CN104817144B - A kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes - Google Patents
A kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes Download PDFInfo
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- CN104817144B CN104817144B CN201510173985.2A CN201510173985A CN104817144B CN 104817144 B CN104817144 B CN 104817144B CN 201510173985 A CN201510173985 A CN 201510173985A CN 104817144 B CN104817144 B CN 104817144B
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Abstract
The present invention relates to a kind of preparation method of capacitive deionization with poly-dopamine modified lithium porous carbon electrodes, porous carbon materials are scattered in dopamine buffer solution by (1) carries out surface aggregate, and the porous carbon materials of poly-dopamine modified lithium are obtained by flushing, drying；(2) poly-dopamine modified lithium porous carbon materials and binding agent are blended and uniform slurries is formed in water, cloud mixture is formed by drying, and this mixture roll-in is covered on inert conductor, obtain poly-dopamine modified lithium porous carbon electrodes.Poly-dopamine modified lithium porous carbon electrodes good hydrophilic property, mechanical stability prepared by the present invention are strong, technique is simple, cost performance is high, diffusion and transmission of the ion in electrode surface can be effectively facilitated, improve electric double layer performance, it is adaptable to assemble ultracapacitor, desalination speed and desalination amount can be improved.
Description
Technical field
The invention belongs to the preparation field of capacitive deionization electrode, more particularly to a kind of capacitive deionization poly-dopamine
The preparation method of modified porous carbon electrode.
Background technology
The principle of supercapacitor desalination cell technology is based in the presence of electrostatic field, the anions and canons difference in solution
It is adsorbed on positive and negative electrode, so as to realize the desalination of water.During capacitive desalination, electrode material is to determine desalting performance
Key factor.Preferable electrode material should possess high-specific surface area, suitable pore-size distribution and good electric conductivity and hydrophilic
Property.
High with specific surface area, the abundant carbon material in space is conventional electrode material, but porous carbon materials are hydrophilic in itself
Property it is poor, diffusion and transmission in electrode surface in capacitive desalination process intermediate ion are limited, so as to reduce desalination speed and de-
Salt amount.Therefore, the hydrophily for improving porous carbon materials is a kind of method for effectively improving carbon electrode desalting performance.W.Li,
Z.M.Xie,Z.M.Li,Synthesis,characterization of polyacrylate-g-carbon black and
its application to soap-freewaterborne coating,J.Appl.Polym.Sci.81(2001)1100–
1106. report one kind obtains hydrophily and dispersiveness preferably modified carbon black in carbon blacksurface graft copolymerization polyacrylate,
But its to there is course of reaction complicated and the shortcomings of using toxic reagent.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of capacitive deionization poly-dopamine modified lithium porous carbon electrodes
Preparation method, the electrode for preparing of the present invention compares with without poly-dopamine modified lithium porous carbon electrodes, and of the invention is poly- more
The modified porous carbon electrode of bar amine, using in the dopamine solution of alkalescence, is reacted in porous carbon by the self-polymerization of dopamine
The hydrophilic poly-dopamine layer of one layer of material surface formation, improves the hydrophily of electrode, improves due to hydrophilic, can promote
Enter diffusion and transmission of the ion in electrode surface, improve the rate of adsorption and adsorbance of electrode pair ion；The poly- DOPA of the present invention
The modified porous carbon electrode preparation method of amine is simple, and cost is low, easy industrial application.
A kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes of the present invention, including：
(1) porous carbon materials are scattered in into stirring 2-24h in dopamine solution to be polymerize, then rinse, dries, obtain
Poly-dopamine modified lithium porous carbon materials；
(2) poly-dopamine modified lithium porous carbon materials and binding agent are blended to form slurries, stand, pump supernatant, obtain
Sediment dried, obtain cloud mixture, then by mixture infiltration and roll-in cover on inert conductor, produce poly-
The modified porous carbon electrode of dopamine, wherein poly-dopamine modified lithium porous carbon materials are 12-15 with binding agent blending mass ratio:1.
Porous carbon materials is in activated carbon, electrically conductive graphite, carbon fiber, CNT, carbon aerogels in the step (1)
It is one or more of.
The solvent of dopamine solution is Tris-HCl buffer solutions, pH=7-8 in the step (1)；Dopamine solution it is dense
Spend for 0.5~2mg/L.
Stirring is mechanical agitation under normal temperature, normal pressure in the step (1), and stir speed (S.S.) is 500r/min.
Rinsed in the step (2) is deionized water rinsing.
Blending is specially in the step (2)：Poly-dopamine modified lithium porous carbon materials are scattered in deionized water and formed
Dispersion liquid, is then added dropwise into dispersion liquid and bonds agent emulsion and stir 2~4h, the wherein concentration of dispersion liquid is 50~80mg/L,
The mass percentage concentration of binding agent is 6~8%.
Binding agent is one in polytetrafluoroethylene PTFE, polyvinylidene fluoride, polyethylene, polypropylene in the step (2)
Plant or several.
Drying temperature is 60-120 DEG C in the step (1), (2), and the time is 5-16h.
The time stood in the step (2) is 2-5h.
Simultaneously roll-in is covered specially for mixture infiltration in the step (2)：Sprayed on mixture after size infiltration (in paste
Shape thing), then covered under strong plane pressure action；Wherein strong plane pressure is 3-6MPa.
The size is the one or more in methanol, ethanol, ice alcohol.
Inert conductor is the one or more in titanium net, graphite paper in the step (2).
The electrode slice thickness of poly-dopamine modified lithium porous carbon electrodes is 0.2-2mm in the step (2).
The present invention electrode be porous carbon and poly-dopamine, poly-dopamine be dopamine under solution state through self-polymerization
Reaction load is formed on porous carbon.
Beneficial effect
The poly-dopamine modified lithium porous carbon electrodes of the present invention, using in the dopamine solution of alkalescence, pass through dopamine
Self-polymerization reaction forms one layer of hydrophilic poly-dopamine layer on porous carbon materials surface, improves the hydrophily of electrode；
The poly-dopamine modified lithium porous carbon electrodes of the present invention, improve due to hydrophilic, can promote ion in electrode table
The diffusion and transmission in face, improve the rate of adsorption and adsorbance of electrode pair ion；
The poly-dopamine modified lithium porous carbon electrodes preparation method of the present invention is simple, and cost is low, easy industrial application.
Brief description of the drawings
Fig. 1 is contact angle figure, wherein (a) is the contact angle figure of pure activated carbon (AC)；(b) it is poly-dopamine modified lithium activated carbon
(PDA-AC) contact angle figure；
Fig. 2：The SEM shape appearance figures of pure activated carbon (AC) electrode；
Fig. 3：The circulation adsorption desorption curve of pure activated carbon (AC) electrode symmetric capacitors (AC | AC)；
Fig. 4：Pure activated carbon (AC) electrode answers symmetric capacitor (AC with poly-dopamine modified lithium activated carbon (PDA-AC) electrode pair
| AC) and (PDA-AC | PDA-AC) circulation adsorption desorption curve；
Fig. 5：Poly-dopamine modified lithium activated carbon (PDA-AC) electrode symmetric capacitors (PDA-AC | PDA-AC) in multiple constant current
Voltage change and corresponding conductivity variations curve in charge and discharge process；
Fig. 6：The cyclic voltammogram of pure activated carbon (AC) electrode and poly-dopamine modified lithium activated carbon (PDA-AC) electrode；
Fig. 7：The AC impedance figure of pure activated carbon (AC) electrode and poly-dopamine modified lithium activated carbon (PDA-AC) electrode.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
Preparation and symmetric capacitor the desalination test of pure activated carbon electrodes：
Compound concentration is 80mg/mL activated carbon mixed serums, and PTFE emulsion is slowly added dropwise, and (mass fraction of PTFE emulsion is
60%), wherein the quality of PTFE emulsion is the 12% of quality of activated carbon, after stirring 2h, stands, pumps supernatant, in 100 DEG C of bakings
Drying obtains cotton-shaped activated carbon/PTFE mixtures in case.A small amount of ethanol is added into above-mentioned activated carbon/PTFE cloud mixtures
Wetting, roll-in is in blocks and is pressed in titanium net, obtains pure activated carbon (AC) electrode.Fig. 2 is the SEM shape appearance figures of pure activated carbon electrodes.
Take the pure activated carbon electrodes of two panels to be assembled into symmetric capacitor (AC | AC), be that desalination is molten with 500mg/L NaCl solution
Liquid, constant current charge-discharge test is carried out under conditions of target voltage is 1.2V.Fig. 3 is that pure activated carbon symmetric capacitor fills in constant current
Electrical conductivity versus time curve under discharge mode.As a result show, the single loop desalination amount of pure activated carbon electrodes is
4.5mg/g, current efficiency is 30%.
Embodiment 2
Poly-dopamine modified lithium activated carbon electrodes are prepared and symmetric capacitor desalination test：
At ambient temperature, 2g activated carbons are dispersed in for 1g/L, pH by 100mL dopamine concentrations by mechanical agitation
In=8.5 Tris-HCl buffer solutions, stirring reaction 4h, then with a large amount of deionized water filtration washings and drying, obtain poly- DOPA
Amine modified activated carbon.Fig. 1 is the contact angle figure of pure activated carbon and poly-dopamine modified lithium activated carbon.
Compound concentration is 80mg/mL poly-dopamine modified lithium activated carbon mixed serum, and 12%PTFE emulsions are slowly added dropwise
(PTFE emulsion mass fraction 60%), the wherein quality of PTFE emulsion are the 12% of poly-dopamine modified lithium quality of activated carbon, mixing
Stir.Stir after 2h, stand, pump supernatant, drying obtains cotton-shaped activated carbon/PTFE mixing in 100 DEG C of baking ovens
Thing.Activated carbon/PTFE mixtures are taken out, ethanol wet formation pastel are sprayed thereto, roll-in is in blocks and is pressed in titanium net, makes
Obtain poly-dopamine modified lithium activated carbon electrodes.With poly-dopamine modified lithium activated carbon (PDA-AC) electrode assembling into symmetric capacitor
(PDA-AC | PDA-AC), constant current charge-discharge test is carried out using 500mg/L NaCl solution.Fig. 4 is constant current charge-discharge cyclic module
Under formula, AC | AC and PDA-AC | PDA-AC symmetric capacitor electrical conductivity versus time curves.As a result show, PDA-AC electrodes
The desalination amount of single loop reaches 12mg/g, about the 2.7 of AC electrodes times, and current efficiency is up to 60%.Fig. 5 is under above-mentioned condition
PDA-AC | PDA-AC capacitors repeated charge is tested.Multiple charge and discharge cycles conductivity variations are basically identical, electrode material
Desalting performance is stable, and electrode regeneration is functional.
Fig. 6 is the cyclic voltammogram of poly-dopamine modified lithium activated carbon (PDA-AC) electrode and pure activated carbon (AC) electrode.With
Pure activated carbon electrodes are compared, and the cyclic voltammetry curve rectangular characteristic of PDA-AC electrodes becomes apparent from, and the double electricity of typical electrochemistry are presented
Layer capacitance characteristic.
Fig. 7 is the AC impedance figure of poly-dopamine modified lithium activated carbon (PDA-AC) electrode and pure activated carbon (AC) electrode.With
Pure activated carbon electrodes are compared, and the charge transfer resistance of PDA-AC electrodes is obviously reduced, and the straight slope of low frequency region electrode is bigger,
Illustrate that ion quickly can be migrated and spread in electrode surface.
Claims (11)
1. a kind of capacitive deionization preparation method of poly-dopamine modified lithium porous carbon electrodes, including：
(1) porous carbon materials are scattered in dopamine solution and stir 2-24h, then rinsed, dry, obtain poly-dopamine modified lithium
Porous carbon materials；
(2) poly-dopamine modified lithium porous carbon materials and binding agent are blended, stand, dries, mixture is obtained, then by mixture
Infiltrate and roll-in is covered on inert conductor, produce poly-dopamine modified lithium porous carbon electrodes, wherein poly-dopamine modified lithium porous carbon
Material is 12-15 with binding agent blending mass ratio:1.
2. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Porous carbon materials is in activated carbon, electrically conductive graphite, carbon fiber, CNT, carbon aerogels in the step (1)
One or more.
3. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：The solvent of dopamine solution is Tris-HCl buffer solutions, pH=7-8 in the step (1)；Dopamine solution it is dense
Spend for 0.5~2mg/L.
4. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Stirring is mechanical agitation under normal temperature, normal pressure in the step (1), and stir speed (S.S.) is 500r/min.
5. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Blending is specially in the step (2)：Poly-dopamine modified lithium porous carbon materials are scattered in deionized water and formed
Dispersion liquid, is then added dropwise into dispersion liquid and bonds agent emulsion and stir 2~4h, the wherein concentration of dispersion liquid is 50~80mg/L,
The mass percentage concentration of binding agent is 6~8%.
6. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Binding agent is one in polytetrafluoroethylene PTFE, polyvinylidene fluoride, polyethylene, polypropylene in the step (2)
Plant or several.
7. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Drying temperature is 60-120 DEG C in the step (1), (2), and the time is 5-16h.
8. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Simultaneously roll-in is covered specially for mixture infiltration in the step (2)：Sprayed on mixture after size infiltration, then
Covered under strong plane pressure action；Wherein strong plane pressure is 3-6MPa.
9. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 8, its
It is characterised by：The size is the one or more in methanol, ethanol, ice alcohol.
10. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：Inert conductor is the one or more in titanium net, graphite paper in the step (2).
11. a kind of preparation method of capacitive deionization poly-dopamine modified lithium porous carbon electrodes according to claim 1, its
It is characterised by：The electrode slice thickness of poly-dopamine modified lithium porous carbon electrodes is 0.2-2mm in the step (2).
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| KR101861013B1 (en) * | 2016-10-18 | 2018-05-25 | 주식회사 제낙스 | Fiber electrode using surface-polymerization and surface modification for the same |
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| CN107768692B (en) * | 2017-08-31 | 2020-02-14 | 华南师范大学 | Polydopamine-coated carbon nanotube-reinforced ascorbic acid/glucose fuel cell |
| CN109632912A (en) * | 2018-12-29 | 2019-04-16 | 中国科学院烟台海岸带研究所 | A method of improving polymer film ion selective electrode stability and service life in biology sample detection |
| CN114538578A (en) * | 2022-03-18 | 2022-05-27 | 南开大学 | Silicon sphere poly-dopamine-cobalt composite derived defect-rich carbon electrode and preparation and application thereof |
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