CN107089707A - Structure capacitance desalination electrode core shell structure three-dimensional graphene composite material and preparation method thereof - Google Patents
Structure capacitance desalination electrode core shell structure three-dimensional graphene composite material and preparation method thereof Download PDFInfo
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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
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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
- C02F2001/46133—Electrodes characterised by the material
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
Abstract
The present invention relates to a kind of structure capacitance desalination electrode core shell structure three-dimensional graphene composite material and preparation method thereof.This method is by the use of metal organic frame as core, and graphene is used as shell；Electrostatic interaction is carried out by certain density graphite oxide solution at a certain temperature and metal organic frame, the presoma of core shell structure three-dimensional composite material is formed；Further by carbonization, pickling obtains three-dimensional graphene composite material；It is coated in after composite, acetylene black and ptfe emulsion are well mixed on graphite paper, structure capacitance desalination electrode is made in drying.Present invention process is quick, and simply, cost is low, can be mass.The electrode of gained has high-ratio surface and satisfactory electrical conductivity, wetability, and potential application foreground is possessed in terms of structure capacitance desalination.
Description
Technical field
The present invention relates to a kind of structure capacitance desalination electrode core shell structure three-dimensional graphene composite material and preparation method thereof.
Background technology
Shortage of fresh water is one of this century maximum resource crisis for facing of the whole world, seawater and bitter desalting skill
Art has caused social extensive concern as the important channel for effectively solving the crisis.Existing desalination process mainly has the way of distillation
And embrane method.Way of distillation operation temperature is high, and energy consumption is larger, bird nest harm and seriously corroded；Embrane method is strict to film properties requirement, and film is damaged
Bad rate height and somewhat expensive.In addition, these desalination process have the shortcomings that high energy consumption, even consume energy minimum reverse osmosis membrane
Method, its energy consumption is also ten times of theoretical value or so.Therefore, the research and development desalting technology that energy consumption is low, cost is low is the demand in epoch.Electricity
Appearance type desalination is a kind of brand-new desalting technology remote based on electric double layer capacitance.This method energy consumption is low, desalting efficiency is high, to environment
It is friendly.In terms of the softening of the desalination, Yi Jigong, agricultural production and the domestic water that can be applied to seawater and bitter, it develops
Space and have a extensive future.
Principle based on structure capacitance desalination has that specific surface area is big, space is flourishing, good conductivity electrode material turns into and obtained
Obtain the key of high capacitance type desalting performance.Porous carbon materials are due to high specific surface area, good conductive capability, unique
Chemical stability, pore structure be easy to control and is always the first choice of structure capacitance desalination device electrode material the features such as good conductivity.Stone
Black alkene is as a kind of carbon material of new bi-dimensional cellular shape structure, and there is good electric conductivity, larger theory to compare surface for it
The superior performance such as product, high mechanical stability, therefore cause extensive concern.But graphene film interlayer π-π interactions are led
Irreversible reunion and stacking have been caused, its specific surface area is reduced, has been unfavorable for the diffusion and absorption of structure capacitance desalination process intermediate ion,
And then limit its application in capacitive desalination field.Degree, extra object are stacked in order to alleviate graphene（Such as：Carbon nanometer
Pipe, activated carbon etc.）Usually need to be added between graphene layer by different modes, the carbon material so obtained is to a certain degree
On alleviate graphene stacking, but it is difficult to ensure that object is evenly dispersed between graphene layer, therefore the group at some positions of graphene
It is poly- effectively to be solved.In addition, for structure capacitance desalination technology, high-specific surface area, Gao You except electrode material
Sequence structure, electric conductivity, the wetability of electrode material is also very crucial.There are numerous studies to find in porous carbon materials by adding
Extra nitrogen source such as furfural（H.-L. Jiang, B. Liu, Y.-Q. Lan, K. Kuratani, T. Akita, H.
Shioyama, F. Zong and Q. Xu, From MetalOrganic Framework to Nanoporous
Carbon: Toward a Very High Surface Area and Hydrogen Uptake. J. Am. Chem.
Soc., 2011, 133, 11854–11857.）, to reach the purpose for improving its machinery, conductive or chemical property.But by
Complicated in preparation process, nitrogen source is not environmentally so that explore that preparation technology is simple, green high nitrogen quantity three-dimensional grapheme material still
It is challenging.
Metal-organic framework compound has high specific surface area, big pore volume and adjustable pore passage structure, recently quilt
Confirmation can prepare porous carbon materials as carbon precursor or template.And zeolitic imidazolate framework material (Zeolitic
Imidazolate Frameworks, ZIFs) as one of branch of metal organic frame, its high thermal stability and chemistry are steady
The nitrogen source being rich in qualitative and imidazoles dentate, becomes the preferable forerunner of the excellent N doping porous carbon of processability
Body.
The content of the invention
An object of the present invention is to overcome problems of the prior art that there is provided a kind of electric double layer capacitance type desalination
Method carries out desalinization processing and uses core shell structure three-dimensional graphene composite material.
The second object of the present invention is the preparation method for providing the composite.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of structure capacitance desalination electrode core shell structure three-dimensional graphene composite material, it is characterised in that the composite be with
Metal organic frame is used as shell as core, graphene；By the way that at 80 DEG C, graphite oxide solution carries out quiet with metal organic frame
Electric attraction is acted on, and the presoma of core shell structure three-dimensional composite material is formed, by allocating metal organic frame and graphene not
With proportioning, control metal organic frame is covered by the quantity between graphene layer as carbon source and nitrogen source.Wherein three-dimensional grapheme
Mass ratio with the carbon of N doping is：0.1:1~0.4:1；While graphene layer is suppressed with interlayer stacking, the three-dimensional stone of control
The nitrogen content of black alkene composite.Nitrogen content is 6% ~ 12% in the carbon of described N doping.
A kind of method for preparing above-mentioned structure capacitance desalination electrode with core shell structure three-dimensional graphene composite material, its feature
It is concretely comprising the following steps for this method：
A. zinc nitrate hexahydrate and 2-methylimidazole are pressed 1:3~1:8 mol ratio is dissolved in methanol solution, and wherein zinc nitrate is dense
Spend for the wt% of 1 wt% ~ 3, be sufficiently mixed under 350rpm/min ~ 500rpm/min stir speed (S.S.)s it is uniform after, centrifuge, methanol
Washing, drying can obtain metal organic frame ZIF-8；
B. metal organic frame ZIF-8 obtained by step a is dispersed in the graphite oxide that mass percent concentration is 0.1 ~ 0.3%
In the aqueous solution, stir, dry, be placed in tube furnace, in the inert atmosphere of nitrogen or argon gas, it is 2 ~ 4 DEG C to control heating rate
/ min, is warming up to 800 DEG C first, is incubated 3 ~ 4 hours at such a temperature, is then down to room temperature；The salt of gained carbon material and 2mol
Acid or sulfuric acid solution are sufficiently stirred for the h of reaction 8 ~ 12, and the mass ratio of wherein carbon material and acid solution is：1:70~1:100；Fully wash
Wash after drying, produce core shell structure three-dimensional graphene composite material.
The preparation of structure capacitance desalination electrode：By the core shell structure three-dimensional graphene composite material of preparation, acetylene black and poly- four
PVF emulsion is 80 according to mass ratio:10:10~90:5:5 be uniformly mixed after be coated on conductive substrates graphite paper, with
Afterwards in 100 ~ 120 DEG C of dryings；Core shell structure three-dimensional graphene composite material structure capacitance desalination electrode is finally made.
The mol ratio of zinc nitrate hexahydrate and 2-methylimidazole is 1 in above-mentioned preparation process:3~1:8；It is obtained above
ZIF-8 should be diameter uniform in size at 0.05 μm ~ 0.2 μm, to obtain particle diameter less if mol ratio is more than this scope
ZIF-8, due to it because bad dispersibility is then difficult to form core shell structure.
Speed is stirred vigorously in above-mentioned preparation process and is maintained at 350rpm/min ~ 500rpm/min, if stir speed (S.S.) mistake
Greatly, then it is unfavorable for the formation of MOF structures；, can the glomerate MOF structures of shape if mixing time is long.
In above-mentioned preparation process, the mass ratio of metal organic frame ZIF-8 and graphite oxide is：5: 1 ~15:1, if two
The quality that person is combined exceedes this scope, then cannot get core shell structure three-dimensional grapheme structure.
The carbonisation in inert atmosphere described in above-mentioned preparation process, which needs to calcine by temperature control, to be realized, control heating
Speed is 2 ~ 4 DEG C/min, and 800 DEG C are warming up to first, is incubated 3 ~ 4 hours at such a temperature, is then down to room temperature；Inertia is protected
Gas includes nitrogen and argon gas, and gas flow rate is 80 ~ 140 mL/min.Carbonisation is carried out under inert gas shielding, favorably
In keeping carbon backbone structure, if being calcined under the conditions of oxygen-containing, caving in for carbon skeleton can be caused.
By the core shell structure three-dimensional graphene composite material prepared, acetylene black and ptfe emulsion are according to quality
Than for 80:10:10~90:5:5 be uniformly mixed after be coated on conductive substrates graphite paper, then 100 ~ 120 DEG C drying；
Core shell structure three-dimensional graphene composite material structure capacitance desalination electrode is finally made.
The inventive method forms nitrogenous carbon as core using metal organic frame ZIF-8, and graphene is shell, by adjusting metal
Organic frame ZIF-8 and graphene different ratio, and then reach that further control metal organic frame is as carbon source and nitrogen source
The quantity between graphene layer is filled into, while improving graphene specific surface area, the nitrogenous of three-dimensional graphene composite material is controlled
Amount, suppresses graphene and stacks.New type structure of hud three-dimensional graphene composite material desalination electrode prepared by the present invention has higher
Surface area, high conductivity, high wettability, the desalination for high-performance, high efficiency, low energy consumption provides new way.The core of formation
Shell structure three-dimensional graphene composite material have high surface area, high conductivity, be applied to desalination the features such as space is flourishing in terms of,
Believe that this new carbon there can be preferable application prospect in desalination field.Present invention can apply to the light of seawater and bitter
Change, new way is provided for low energy consumption, low cost, high-performance desalination.
Brief description of the drawings
Fig. 1 shines for the transmission electron microscope of core shell structure three-dimensional graphene composite material prepared by the embodiment of the present invention 1
Piece.
Embodiment
After now the specific embodiment of the present invention is described in.The preparation side for the metal organic frame ZIF-8 that the present invention is used
Method refer to following document：Z. Wang, T. Yan, J. Fang, L. Shi, D. Zhang, Nitrogen-doped
porous carbon derived from a bimetallic metal–organic framework as highly
efficient electrodes for flow-through deionization capacitors, J. Mater.
Chem. A, 4 (2016) 10858-10868。
Embodiment 1：By mol ratio 1:4 zinc nitrate hexahydrate is dissolved in 200 ml methanol solutions with 2-methylimidazole, its
Middle nitric acid zinc concentration is 1.5 wt%, is stirred vigorously 12 hours stirring under speed is 350rpm/min, centrifugation, methanol solution wash 2 ~
3 times, drying can obtain metal organic frame ZIF-8；Metal organic frame ZIF-8 obtained by 0.2g is dispersed in into mass concentration is
The 0.1wt% graphite oxide aqueous solution, in 80 ° of stirring in water bath uniformly to dry；By gained core shell structure three-dimensional grapheme composite wood
Material is placed in tube furnace, in gas flow rate under 80 mL/min nitrogen protection, it is 2 DEG C/min, heating to control heating rate
To 800 DEG C, 3 h are incubated at 800 DEG C, is cooled to after room temperature and adds the stirring of 2M hydrochloric acid solutions except the h of metal oxide 12, fill
After dividing washing dry, that is, obtain core shell structure three-dimensional graphene composite material.The core shell structure three-dimensional grapheme of gained is combined
Material is respectively with acetylene black and ptfe emulsion according to mass ratio 80:10:10 it is well mixed after be coated on graphite paper, with
Afterwards in 100 DEG C ~ 120 DEG C dryings.Core shell structure three-dimensional graphene composite material structure capacitance desalination electrode is finally made.
Test above-mentioned core shell structure three-dimensional graphene composite material structure capacitance desalination electrode specific capacitance.Use CHI-660D types
Electrochemical workstation, electrolyte is 0.5M sodium chloride solutions, and sweep speed is 5mV/s, and voltage range is -0.5V ~ 0.5V；Measure
The specific capacitance of the electrode is more than 100F/g.Its desalting performance of the electrode test of above-mentioned preparation, in 100ppm salt solution, its desalination
Efficiency is more than 80%.
Embodiment 2：By mol ratio 1:6 zinc nitrate hexahydrate is dissolved in 100 ml methanol solutions with 2-methylimidazole, its
Middle nitric acid zinc concentration is 3 wt%, is stirred vigorously 12 hours stirring under speed is 400 rpm/min, centrifugation, methanol solution wash 2 ~ 3
Secondary, drying can obtain metal organic frame ZIF-8；Metal organic frame ZIF-8 obtained by 0.4g is dispersed in into mass concentration is
The 0.2wt% graphite oxide aqueous solution, in 80 ° of stirring in water bath uniformly to dry；By gained core shell structure three-dimensional graphene composite material
It is placed in tube furnace, in gas flow rate under 100 mL/min nitrogen protection, it is 3 DEG C/min, heating to control heating rate
To 800 DEG C, 3 h are incubated at 800 DEG C, is cooled to after room temperature and adds the stirring of 2M hydrochloric acid solutions except the h of metal oxide 10, fill
After dividing washing dry, that is, obtain core shell structure three-dimensional graphene composite material.The core shell structure three-dimensional grapheme of gained is combined
Material is respectively with acetylene black and ptfe emulsion according to mass ratio 85:10:5 it is well mixed after be coated on graphite paper, with
Afterwards in 100 DEG C ~ 120 DEG C dryings.Core shell structure three-dimensional graphene composite material structure capacitance desalination electrode is finally made.
Test above-mentioned core shell structure three-dimensional graphene composite material structure capacitance desalination electrode specific capacitance.Use CHI-660D
Type electrochemical workstation, electrolyte is 0.5M sodium chloride solutions, and sweep speed is 5mV/s, and voltage range is -0.5V ~ 0.5V；Survey
The specific capacitance for obtaining the electrode is more than 95F/g.Its desalting performance of the electrode test of above-mentioned preparation, in 300ppm salt solution, it takes off
Salt efficiency is more than 80%.
Embodiment 3：By mol ratio 1:8 zinc nitrate hexahydrate is dissolved in 300 ml methanol solutions with 2-methylimidazole, its
Middle nitric acid zinc concentration is 1 wt%, is stirred vigorously 12 hours stirring under speed is 460rpm/min, centrifugation, methanol solution wash 2 ~ 3
Secondary, drying can obtain metal organic frame ZIF-8；Metal organic frame ZIF-8 obtained by 0.8g is dispersed in into mass concentration is
The 0.1wt% graphite oxide aqueous solution, in 80 ° of stirring in water bath uniformly to dry；By gained core shell structure three-dimensional grapheme composite wood
Material is placed in tube furnace, in gas flow rate under 110mL/min nitrogen protection, it is 4 DEG C/min, heating to control heating rate
To 800 DEG C, 3 h are incubated at 800 DEG C, is cooled to after room temperature and adds the stirring of 2M sulfuric acid solutions except the h of metal oxide 12, fill
After dividing washing dry, that is, obtain core shell structure three-dimensional graphene composite material.The core shell structure three-dimensional grapheme of gained is combined
Material is respectively with acetylene black and ptfe emulsion according to mass ratio 90:5:5 it is well mixed after be coated on graphite paper, then
In 100 DEG C ~ 120 DEG C dryings.Core shell structure three-dimensional graphene composite material structure capacitance desalination electrode is finally made.
Test above-mentioned core shell structure three-dimensional graphene composite material structure capacitance desalination electrode specific capacitance.Use CHI-660D types
Electrochemical workstation, electrolyte is 0.5M sodium chloride solutions, and sweep speed is 5mV/s, and voltage range is -0.5V ~ 0.5V；Measure
The specific capacitance of the electrode is more than 100F/g.Its desalting performance of the electrode test of above-mentioned preparation, in 50ppm salt solution, its desalination
Efficiency is more than 85%.
Claims (2)
1. a kind of structure capacitance desalination electrode core shell structure three-dimensional graphene composite material, it is characterised in that the composite be with
Metal organic frame ZIF-8 is as core, and the three-dimensional structure graphene that nitrogen mixes is as shell；Acted on by electrostatic attraction, form core
Shell structure three-dimensional composite material；The mass ratio for the three-dimensional structure graphene that described organic frame ZIF-8 mixes with nitrogen is：5: 1
~15: 1。
2. a kind of prepare structure capacitance desalination electrode core shell structure three-dimensional graphene composite material according to claim 1
Method, it is characterised in that this method is concretely comprised the following steps：
A. zinc nitrate hexahydrate and 2-methylimidazole are pressed 1:3~1:8 mol ratio is dissolved in methanol solution, and wherein zinc nitrate is dense
Spend for the wt% of 1 wt% ~ 3, be sufficiently mixed under 350rpm/min ~ 500rpm/min stir speed (S.S.)s it is uniform after, centrifuge, methanol
Washing, drying can obtain metal organic frame ZIF-8；
B. metal organic frame ZIF-8 obtained by step a is dispersed in the graphite oxide that mass percent concentration is 0.1 ~ 0.3%
In the aqueous solution, stir, dry, be placed in tube furnace, in the inert atmosphere of nitrogen or argon gas, it is 2 ~ 4 DEG C to control heating rate
/ min, is warming up to 800 DEG C first, is incubated 3 ~ 4 hours at such a temperature, is then down to room temperature, obtains carbon material；Described metal
The mass ratio of organic frame ZIF-8 and graphite oxide is：5: 1 ~15: 1；
C. the hydrochloric acid or sulfuric acid solution of carbon material obtained by step b and 2mol are sufficiently stirred for the h of reaction 8 ~ 12, wherein carbon material with
The mass ratio of acid solution is：1:70~1:100；After fully washing is dried, core shell structure three-dimensional graphene composite material is produced.
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| CN109097788A (en) * | 2018-08-10 | 2018-12-28 | 复旦大学 | A kind of double carbon coupling transiting metal nickel based quantum dot elctro-catalyst and preparation method thereof |
| CN109935812A (en) * | 2019-03-13 | 2019-06-25 | 河源广工大协同创新研究院 | A kind of novel lithium sulfur battery anode material and preparation method thereof |
| CN110156120A (en) * | 2019-06-26 | 2019-08-23 | 中南大学 | Sewage-treatment plant and processing method |
| CN113830866A (en) * | 2021-08-23 | 2021-12-24 | 南京公诚节能新材料研究院有限公司 | Deionization electrode material for capacitor and preparation method thereof |
| CN114496586A (en) * | 2022-02-18 | 2022-05-13 | 常州大学 | Nitrogen-doped three-dimensional graphene/MOF (Metal organic framework) derived carbon composite electrode material for capacitive deionization and preparation and application thereof |
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