CN110422914A - A kind of charcoal base capacitance electrode material and the capacitive electrode using its preparation - Google Patents
A kind of charcoal base capacitance electrode material and the capacitive electrode using its preparation Download PDFInfo
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- CN110422914A CN110422914A CN201910709680.7A CN201910709680A CN110422914A CN 110422914 A CN110422914 A CN 110422914A CN 201910709680 A CN201910709680 A CN 201910709680A CN 110422914 A CN110422914 A CN 110422914A
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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
Abstract
The invention belongs to capacitive deionization technical fields, and in particular to a kind of charcoal base capacitance electrode material, the capacitive electrode using its preparation and its application.The electrode material includes charcoal, conductive black and Kynoar, and the mass ratio of the charcoal, conductive black and Kynoar is 6-9:1-1.5:1-1.5, and the charcoal is made by ligno-cellulosic materials charing process；Charcoal base capacitance electrode is prepared using the material, the electrode has biggish Electro Sorb specific volume and lesser impedance, under the sweep speed of electrochemical workstation 5mV/s, its specific capacity is up to 173F/g, the Electro Sorb effect for greatly improving electrode, in addition, using raw material of the non-activated charcoal as electrode material in the electrode material, cost is lower, is conducive to being widely popularized for Electro Sorb technology.
Description
Technical field
The invention belongs to capacitive deionization technical fields, and in particular to a kind of charcoal base capacitance electrode material uses
Its capacitive electrode prepared and its application.
Background technique
As globalization process is accelerated, population constantly increases, and water resources problems become increasingly conspicuous.The ocean area of the earth accounts for entirely
70 or more the percent of sphere area, seawater salt content is very high, needs to desalinate can be used as freshwater resources use.It is handed over compared to ion
It changes, the desalting technology that ultrafiltration and nanofiltration, reverse osmosis etc. are traditional, for Electro Sorb without pressurization, low energy consumption and recyclable, environmental-friendly.
Ion-exchange, regeneration trouble, is also easy to produce secondary pollution；Ultrafiltration and nanofiltration process generally require secondary pressurized, need to pump raising
Additional energy, ultrafiltration membrane and nanofiltration membrane easily block easy to aging, and film is at high cost, and reverse osmosis technology energy consumption is higher and desalination is not thorough.
Electro Sorb technology because its water treatment efficiency height, energy-saving consumption etc. many merits and receive significant attention.
Capacitive deionization technology is a kind of efficient water treatment technology based on Electrostatic Absorption, applied to the ionic in water
Pollutant removal.As a kind of emerging water treatment technology, the technology is environmental-friendly because having, and easy to operate and design is simple
The advantages that and receive significant attention.Currently, a variety of materials are used to prepare electric adsorption electrode in order to improve Electro Sorb capacity, as
Active carbon, carbon nanotube, charcoal aerosol, graphene, carbon cloth and various metal oxides and emerging nano material etc..It is comprehensive
On, although active carbon is most common electrode material, in actual extension process, active carbon be used as electric adsorption electrode at
This is still very high, hinders Electro Sorb technological industrialization and promotes therefore, it is necessary to seek price more cheap, environmental-friendly
Material is used to prepare electric adsorption electrode.
Summary of the invention
To solve the above problems, the present invention provides a kind of charcoal base capacitance electrode material, the material is directly with wooden
Cellulosic material is that raw material charing is charcoal, further activates without activator, i.e., is prepared by mixing into electricity with materials such as carbon blacks
Tolerant electrode material, and the capacitive electrode capacitance of material preparation is higher.
A kind of charcoal base capacitance electrode material, including charcoal, conductive black and Kynoar, the biology
The mass ratio of charcoal, conductive black and Kynoar is 6-9:1-1.5:1-1.5, and the charcoal is by ligno-cellulosic materials charcoal
Change processing to be made.
Preferably, the plant containing lignocellulosic in the nature of the wood fibre, as cattail, reed,
Straw, stalk, timber etc..
Preferably, the mass ratio of the charcoal, conductive black and Kynoar is 8:1-1.5:1-1.5.
Preferably, the charing process refers to: under nitrogen atmosphere, 450-800 DEG C of charing 0.5-5h.
Preferably, the charing process refers to: under nitrogen atmosphere, 800 DEG C of charing 2.5h.
Preferably, cleaned, crushing and sieving, the sieving referred to before the ligno-cellulosic materials charing process
60-300 mesh.More preferably, the sieving referred to 200 meshes.
The present invention also provides a kind of charcoal base capacitance electrode prepared using above-mentioned material, the electricity of the capacitive electrode
Capacity is higher, which is the collector that load has above-mentioned charcoal base capacitance electrode material.
Preferably, the amount that the charcoal is loaded on the collector is 5-50mg/cm2。
Preferably, the collector is nickel foam.
The present invention also provides the preparation method of above-mentioned charcoal base capacitance electrode, by the capacitive electrode material and
Organic solvent is uniformly mixed to obtain electrode slurries, infiltrates collector using the electrode slurries, dry, and charcoal base capacitance is made
Electrode material.
Preferably, the organic solvent is selected from ethyl alcohol, acetone, DMF (n,N-Dimethylformamide), N-Methyl pyrrolidone
With one of dimethyl acetamide or a variety of.
Preferably, the temperature of the drying is 60-150 DEG C.
Preferably, it can infiltrate repeatedly, dry to collector and coated completely.
The beneficial effects of the present invention are:
(1) charcoal in capacitive electrode material of the invention is using ligno-cellulosic materials i.e. natural material as raw material
Charcoal is prepared, the pore size distribution of the charcoal is mainly distributed on the range of 0.55-0.60nm, biggish micropore and Bi Biao
The transmission and storage that area is conducive to Electro Sorb process ion obtain charcoal then by the charcoal and certain material compatibility
Base capacitance electrode material prepares charcoal base capacitance electrode using the material, which has biggish Electro Sorb specific volume
With lesser impedance, under the sweep speed of electrochemical workstation 5mV/s, specific capacity is up to 173F/g, greatly improves electrode
Suction-operated；
(2) lignocellulosic that capacitive electrode material of the invention uses is not necessarily to before and after charing process for natural material
It is activated, has greatly saved the cost of electrode material, furthermore, the preparation cost of charcoal is $ 350 per ton every to $ 1200
Ton, and the preparation cost of active carbon is $ 1100 per ton per ton to $ 1700, it is clear that use charcoal to be more conducive to electric suction as raw material
Attached technology is widely popularized.
Detailed description of the invention
Fig. 1 is the photo of charcoal electrode slice prepared by embodiment 1；
Fig. 2 is the electron-microscope scanning figure of cattail charcoal prepared by embodiment 1；
Fig. 3 is the characterization result of cattail charcoal prepared by embodiment 1, wherein (a) is nitrogen adsorption-analysis diagram, (b)
For micropore distribution map；
Fig. 4 is the cyclic voltammetry curve figure of charcoal base capacitance electrode prepared by embodiment 1；
Fig. 5 is the electron-microscope scanning figure for the active carbon that comparative example 1 uses；
Fig. 6 is the characterization result for the active carbon that comparative example 1 uses, wherein (a) is nitrogen adsorption-analysis diagram, (b) is micro-
Pore size distribution figure；
Fig. 7 is the cyclic voltammetry curve figure of active carbon base capacitance electrode prepared by comparative example 1；
Fig. 8 is the impedance plot of charcoal base capacitance electrode and active carbon capacitive electrode；
Fig. 9 is charcoal base capacitance electrode and active carbon base capacitance electrode electro-adsorption demineralization experiment dress in embodiment 2
It sets；
Figure 10 is charcoal base capacitance electrode and active carbon base capacitance electrode electro-adsorption demineralization effect in embodiment 2
Figure.
Specific embodiment
The preparation of embodiment 1 charcoal base capacitance electrode material and charcoal base capacitance electrode
1) park wetland discards cattail and collects cleaning, air-dried, crushing, crosses 200 meshes, in pipe under 800 DEG C of logical condition of nitrogen gas
(Nanjing Bo Yuntong instrument Science and Technology Ltd., model RTL1200-1200-I) carbonizes 2.5 hours obtained cattail biologies in formula furnace
Charcoal；
2) cattail charcoal, conductive black (Japanese lion king Ketjen black, model EC300), Kynoar, 50mL N are used
N- dimethyl acetamide (doing solvent use) is uniformly mixed preparation electrode slurries, the cattail charcoal, conductive black, polyvinylidene fluoride
The mass ratio of alkene is 8:1:1；
3) 80 DEG C of dryings in air dry oven after nickel foam (80 × 80 × 1.5mm) infiltration electrode slurries, infiltrate repeatedly
Dry obtained charcoal base capacitance electrode (Fig. 1), electrode slice surface reactive material Load Balanced, charcoal on every plate electrode
Load capacity is 0.4g.
Electron-microscope scanning is carried out to the cattail charcoal of above-mentioned preparation, electron-microscope scanning figure as shown in Fig. 2, biomass in high temperature item
The following solution of part, which is appointed, retains vascular structure (Fig. 2 a), and vascular structure is conducive to ion transmission, reduces the resistance of ion transmission
Power.Part vascular bundle, which is crushed (Fig. 2 b), leads to the high-specific surface area of charcoal, and the charcoal of high-specific surface area is conducive to ion
Storage.
Specific surface and micropore size characterization are carried out to the charcoal of above-mentioned preparation, as a result as shown in figure 3, Fig. 3 a is charcoal
To the absorption analysis diagram of nitrogen, absorption-desorption curve shows the typical curve of carbon material, contains a large amount of suction under low pressure
It is attached, specific surface area 733.622m2/g.Fig. 3 b shows that the pore size distribution of charcoal is mainly distributed on 0.55-0.60nm's
Range, biggish micropore and specific surface area are conducive to the transmission and storage of Electro Sorb process ion.
Electrochemistry cyclic voltammetric characterization carried out to the charcoal base capacitance electrode of above-mentioned preparation, result referring to fig. 4, root
According to calculating it is found that charcoal base capacitance electrode reaches 173F/g specific capacity under the conditions of sweeping fast 5mV/s.
The preparation of embodiment 2 charcoal base capacitance electrode material and charcoal base capacitance electrode
1) peanut shell collects cleaning, air-dries, crushes, crossing 200 meshes, 650 DEG C of (Nanjing Bo Yuntong instrument sections in tube furnace
Skill Co., Ltd, model RTL1200-1200-I) under logical condition of nitrogen gas charing process 4.0 hours at peanut hull biologic charcoal；
2) peanut hull biologic charcoal, conductive black (Japanese lion king Ketjen black, model EC-600JD), Kynoar, N- are used
Methyl pyrrolidone 50mL is uniformly mixed and prepares electrode slurries, the peanut hull biologic charcoal, conductive black, Kynoar
Mass ratio is 8:1:1；
3) 70 DEG C of dryings in air dry oven after nickel foam leaching (80 × 80 × 1.0mm) profit electrode slurries, infiltrate repeatedly
Dry obtained peanut hull biologic charcoal base capacitance electrode, electrode slice surface reactive material Load Balanced, charcoal on every plate electrode
Load capacity be 0.38g.
Specific surface and micropore size characterization, adsorption capacity 733.62m are carried out to the charcoal of above-mentioned preparation2/ g, biology
The pore size distribution of charcoal is mainly distributed on the range of 0.60-1.10nm, and biggish micropore and specific surface area are conducive to Electro Sorb
The transmission and storage of process ion.
Electrochemistry cyclic voltammetric characterization is carried out to the charcoal base capacitance electrode of above-mentioned preparation, is sweeping fast 5mV/s condition
Under reach 162.6F/g specific capacity.
The preparation of 1 active carbon base capacitance electrode of comparative example
1) the common commercial active carbon (Shanghai Aladdin biochemical technology limited liability company) of purchase, crosses 200 meshes, after dry
It is ready to use in and prepares activated carbon electrodes；
2) active carbon, conductive black (Japanese lion king Ketjen black, model EC300), Kynoar, 50mL N N- diformazan
Yl acetamide (doing solvent use) is uniformly mixed preparation electrode slurries, the active carbon, conductive black, the mass ratio of Kynoar
For 8:1:1；
3) 80 DEG C of dryings in air dry oven after nickel foam (80 × 80 × 1.5mm) infiltration electrode slurries, infiltrate repeatedly
Dry that active carbon base capacitance Electro Sorb material is made, the load capacity of charcoal is 0.4g on every plate electrode.
Electron-microscope scanning is carried out to above-mentioned active carbon, electron-microscope scanning figure is as shown in figure 5, active carbon is relatively raw in micrometer scale surface
Object charcoal is smooth, and the gap of micron-scale is less.
Specific surface and micropore size characterization are carried out to above-mentioned active carbon, as a result as shown in fig. 6, Fig. 6 a is activity to nitrogen
Adsorb analysis diagram, specific surface area 1021.408m2/ g, Fig. 6 b show that the pore size distribution of active carbon is mainly distributed on 0.32-
The range of 0.50nm, peak value appear in 0.42nm, although active carbon reference area is bigger, its micropore is smaller with biggish
Hole resistance is unfavorable for the transmission of Electro Sorb ion, the following Fig. 7 of cyclic voltammetric characterization result, biological carbon resistance rod and activated carbon electrodes
Impedance characterization it is as shown in Figure 8.
Activated carbon electrodes reach 136.50F/g specific capacity under the conditions of sweeping fast 5mV/s, than biological carbon resistance rod specific capacity
(136.50F/g) is small.The impedance of biological carbon resistance rod (3.90 ohm) and activated carbon electrodes (11.37 ohm) shows charcoal
The impedance of electrode is smaller, is more advantageous to ion transmission.
2 charcoal base capacitance electrode of embodiment and active carbon base capacitance electrode electro-adsorption demineralization Experimental comparison fruit
1) experimental provision is as shown in figure 5, constant voltage source (million letters, KXN-3030D), universal meter (ELECALL, 33D),
Peristaltic pump (outstanding perseverance peristaltic pump, BT-600EA/DGX).Water distribution: the sodium chloride solution of 150mL, 50mg/L is tested, with 10mL/min
Flow velocity circulates between electrode.Voltage difference is 1.2V between electric adsorption electrode.
After power-up, each certain time water sampling simultaneously measures water sodium chloride concentration with ion chromatography prison ICS-5000.Experiment
Shown in result figure 10:
Biological carbon resistance rod is to the salt ion Electro Sorb effect in salt water significantly better than active carbon electricity in sequencing batch reactor
Pole.In 40 minutes, biological carbon resistance rod makes salt water salt content drop to 14.94mg/L from 50mg/L, is than adsorption capacity
13.15mg/g, and activated carbon electrodes make salt water salt content drop to 26.03mg/L from 50mg/L in 40 minutes, hold than absorption
Amount is 8.99mg/g.
Claims (10)
1. a kind of charcoal base capacitance electrode material, including charcoal, conductive black and Kynoar, the charcoal are led
The mass ratio of electric carbon black and Kynoar is 6-9:1-1.5:1-1.5, and the charcoal is by ligno-cellulosic materials charing
Reason is made.
2. charcoal base capacitance electrode material according to claim 1, which is characterized in that the charcoal, conductive charcoal
Black and Kynoar mass ratio is 8:1-1.5:1-1.5.
3. charcoal base capacitance electrode material according to claim 1, which is characterized in that the charing process refers to:
Under nitrogen atmosphere, 450-800 DEG C of charing 0.5-5h.
4. charcoal base capacitance electrode material according to claim 3, which is characterized in that the charing process refers to:
Under nitrogen atmosphere, 800 DEG C of charing 2.5h.
5. charcoal base capacitance electrode material according to claim 1, which is characterized in that the ligno-cellulosic materials
Cleaned before charing process, crushing and sieving, the sieving referred to 60-300 mesh.More preferably, the sieving refers to
Cross 200 meshes.
6. a kind of charcoal base capacitance electrode using any one of the claim 1-5 material preparation, which is characterized in that institute
Stating charcoal base capacitance electrode is that load has the right to require the afflux of any one of 1-5 charcoal base capacitance electrode material
Body.
7. charcoal base capacitance electrode according to claim 6, which is characterized in that load the life on the collector
The amount of object charcoal is 5-50mg/cm2。
8. charcoal base capacitance electrode according to claim 7, which is characterized in that the collector is nickel foam.
9. the preparation method of any one of the claim 6-8 charcoal base capacitance electrode, by the charcoal base capacitance
Electrode material and organic solvent are uniformly mixed to obtain electrode slurries, infiltrate collector using the electrode slurries, dry, and biology is made
Charcoal base capacitance electrode material.
10. preparation method according to claim 9, which is characterized in that the organic solvent be selected from ethyl alcohol, acetone, DMF,
One of N-Methyl pyrrolidone and dimethyl acetamide are a variety of, it is preferred that the temperature of the drying is 60-150 DEG C.
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Cited By (5)
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|---|---|---|---|---|
| CN111252866A (en) * | 2020-01-20 | 2020-06-09 | 中南大学 | CDI electrode active material and preparation and application thereof |
| CN112051384A (en) * | 2020-09-02 | 2020-12-08 | 盐城工学院 | In-situ biochar-soil mineral composite sample collection method |
| KR20220007535A (en) * | 2020-07-10 | 2022-01-18 | 고려대학교 산학협력단 | Method for fabricating biochar based eledctrode and electrical energy storage device including the same |
| CN113979434A (en) * | 2021-12-08 | 2022-01-28 | 吉林大学 | Biomass-based carbon electrode material and preparation method and application thereof |
| CN114314771A (en) * | 2021-12-13 | 2022-04-12 | 江南大学 | Activated blue algae biochar cathode material and application thereof in degradation of antibiotics |
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| CN109422263A (en) * | 2017-08-21 | 2019-03-05 | 中国科学院理化技术研究所 | A kind of fibrination mesoporous activated carbon and the preparation method and application thereof |
| CN109467082A (en) * | 2018-12-18 | 2019-03-15 | 济南大学 | A kind of preparation method being graphitized the derivative carbon electrode material of porous corncob |
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| CN104715934A (en) * | 2013-12-16 | 2015-06-17 | 中国科学院兰州化学物理研究所 | Hybrid super capacitor and manufacturing method thereof |
| CN106784729A (en) * | 2017-01-20 | 2017-05-31 | 武汉科技大学 | Carbide-derived carbon/charcoal composite energy-storage material and preparation method and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111252866A (en) * | 2020-01-20 | 2020-06-09 | 中南大学 | CDI electrode active material and preparation and application thereof |
| KR20220007535A (en) * | 2020-07-10 | 2022-01-18 | 고려대학교 산학협력단 | Method for fabricating biochar based eledctrode and electrical energy storage device including the same |
| CN112051384A (en) * | 2020-09-02 | 2020-12-08 | 盐城工学院 | In-situ biochar-soil mineral composite sample collection method |
| CN112051384B (en) * | 2020-09-02 | 2022-09-09 | 盐城工学院 | In-situ biochar-soil mineral composite sample collection method |
| CN113979434A (en) * | 2021-12-08 | 2022-01-28 | 吉林大学 | Biomass-based carbon electrode material and preparation method and application thereof |
| CN114314771A (en) * | 2021-12-13 | 2022-04-12 | 江南大学 | Activated blue algae biochar cathode material and application thereof in degradation of antibiotics |
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