concentration of dispersion liquid is 50 ~ 80mg/L, and the mass percentage concentration of binding agent is 6 ~ 8%.
In described step (2), binding agent is one or more in polytetrafluoroethylene PTFE, poly(vinylidene fluoride), polyethylene, polypropylene.
In described step (1), (2), bake out temperature is 60-120 DEG C, and the time is 5-16h.
The time left standstill in described step (2) is 2-5h.
Mixture infiltrates and roll-in covers and is specially in described step (2): mixture sprays treating compound infiltrate after (in the pasty state thing), then to cover under strong plane pressure action; Wherein strong plane pressure is 3-6MPa.
Described treating compound is one or more in methyl alcohol, ethanol, ice alcohol.
In described step (2), inert conductor is one or more in titanium net, graphite paper.
In described step (2), the electrode slice thickness of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL is 0.2-2mm.
Electrode of the present invention is porous carbon and poly-Dopamine HCL, and poly-Dopamine HCL is that Dopamine HCL is formed on porous carbon through self-polymerization reaction load under solution state.
beneficial effect
The modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL of the present invention, utilizes in the dopamine solution of alkalescence, forms the hydrophilic poly-DOPA amine layer of one deck, improve the wetting ability of electrode by the self-polymerization reaction of Dopamine HCL on porous carbon materials surface;
The modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL of the present invention, due to hydrophilic improvement, can promote that ion is in the diffusion of electrode surface and transmission, improve adsorption rate and the adsorptive capacity of electrode pair ion;
The modified porous carbon dioxide process carbon electrode preparation method of poly-Dopamine HCL of the present invention is simple, and cost is low, easy industrial application.
Accompanying drawing explanation
Fig. 1 is contact angle figure, and wherein (a) is the contact angle figure of pure gac (AC); B () is the contact angle figure of poly-Dopamine HCL modified activated carbon (PDA-AC);
Fig. 2: the SEM shape appearance figure of pure gac (AC) electrode;
Fig. 3: the circulation adsorption desorption curve of pure gac (AC) electrode symmetric capacitors (AC|AC);
Fig. 4: the circulation adsorption desorption curve of symmetric capacitor (AC|AC) and (PDA-AC|PDA-AC) answered by pure gac (AC) electrode and poly-Dopamine HCL modified activated carbon (PDA-AC) electrode pair;
Fig. 5: the conductivity variations curve of poly-Dopamine HCL modified activated carbon (PDA-AC) electrode symmetric capacitors (PDA-AC|PDA-AC) voltage change and correspondence in repeatedly constant current charge-discharge process;
Fig. 6: the cyclic voltammogram of pure gac (AC) electrode and poly-Dopamine HCL modified activated carbon (PDA-AC) electrode;
Fig. 7: the alternating-current impedance figure of pure gac (AC) electrode and poly-Dopamine HCL modified activated carbon (PDA-AC) electrode.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
The preparation of pure activated carbon electrodes and symmetric capacitor desalination test:
Compound concentration is 80mg/mL gac mixed serum, slow dropping PTFE emulsion (massfraction of PTFE emulsion is 60%), wherein the quality of PTFE emulsion is 12% of quality of activated carbon, after stirring 2h, leave standstill, pump supernatant liquor, dry in 100 DEG C of baking ovens and obtain cotton-shaped gac/PTFE mixture.In above-mentioned gac/PTFE cloud mixture, add a small amount of ethanol wet, roll-in in flakes and to be pressed in titanium online, obtains pure gac (AC) electrode.Fig. 2 is the SEM shape appearance figure of pure activated carbon electrodes.
Getting the pure activated carbon electrodes of two panels and be assembled into symmetric capacitor (AC|AC), is desalting soln by the NaCl solution of 500mg/L, is to carry out constant current charge-discharge test under the condition of 1.2V at target voltage.Fig. 3 is pure gac symmetric capacitor specific conductivity curve over time under constant current charge-discharge pattern.Result shows, the single circulation desalination amount of pure activated carbon electrodes is 4.5mg/g, and current efficiency is 30%.
Embodiment 2
Poly-Dopamine HCL modified active carbon electrode preparation and symmetric capacitor desalination test:
At ambient temperature, by mechanical stirring, 2g gac being dispersed in 100mL dopamine concentration is in the Tris-HCl damping fluid of 1g/L, pH=8.5, stirring reaction 4h, then uses a large amount of deionized water filtration washing and drying, obtains poly-Dopamine HCL modified activated carbon.Fig. 1 is the contact angle figure of pure gac and poly-Dopamine HCL modified activated carbon.
Compound concentration is the poly-Dopamine HCL modified activated carbon mixed serum of 80mg/mL, slow dropping 12%PTFE emulsion (PTFE emulsion massfraction 60%), wherein the quality of PTFE emulsion is 12% of poly-Dopamine HCL modified activated carbon quality, mixing and stirring.After stirring 2h, leave standstill, pump supernatant liquor, dry in 100 DEG C of baking ovens and obtain cotton-shaped gac/PTFE mixture.Take out gac/PTFE mixture, spray ethanol wet wherein and form mashed prod, roll-in in flakes and to be pressed in titanium online, obtained poly-Dopamine HCL modified active carbon electrode.Become symmetric capacitor (PDA-AC|PDA-AC) with poly-Dopamine HCL modified activated carbon (PDA-AC) electrode assembling, adopt the NaCl solution of 500mg/L to carry out constant current charge-discharge test.Fig. 4 is under constant current charge-discharge circulation pattern, AC|AC and PDA-AC|PDA-AC symmetric capacitor specific conductivity curve over time.Result shows, the desalination amount of the single circulation of PDA-AC electrode reaches 12mg/g, and be about 2.7 times of AC electrode, current efficiency can reach 60%.Fig. 5 is PDA-AC|PDA-AC electrical condenser repeated charge test under above-mentioned condition.Repeatedly charge and discharge cycles conductivity variations is basically identical, and the desalting performance of electrode materials is stablized, and electrode regeneration is functional.
Fig. 6 is for gathering the cyclic voltammogram of Dopamine HCL modified activated carbon (PDA-AC) electrode and pure gac (AC) electrode.Compared with pure activated carbon electrodes, the cyclic voltammetry curve rectangular characteristic of PDA-AC electrode is more obvious, presents typical electrochemical double layer capacitance characteristic.
Fig. 7 is for gathering the alternating-current impedance figure of Dopamine HCL modified activated carbon (PDA-AC) electrode and pure gac (AC) electrode.Compared with pure activated carbon electrodes, the charge transfer resistance of PDA-AC electrode obviously reduces, and the straight slope of low frequency range electrode is larger, illustrates that ion can move and spread quickly at electrode surface.
Claims (11)
1. a capacitive deionization preparation method for the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, comprising:
(1) porous carbon materials is scattered in dopamine solution stirs 2-24h, then rinse, dry, obtain the modified porous carbon material of poly-Dopamine HCL;
(2) the modified porous carbon material of Dopamine HCL will be gathered and binding agent blended, leave standstill, dry, obtain mixture, then mixture being infiltrated also roll-in covers on inert conductor, obtain the modified porous carbon dioxide process carbon electrode of poly-Dopamine HCL, wherein the poly-modified porous carbon material of Dopamine HCL and the blended mass ratio of binding agent are 12-15:1.
2. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (1), porous carbon materials is one or more in gac, electrically conductive graphite, carbon fiber, carbon nanotube, carbon aerogels.
3. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (1), the solvent of dopamine solution is Tris-HCl damping fluid, pH=7-8; The concentration of dopamine solution is 0.5 ~ 2mg/L.
4. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: stir in described step (1) as mechanical stirring under normal temperature, normal pressure, stir speed (S.S.) is 500r/min.
5. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, it is characterized in that: blendedly in described step (2) to be specially: the poly-modified porous carbon material of Dopamine HCL is scattered in deionized water and forms dispersion liquid, then in dispersion liquid, drip binding agent emulsion and stir 2 ~ 4h, wherein the concentration of dispersion liquid is 50 ~ 80mg/L, and the mass percentage concentration of binding agent is 6 ~ 8%.
6. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (2), binding agent is one or more in polytetrafluoroethylene PTFE, poly(vinylidene fluoride), polyethylene, polypropylene.
7. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (1), (2), bake out temperature is 60-120 DEG C, and the time is 5-16h.
8. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, it is characterized in that: mixture infiltrates and roll-in covers and is specially in described step (2): mixture sprays after treating compound infiltrates, then cover under strong plane pressure action; Wherein strong plane pressure is 3-6MPa.
9. a kind of capacitive deionization according to claim 8 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: described treating compound is one or more in methyl alcohol, ethanol, ice alcohol.
10. a kind of capacitive deionization according to claim 1 preparation method of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (2), inert conductor is one or more in titanium net, graphite paper.
11. a kind of capacitive deionization according to claim 1 preparation methods of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL, is characterized in that: in described step (2), the electrode slice thickness of the poly-modified porous carbon dioxide process carbon electrode of Dopamine HCL is 0.2-2mm.
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| CN105712448A (en) * | 2016-02-26 | 2016-06-29 | 东华大学 | Preparation method of Nafion/porous carbon composite electrode material for capacitive adsorption desalting |
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