CN109019781A - A kind of cement base composite carbon electrode and the preparation method and application thereof - Google Patents
A kind of cement base composite carbon electrode and the preparation method and application thereof Download PDFInfo
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- CN109019781A CN109019781A CN201810924262.5A CN201810924262A CN109019781A CN 109019781 A CN109019781 A CN 109019781A CN 201810924262 A CN201810924262 A CN 201810924262A CN 109019781 A CN109019781 A CN 109019781A
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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
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
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- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The present invention relates to a kind of cement base composite carbon electrodes and the preparation method and application thereof, electrode includes composite material and the Pt-Bi that is carried on composite material, composite material includes following components and parts by weight content: 40-50 parts of cement, 25-35 parts of flyash, 10-20 parts of active carbon and 5-15 parts of graphite powder, also doped with graphene in composite material;When preparation, first prepare active carbon-graphene complex, then prepare muddy solids, later carry out cement conservation obtain composite material, finally by Pt-Bi load on the composite to get arrive cement base composite carbon electrode;Cement base composite carbon electrode is for the pollutant in sewage of degrading.Compared with prior art, electrode adhesion power of the present invention increases substantially, and extends service life, and difficult for biological degradation pollutant that can efficiently in fast degradation sewage, reduces the cost of electrode.
Description
Technical field
The invention belongs to technical field of sewage, it is related to a kind of cement base composite carbon electrode and preparation method thereof and answers
With.
Background technique
With the quickening of industrialization and urbanization process, municipal sewage mainly by the sanitary sewage containing high concentration N-P and
Trade effluent composition.Due to pollutant component complexity, not degradable, water quality has no longer been traditional " municipal wastewater ".Another party
Face, people are to water pollution problems pay attention to day by day, and especially since country in 2006 implements energy-saving and emission-reduction, government is to municipal sewage
More stringent requirements are proposed for treatment plant's effluent quality.China gradually comes into effect " urban wastewater treatment firm pollutant emission mark
It is quasi- " (GB18918-2002) level-one A standard.Currently, most of sewage treatment plant of China still uses oxidation ditch, A2/ O activity
The conventional methods such as Treatment of Sludge method, SBR method are only capable of that water quality is made to meet GB18918-2002 secondary standard, i.e. COD highest allows to arrange
Putting concentration (annual average) is 100mg/L;And be unable to satisfy GB18918-2002 level-one A standard or level-one B standard, i.e. COD highest
Allowing concentration of emission (annual average) is 50mg/L or 60mg/L.Therefore, Novel sewage processing technique is probed into, becomes people and increasingly closes
The emphasis of note.
Electrochemical method is high with its treatment effeciency, clean, feature without secondary pollution is favored by people, but excessive
Power consumption becomes one of an important factor for restricting its development.Therefore, in electrochemical degradation treatment process, in addition to operating condition
Except equipment, the selection of electrode is particularly important.Electrode needs to have good recyclability, reproducibility, adsorptivity, resistance to punching
The advantages that hitting load and efficient electrocatalysis, to reduce the consumption of electric energy in treatment process.
Existing electrode is in practical electrolytic process, the drawbacks such as that there are cohesive forces is inadequate, surfacing is easy to fall off, not only shadow
The degradation effect to dirty Organic substance in water is rung, and service life is shorter.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of cement base composite carbons
Electrode and the preparation method and application thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of cement base composite carbon electrode, the electrode include composite material and the Pt-Bi that is carried on composite material, institute
The composite material stated includes following components and parts by weight content: 40-50 parts of cement, 25-35 parts of flyash, 10-20 parts of active carbon
And 5-15 parts of graphite powder, also doped with graphene in the composite material.
The composite material includes following components and parts by weight content as a preferred technical solution: 45 parts of cement, powder
30 parts of coal ash, 15 parts of active carbon and 10 parts of graphite powder.
Further, the doping of the graphene is the 0.2-0.25% of composite material quality.
As a preferred technical solution, in the electrode, the mass ratio of Pt and composite material is (2-3) × 10-8: 1, preferably
2.2×10-8:1;The mass ratio of Bi and composite material is (6-7) × 10-8: 1, preferably 6.5 × 10-8:1。
Further, which further includes graphite paper, and the composite material is coated in the two sides of graphite paper.
Further, multiple holes are offered on the graphite paper.
A kind of preparation method of cement base composite carbon electrode, method includes the following steps:
1) active carbon-graphene complex is prepared, later by active carbon-graphene complex, cement, flyash, activity
Charcoal and graphite powder are added into water, obtain muddy solids after mixing;
2) muddy solids is coated in the two sides of graphite paper, cement conservation is carried out later, obtains composite material;
3) by Pt-Bi load on the composite to get arrive the cement base composite carbon electrode.
Further, in step 1), active carbon-graphene complex preparation process are as follows:
1-1) graphite oxide is added into water, active carbon is added after ultrasound, and be uniformly mixed;
It is 6.5-7.5 that hydrazine hydrate, which 1-2) is added, to pH, and solid is isolated after standing to get the active carbon-graphite is arrived
Alkene compound.
Further, in step 2), the cement conservation process carries out in concrete curing box, the concrete
Humidity in curing box is 85-95%, and temperature is 20-30 DEG C, and curing time is 2-4 days.
Further, in step 3), Pt-Bi is loaded on the composite using three-electrode system electrochemical deposition method.
A kind of application of cement base composite carbon electrode, the cement base composite carbon electrode is for the pollution in sewage of degrading
Object.
Present invention employs Pt-Bi binary metal nanometer particle load electrodes, using cement as binder, and utilize flyash
The cohesive force of cement is improved with graphene, so that electrode service life with higher;Graphite paper is punched, is made double
Face electrode is also beneficial to improve the fastness of electrode;The preferable adsorptivity of active carbon is utilized and graphite powder, graphene are preferable
Electric conductivity handles the waste water of difficult for biological degradation.
Compared with prior art, the invention has the characteristics that:
1) present invention is transformed existing electrode, adulterates a small amount of graphene, in the electrodes to further increase electrode
Cohesive force, finally prepare cement-fly ash-active carbon-graphene-graphite powder combination electrode, cohesive force is by original
0.16N is increased to 1N, and electrode adhesion power increases substantially, and extends service life, and can be efficiently in fast degradation sewage
Difficult for biological degradation pollutant reduces the cost of electrode;
2) in the present invention, active carbon has adsorption effect, and graphite powder is conductive, and the doping of graphene can not only mention
The cohesive force of high cement material, while can also have a degree of improvement to the capacitor of electrode, from 19.91Fcm-2It is increased to
30F·cm-2Left and right, can guarantee the degradation rate to organic matter.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of graphite paper in embodiment 1.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1:
The preparation step of cement base composite carbon electrode is as follows:
(1) graphite paper punches:
As shown in Figure 1, the aperture that 8 diameters are 5mm is uniformly bored on the graphite paper surface of 20mm × 40mm, it is two neighboring small
The distance between hole is 5mm, and aperture is 2.5mm at a distance from graphite paper edge.
(2) active carbon-graphene complex is prepared:
Graphite oxide is prepared using Hummers method is improved, and it is ultrasonic in deionized water to weigh a certain amount of graphite oxide
30min is added active carbon 100 times of graphite oxide quality (quality be), ultrasonic 2h later, stirs 6h so that graphite oxide with
Active carbon is sufficiently mixed;Hydrazine hydrate is added dropwise to pH value of solution close to 7.0, stands overnight, dries and saves after separation of solid and liquid.
(3) cement-fly ash-active carbon-graphene-graphite powder composite material is prepared:
It mixes, makes after weighing cement, flyash, active carbon, graphite powder and active carbon-graphene complex by weight ratio
Cement: flyash: active carbon: graphite powder=45:30:15:10, graphene account for the 0.2-0.25% of total content;Addition is gone in right amount
Ionized water is sufficiently stirred, until being mixed thoroughly.The muddy solids obtained in right amount is taken to suppress in the two sides of graphite paper,
So that surface coating is smooth, it is then placed into concrete curing box, is placed 3 days at humidity 90% and 25 DEG C of temperature,
Cement-fly ash-active carbon-graphene-graphite powder composite material is prepared, electrode effective area is 20 × 40mm, with a thickness of
2mm。
(4) cement-fly ash-active carbon-graphene-graphite powder composite carbon of electrochemical deposition method preparation supporting Pt-Bi
Electrode:
Using cement-fly ash-active carbon-graphene-stone of three-electrode system electrochemical deposition method preparation supporting Pt-Bi
Ink powder combination electrode, using the composite material of preparation as working electrode, platinum electrode is as auxiliary electrode, Ag/AgCl electrode conduct
Reference electrode, the H by 50mL containing 0.5g/L2PtCl6, 0.5mmol/L Bi (NO)3, 2g/L citric acid and 1%HNO3It is molten
Liquid is as deposition liquid, the electro-deposition 240s under -0.8V constant potential.The good electrode of electro-deposition is placed in air dry oven,
Cement-fly ash-active carbon-graphene-graphite powder composite carbon of supporting Pt-Bi can be obtained in the freeze-day with constant temperature 2d at 40 DEG C
Electrode, the capacitor of the electrode are 30Fcm-2, cohesive force is 1N or so, and electrode fastness, which has, to be increased substantially.
Using cement base composite carbon electrode fast degradation Methyl Orange in Wastewater manufactured in the present embodiment, process is as follows:
By three-electrode system electrochemical degradation methyl orange, using cement base composite carbon electrode as working electrode, it is with titanium net
Auxiliary electrode is 20mg/L's with 150mL concentration under the stirring of 150r/min revolving speed with Ag/AgCl (saturation) for reference electrode
Methyl orange solution is degradation object, and applying square wave current potential, [upper current potential (Eu) and lower current potential (El) are respectively 1.5V and -1.5V, are handed over
It is 1min for period (T), every 30min methyl orange concentration of spectrophotometric determination, degradation total time is 4h, methyl orange
Degradation rate be about 73%.
Embodiment 2:
A kind of cement base composite carbon electrode, the electrode include composite material and the Pt-Bi that is carried on composite material, multiple
Condensation material includes following components and parts by weight content: 40 parts of cement, 35 parts of flyash, 10 parts of active carbon and 15 parts of graphite powder, multiple
Also doped with graphene in condensation material, the doping of graphene is the 0.2% of composite material quality.
The electrode further includes graphite paper, and multiple holes are offered on graphite paper, and composite material is coated in the two sides of graphite paper.
The preparation method of the cement base composite carbon electrode, comprising the following steps:
1) active carbon-graphene complex is prepared, process is as follows:
1-1) graphite oxide is added into water, active carbon is added after ultrasound, and be uniformly mixed;
It is 7.5 that hydrazine hydrate, which 1-2) is added, to pH, and solid is isolated after standing to get active carbon-graphene complex is arrived.
Active carbon-graphene complex, cement, flyash, active carbon and graphite powder are added into water later, mixing is equal
Muddy solids is obtained after even;
2) muddy solids is coated in the two sides of graphite paper, cement conservation is carried out later, in concrete curing box
Cement conservation is carried out, the humidity in concrete curing box is 85%, and temperature is 30 DEG C, and curing time is 2 days, obtains composite wood
Material;
3) Pt-Bi is loaded on the composite to get compound to cement base using three-electrode system electrochemical deposition method
Carbon electrode.
The cement base composite carbon electrode is for the pollutant in sewage of degrading.
Embodiment 3:
A kind of cement base composite carbon electrode, the electrode include composite material and the Pt-Bi that is carried on composite material, multiple
Condensation material includes following components and parts by weight content: 50 parts of cement, 25 parts of flyash, 20 parts of active carbon and 5 parts of graphite powder, compound
Also doped with graphene in material, the doping of graphene is the 0.25% of composite material quality.
The electrode further includes graphite paper, and multiple holes are offered on graphite paper, and composite material is coated in the two sides of graphite paper.
The preparation method of the cement base composite carbon electrode, comprising the following steps:
1) active carbon-graphene complex is prepared, process is as follows:
1-1) graphite oxide is added into water, active carbon is added after ultrasound, and be uniformly mixed;
It is 6.5 that hydrazine hydrate, which 1-2) is added, to pH, and solid is isolated after standing to get active carbon-graphene complex is arrived.
Active carbon-graphene complex, cement, flyash, active carbon and graphite powder are added into water later, mixing is equal
Muddy solids is obtained after even;
2) muddy solids is coated in the two sides of graphite paper, cement conservation is carried out later, in concrete curing box
Cement conservation is carried out, the humidity in concrete curing box is 95%, and temperature is 20 DEG C, and curing time is 4 days, obtains composite wood
Material;
3) Pt-Bi is loaded on the composite to get compound to cement base using three-electrode system electrochemical deposition method
Carbon electrode.
The cement base composite carbon electrode is for the pollutant in sewage of degrading.
Embodiment 4:
A kind of cement base composite carbon electrode, the electrode include composite material and the Pt-Bi that is carried on composite material, multiple
Condensation material includes following components and parts by weight content: 45 parts of cement, 30 parts of flyash, 15 parts of active carbon and 10 parts of graphite powder, multiple
Also doped with graphene in condensation material, the doping of graphene is the 0.22% of composite material quality.
The electrode further includes graphite paper, and multiple holes are offered on graphite paper, and composite material is coated in the two sides of graphite paper.
The preparation method of the cement base composite carbon electrode, comprising the following steps:
1) active carbon-graphene complex is prepared, process is as follows:
1-1) graphite oxide is added into water, active carbon is added after ultrasound, and be uniformly mixed;
It is 7 that hydrazine hydrate, which 1-2) is added, to pH, and solid is isolated after standing to get active carbon-graphene complex is arrived.
Active carbon-graphene complex, cement, flyash, active carbon and graphite powder are added into water later, mixing is equal
Muddy solids is obtained after even;
2) muddy solids is coated in the two sides of graphite paper, cement conservation is carried out later, in concrete curing box
Cement conservation is carried out, the humidity in concrete curing box is 90%, and temperature is 25 DEG C, and curing time is 3 days, obtains composite wood
Material;
3) Pt-Bi is loaded on the composite to get compound to cement base using three-electrode system electrochemical deposition method
Carbon electrode.
The cement base composite carbon electrode is for the pollutant in sewage of degrading.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of cement base composite carbon electrode, which is characterized in that the electrode includes composite material and is carried on composite material
Pt-Bi, the composite material includes following components and parts by weight content: 40-50 parts of cement, 25-35 parts of flyash, activity
10-20 parts of charcoal and 5-15 parts of graphite powder, also doped with graphene in the composite material.
2. a kind of cement base composite carbon electrode according to claim 1, which is characterized in that the composite material include with
Lower component and parts by weight content: 45 parts of cement, 30 parts of flyash, 15 parts of active carbon and 10 parts of graphite powder.
3. a kind of cement base composite carbon electrode according to claim 1, which is characterized in that the doping of the graphene
For the 0.2-0.25% of composite material quality.
4. a kind of cement base composite carbon electrode according to claim 1, which is characterized in that the electrode further includes graphite paper,
The composite material is coated in the two sides of graphite paper.
5. a kind of cement base composite carbon electrode according to claim 4, which is characterized in that offered on the graphite paper
Multiple holes.
6. a kind of preparation method of such as cement base composite carbon electrode described in any one of claim 1 to 5, which is characterized in that should
Method the following steps are included:
1) prepare active carbon-graphene complex, later by active carbon-graphene complex, cement, flyash, active carbon and
Graphite powder is added into water, obtains muddy solids after mixing;
2) muddy solids is coated in the two sides of graphite paper, cement conservation is carried out later, obtains composite material;
3) by Pt-Bi load on the composite to get arrive the cement base composite carbon electrode.
7. a kind of preparation method of cement base composite carbon electrode according to claim 6, which is characterized in that in step 1),
Active carbon-graphene complex preparation process are as follows:
1-1) graphite oxide is added into water, active carbon is added after ultrasound, and be uniformly mixed;
It is 6.5-7.5 that hydrazine hydrate, which 1-2) is added, to pH, and solid is isolated after standing to get multiple to the active carbon-graphene
Close object.
8. a kind of preparation method of cement base composite carbon electrode according to claim 6, which is characterized in that in step 2),
The cement conservation process carries out in concrete curing box, and the humidity in the concrete curing box is 85-95%, temperature
Degree is 20-30 DEG C, and curing time is 2-4 days.
9. a kind of preparation method of cement base composite carbon electrode according to claim 6, which is characterized in that in step 3),
Pt-Bi is loaded on the composite using three-electrode system electrochemical deposition method.
10. a kind of application of such as cement base composite carbon electrode described in any one of claim 1 to 5, which is characterized in that described
Cement base composite carbon electrode is for the pollutant in sewage of degrading.
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CN110963551A (en) * | 2019-11-26 | 2020-04-07 | 西安建筑科技大学 | Preparation method of graphene inorganic polymer composite electrode |
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