CN109110756A - Derivative carbon electrode material of a kind of homogeneous corncob and preparation method thereof - Google Patents
Derivative carbon electrode material of a kind of homogeneous corncob and preparation method thereof Download PDFInfo
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- CN109110756A CN109110756A CN201811239964.6A CN201811239964A CN109110756A CN 109110756 A CN109110756 A CN 109110756A CN 201811239964 A CN201811239964 A CN 201811239964A CN 109110756 A CN109110756 A CN 109110756A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses derivative carbon electrode material of a kind of homogeneous corncob for supercapacitor and preparation method thereof, this method realizes the homogeneous preparation of the derivative charcoal particle of corncob using screening pre-selection and subsequent carbonization-activation.Specific step of preparation process is as follows: first crushing biomass corncob, the corncob powder particle with different particle size distribution range, and high temperature carbonization are obtained by screening；Then use activator by gained carbonized material powder particle high-temperature activation；Finally by product pickling, the drying after activation, the derivative carbon electrode material of homogeneous corncob is obtained.When the derivative carbon electrode material of homogeneous corncob of the invention is used as electrode material for super capacitor, high specific capacitance and high rate performance are shown.The features such as this method has simple process, and abundant raw materials are environmental-friendly, and added value is higher.
Description
Technical field
The present invention relates to a kind of biomass derived carbon electrode material and preparation method thereof more particularly to a kind of homogeneous corncobs
Derivative carbon electrode material and preparation method thereof；Belong to new energy materials field.
Background technique
With the increasingly failure of fossil energy and being on the rise for environmental pollution, biomass derived charcoal super capacitor electrode
Material, the favor due to the features such as raw material sources are extensive, low in cost, renewable, pollution-free by vast researcher.
Biomass corncob abundance, hole are flourishing, are prepared as active carbon and not only reduce to be abandoned or directly
Burning bring environmental pollution is connect, while being also converted into high performance electrode material for super capacitor, corncob is become
Waste be changed into values, improves its added value, realizes utilization of resources.Qu et al. (Bioresource Technology, 2015,
The porous charcoal that high added value 189:285-291) is obtained by a step steam activation corncob residue, in the scanning speed of 5mV/s
Under rate, specific capacitance is up to 314 F/g, and under the high sweep speed of 100 mV/s, capacitor still retains 259 F/g.Specific capacitance conservation rate
Up to 82%, there is excellent high rate performance.Li et al. people (Journal of Materials Chemistry A, 2017,5:
3875-3887) corncob is handled using the concentrated sulfuric acid first, carbonization at high temperature is then mixed with melamine and is situated between
Hole charcoal, under the current density of 1 A/g, specific capacity is up to 538 F/g.Equally, the derivative charcoal of the corncob shows excellent electricity
Chemical property.
Although the derivative charcoal of corncob shows good supercapacitor chemical property, but is obtaining high-performance corn
When the derivative porous activated carbon of core, all to corncob carried out cumbersome pretreatment (being handled as obtained corncob residue or acid) or
Modified (as melamine is added), therefore a kind of high efficiency preparation method of simple biomass corncob electrode material is found to life
The significant science of the development of substance corncob electrode material and social value.
Summary of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned existing technology of preparing, a kind of simple, safety homogeneous is provided
Corncob derives carbon electrode material preparation method.It is well known that corncob is mainly by cellulose, hemicellulose, lignin three
Kind at being grouped as, and the microstructure of these three ingredients is completely different, thus in order to obtain equal activated carbon before
Mention is using the more uniform corncob of ingredient as presoma.It is more uniform to obtain ingredient to generally use electroplating effluent recycling
Corncob presoma, then carbonization-activation obtains the absorbent charcoal material of better performances, and has good consistency, but should
The waste liquid that method generates will cause environmental pollution.In addition, cellulose, hemicellulose, lignin are due to microstructure in corncob
Difference, so their mechanical strength is also different, when crushing, heterogeneity part will form different size of particle.
Therefore, the present invention develops the corncob presoma that a kind of simple physics sieve method can be readily available homogeneous, in turn
Overcome this defect of homogeneous corncob presoma difficulty acquisition.
When the derivative carbon electrode material of the corncob of this method preparation is used as electrode material for super capacitor, since micro-structure is equal
It is even consistent, show excellent chemical property.This method has apparatus and process simple, and low production cost is environmental-friendly, can
The features such as large-scale production.It is specific the preparation method is as follows:
Step 1, by the biomass corncob cleaning of collection, dry, crushing, being obtained using the sieve screening of different meshes is had
The corncob powder particle of different particle size distribution range；
Biomass corn cob granule after screening is put into tube furnace by step 2, is carbonized, is carbonized in nitrogen atmosphere high temperature
Material；
Carbonized material is mixed from activator by different mass ratioes, is fully ground, activates in nitrogen atmosphere high temperature by step 3,
Obtain activation products；
Gained activation products are impregnated using different acid solutions, are then alternately cleaned with deionized water and alcohol, most by step 4
It is dry in 50~150 DEG C of drying boxes afterwards, obtain the derivative carbon electrode material of homogeneous corncob.
The derivative carbon electrode material microstructure of gained homogeneous corncob is uniform, especially state of distribution of pores, active carbon particle
Particle size distribution is uniform.
The mesh number of sieve described in step 1 is 10 mesh~400 mesh, the particle size distribution range 0.03 of corncob powder particle
Mm~2mm.
The heating rate of high temperature cabonization described in step 2 is 3~20 DEG C/min, and carbonization temperature is 600~1000 DEG C,
Soaking time is 1~24 h.
The mass ratio of carbonized material described in step 3 and activator is 1:1~1:6, the heating rate of high-temperature activation is 3~
20 DEG C/min, activation temperature is 600~1000 DEG C, and soaking time is 1~24 h.
Activator described in step 3 is potassium hydroxide, sodium hydroxide, zinc chloride, magnesium chloride one or more of them.Institute
The activating agent of selection can be chosen according to particle size distribution, can obtain the performance more preferably derivative charcoal super capacitor of corncob
Device electrode material.
Acid solution described in step 4 is hydrochloric acid or sulfuric acid, and concentration is the M of 1 M~6, and soaking time is 1~24 h.According to
Selected activator is different, chooses different acid, can obtain the performance more preferably derivative charcoal super capacitor electrode material of corncob.
The invention has the benefit that
1. the present invention obtains the corncob presoma of homogeneous by simple physics sieve method, and then realizes homogeneous corncob
The preparation of derivative carbon electrode material overcomes conventional chemistry and obtains this defect of homogeneous corncob forerunner's body pollution environment.
2. homogeneous corncob prepared by the present invention derives carbon electrode material, since the ingredient of presoma used is more uniform
Unanimously, therefore during subsequent carbonization-activation, the active carbon that degree of carbonization and activation degree more uniform can be obtained
Particle.
3. homogeneous corncob prepared by the present invention derive carbon electrode material, since micro-structure is more uniform, with
When making electrode material for super capacitor, in electrochemical reaction process, each charcoal particle can be made full use of to carry out energy storage.
4. abundant raw materials selected by the present invention, preparation process is simple, and cost is relatively low, clean and environmental protection, it is easy to accomplish produces
Industry.
Make furtherly below with reference to technical effect of the attached drawing to design of the invention, specific material structure and generation
It is bright, to fully understand the purposes, features and effects of the present invention.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) of the derivative carbon electrode material of homogeneous corncob prepared by the embodiment of the present invention 1
Figure.
Fig. 2 is the pore size distribution curve figure of the derivative carbon electrode material of homogeneous corncob prepared by the embodiment of the present invention 1.
It in current density is 0.5-5A/g that Fig. 3, which is the derivative carbon electrode material of homogeneous corncob prepared by the embodiment of the present invention 1,
Under constant current charge-discharge curve.
Fig. 4 is the high rate performance figure of the derivative carbon electrode material of homogeneous corncob prepared by the embodiment of the present invention 1.
Fig. 5 is the scanning electron microscope (SEM) of the derivative carbon electrode material of homogeneous corncob prepared by the embodiment of the present invention 2
Figure.
Specific embodiment
The present invention is described in further detail the content of present invention in conjunction with Figure of description, but the application by embodiment
It is not limited to these embodiments.
Embodiment 1
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 10~18 mesh；By gained jade
Rice core powder particle is transferred to tube furnace, is heated to 800 DEG C of 2 h of heat preservation in nitrogen atmosphere with the heating rate of 5 DEG C/min, into
Row charing process；Gained carbonized material is mixed with KOH 1:3 in mass ratio, is fully ground, with 5 DEG C/min's in nitrogen atmosphere
Heating rate is heated to 800 DEG C of 2 h of heat preservation, obtains activation products；Gained activation products are soaked using the HCl solution of 1 mol/L
Bubble is then alternately cleaned with deionized water and alcohol, finally dry in 60 DEG C of drying boxes, obtains the derivative charcoal of homogeneous corncob
Electrode material.
Scanning electron microscope (SEM) figure of the derivative carbon electrode material of obtained homogeneous corncob is as shown in Figure 1, by Fig. 1
Know that prepared active carbon electrode material microstructure is all relatively uniform consistent with granular size.Fig. 2 is prepared homogeneous
The pore size distribution curve figure of the derivative carbon electrode material of corncob, it can be seen that prepared active carbon has relatively narrow pore-size distribution
Range shows that the active carbon has more uniform pore-size distribution.By the electrode material, binder and conductive charcoal according to
It is coated on nickel foam (1 × 1 cm) after the ratio grinding uniformly of 80:10:10 and (70 DEG C) is dried, working electrode is made,
(platinized platinum is used as to electrode, and Ag/AgCl electrode is as reference electrode, and the aqueous sodium persulfate solution of 1 M is as electrolysis under three-electrode system
Liquid), test can be carried out to its electrochemistry.For the electrode when current density is 0.5A/g, specific capacitance value is 108 F/g；Work as electricity
When current density is 5 A/g, specific capacitance value is 99 F/g, specific capacity conservation rate up to 91.7%, show superior times it is forthright
Energy.
Embodiment 2
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 170~200 mesh；By gained
Corncob powder particle is transferred to tube furnace, is heated to 600 DEG C of heat preservations 24 in nitrogen atmosphere with the heating rate of 20 DEG C/min
H carries out charing process；Gained carbonized material is mixed with KOH 1:1 in mass ratio, is fully ground, in nitrogen atmosphere with 10 DEG C/
The heating rate of min is heated to 1000 DEG C of 12 h of heat preservation, obtains activation products；By gained activation products using 6 mol/L's
HCl solution impregnates, and is then alternately cleaned with deionized water and alcohol, finally dry in 150 DEG C of drying boxes, obtains homogeneous jade
The derivative carbon electrode material of rice core.
Scanning electron microscope (SEM) figure of the derivative carbon electrode material of obtained homogeneous corncob is as shown in figure 5, by Fig. 5
Know that prepared active carbon electrode material microstructure is all relatively uniform consistent with granular size.
Embodiment 3
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 325~400 mesh；By gained
Corncob powder particle is transferred to tube furnace, is heated to 1000 DEG C of heat preservations 1 in nitrogen atmosphere with the heating rate of 3 DEG C/min
H carries out charing process；Gained carbonized material is mixed with KOH 1:6 in mass ratio, is fully ground, in nitrogen atmosphere with 20 DEG C/
The heating rate of min is heated to 600 DEG C of 24 h of heat preservation, obtains activation products；Gained activation products are used to the HCl of 3 mol/L
Solution impregnates, and is then alternately cleaned with deionized water and alcohol, finally dry in 50 DEG C of drying boxes, obtains homogeneous corncob
Derivative carbon electrode material.
Embodiment 4
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 10~18 mesh；By gained jade
Rice core powder particle is transferred to tube furnace, is heated to 800 DEG C of 2 h of heat preservation in nitrogen atmosphere with the heating rate of 10 DEG C/min,
Carry out charing process；Gained carbonized material is mixed with NaOH 1:3 in mass ratio, is fully ground, in nitrogen atmosphere with 5 DEG C/
The heating rate of min is heated to 800 DEG C of 2 h of heat preservation, obtains activation products；Gained activation products are used to the H of 1 mol/L2SO4
Solution impregnates, and is then alternately cleaned with deionized water and alcohol, finally dry in 60 DEG C of drying boxes, obtains homogeneous corncob
Derivative carbon electrode material.
Embodiment 5
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 10~18 mesh；By gained jade
Rice core powder particle is transferred to tube furnace, is heated to 800 DEG C of 2 h of heat preservation in nitrogen atmosphere with the heating rate of 5 DEG C/min, into
Row charing process；By gained carbonized material and ZnCl21:3 in mass ratio mixing, be fully ground, in nitrogen atmosphere with 10 DEG C/
The heating rate of min is heated to 800 DEG C of 2 h of heat preservation, obtains activation products；Gained activation products are used to the HCl of 1 mol/L
Solution impregnates, and is then alternately cleaned with deionized water and alcohol, finally dry in 60 DEG C of drying boxes, obtains homogeneous corncob
Derivative carbon electrode material.
Embodiment 6
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 10~18 mesh；By gained jade
Rice core powder particle is transferred to tube furnace, is heated to 800 DEG C of 2 h of heat preservation in nitrogen atmosphere with the heating rate of 5 DEG C/min, into
Row charing process；By gained carbonized material and MgCl2The mixing of 1:3 in mass ratio, is fully ground, with 5 DEG C/min in nitrogen atmosphere
Heating rate be heated to 800 DEG C of 2 h of heat preservation, obtain activation products；Gained activation products are used to the HCl solution of 1 mol/L
It impregnates, is then alternately cleaned with deionized water and alcohol, it is finally dry in 60 DEG C of drying boxes, it is derivative to obtain homogeneous corncob
Carbon electrode material.
Embodiment 7
By the corncob cleaning of collection, dry, crushing, screening obtains corncob powder particle between 10~18 mesh；By gained jade
Rice core powder particle is transferred to tube furnace, is heated to 800 DEG C of 2 h of heat preservation in nitrogen atmosphere with the heating rate of 5 DEG C/min, into
Row charing process；By gained carbonized material and KOH and MgCl2The mixing of 1:3 in mass ratio, is fully ground, with 5 in nitrogen atmosphere
DEG C/heating rate of min is heated to 800 DEG C of 2 h of heat preservation, obtain activation products；By gained activation products using 1 mol/L's
HCl solution impregnates, and is then alternately cleaned with deionized water and alcohol, finally dry in 60 DEG C of drying boxes, obtains homogeneous corn
Core derives carbon electrode material.
Claims (8)
1. a kind of preparation method of the derivative carbon electrode material of homogeneous corncob, characterized in that it comprises the following steps:
Step 1, by the biomass corncob cleaning of collection, dry, crushing, being obtained using the sieve screening of different meshes is had
The corncob powder particle of different particle size distribution range；
Biomass corn cob granule after screening is put into tube furnace by step 2, is carbonized, is carbonized in nitrogen atmosphere high temperature
Material；
Carbonized material is mixed from activator by different mass ratioes, is fully ground, activates in nitrogen atmosphere high temperature by step 3,
Obtain activation products；
Gained activation products are impregnated using different acid solutions, are then alternately cleaned with deionized water and alcohol, most by step 4
It is dry in 50~150 DEG C of drying boxes afterwards, obtain the derivative carbon electrode material of homogeneous corncob.
2. preparation method according to claim 1, it is characterised in that: the derivative carbon electrode material of gained homogeneous corncob is microcosmic
Structure is uniform, and active carbon particle particle size distribution is uniform.
3. preparation method according to claim 1, it is characterised in that: the mesh number of sieve described in step 1 be 10 mesh~
400 mesh, 0.03 mm of particle size distribution range~2mm of corncob powder particle.
4. preparation method according to claim 1, it is characterised in that: the heating rate of high temperature cabonization described in step 2 is
3~20 DEG C/min, carbonization temperature is 600~1000 DEG C, and soaking time is 1~24 h.
5. preparation method according to claim 1, it is characterised in that: the quality of carbonized material described in step 3 and activator
Than being 3~20 DEG C/min for the heating rate of 1:1~1:6, high-temperature activation, activation temperature is 600~1000 DEG C, soaking time
For 1~24 h.
6. preparation method according to claim 1, it is characterised in that: activator described in step 3 is potassium hydroxide, hydrogen
Sodium oxide molybdena, zinc chloride, magnesium chloride one or more of them.
7. preparation method according to claim 1, it is characterised in that: acid solution described in step 4 be hydrochloric acid or sulfuric acid,
Concentration is the M of 1 M~6, and soaking time is 1~24 h.
8. the derivative carbon electrode material of homogeneous corncob according to claim 2, it is characterised in that: the microstructure is hole
Distribution.
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Cited By (6)
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| CN110165234A (en) * | 2019-05-22 | 2019-08-23 | 广州大学 | A kind of corncob electrode material and its preparation method and application |
| CN111924842A (en) * | 2020-08-17 | 2020-11-13 | 四川轻化工大学 | Lotus stalk-based electrode material and preparation method thereof |
| CN113845116A (en) * | 2021-09-16 | 2021-12-28 | 安徽理工大学 | Method for preparing electromagnetic wave absorbing material based on corncobs |
| CN109809403B (en) * | 2019-03-18 | 2022-04-26 | 中国药科大学 | Preparation method and application of biogas residue-based activated carbon with high adsorption performance |
| CN115424870A (en) * | 2022-08-30 | 2022-12-02 | 南昌工程学院 | Biomass-derived carbon material and preparation method and application thereof |
| CN116272855A (en) * | 2022-12-21 | 2023-06-23 | 华南理工大学 | Wood pulp derived carbon and zirconium hydrogen phosphate mixed adsorption material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809403B (en) * | 2019-03-18 | 2022-04-26 | 中国药科大学 | Preparation method and application of biogas residue-based activated carbon with high adsorption performance |
| CN110165234A (en) * | 2019-05-22 | 2019-08-23 | 广州大学 | A kind of corncob electrode material and its preparation method and application |
| CN111924842A (en) * | 2020-08-17 | 2020-11-13 | 四川轻化工大学 | Lotus stalk-based electrode material and preparation method thereof |
| CN113845116A (en) * | 2021-09-16 | 2021-12-28 | 安徽理工大学 | Method for preparing electromagnetic wave absorbing material based on corncobs |
| CN115424870A (en) * | 2022-08-30 | 2022-12-02 | 南昌工程学院 | Biomass-derived carbon material and preparation method and application thereof |
| CN116272855A (en) * | 2022-12-21 | 2023-06-23 | 华南理工大学 | Wood pulp derived carbon and zirconium hydrogen phosphate mixed adsorption material and preparation method and application thereof |
| CN116272855B (en) * | 2022-12-21 | 2023-12-29 | 华南理工大学 | Wood pulp derived carbon and zirconium hydrogen phosphate mixed adsorption material and preparation method and application thereof |
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