CN108198696B - The preparation method and applications of porous carbon materials - Google Patents
The preparation method and applications of porous carbon materials Download PDFInfo
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- CN108198696B CN108198696B CN201711452620.9A CN201711452620A CN108198696B CN 108198696 B CN108198696 B CN 108198696B CN 201711452620 A CN201711452620 A CN 201711452620A CN 108198696 B CN108198696 B CN 108198696B
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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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- 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
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention provides a kind of preparation method of porous carbon materials, comprising the following steps: (1) cellulose fibre is impregnated 30-60min in the liquor zinci chloridi of 5wt%-40wt%, make the dissolution of partial fiber surface of cellulose fibre；(2) it after solidifying a moment in deionized water, is put into drying device and is dried；(3) it is carbonized using argon gas as protective atmosphere.Present invention firstly provides completely new process, that is, selective surface's dissolution methods using a kind of simple possible, high temperature cabonization again after being pre-processed to cellulose fibre, it is studied by the influence to various process parameters to pore structure and chemical property, obtain optimal procedure parameters, the porous active carbon material of bigger serface, abundant pore structure is prepared, it is prepared into supercapacitor as absolute electrode material (not needing to dose conductive agent and binder), specific capacitance can reach 488F/g, considerably beyond existing similar supercapacitor, have a extensive future.
Description
Technical field
The invention belongs to electrode material technical fields, and in particular to a kind of preparation method and applications of porous carbon materials.
Background technique
Supercapacitor is received more and more attention as the energy storage device haveing excellent performance, and has been applied to new energy vapour
Vehicle, rail traffic charging equipment, portable electronic product etc..Active carbon is the electrode material of most widely used supercapacitor
Material, it has the advantages that, and light-weight, from a wealth of sources, cheap, specific surface area is larger, good conductivity.
The specific surface area and pore structure of electrode material for super capacitor are to influence the principal element of capacitor chemical property,
Existing active carbon pore structure is relatively simple (based on micropore), although the not small (1400m of its specific surface area2/ g), but it is a large amount of
Micropore is diffused with sizable inhibition, therefore super electricity of this active carbon as electrode material to the ion in electrolyte
The specific capacitance of container is not high, and the specific capacitance of the existing supercapacitor as electrode material that uses active carbon is in the market
175F/G。
In general the preparation process of active carbon includes activation process and carbonisation.Activation process is prepared by active carbon
In journey the step of most critical, in activation process, the pore structure of absorbent charcoal material is formed, and specific surface area increases.It is more general at present
It is to be carried out in acid or aqueous slkali to wood material, coal measures raw material, petroleum or Plastic raw material all over the activation process used
High temperature (more than 600 DEG C) activation, this method need to consume during the preparation process a large amount of acid-base reagents and the energy, the active carbon of preparation
It needs to dose and could be used as electrode material after conductive agent and binder, make that the production cost increases and pollutes the environment.Mesh
The maximum specific capacitance of high-temperature activation and the obtained active carbon that is carbonized is used in preceding document report for 100-250F/g, although specific capacitance
It improves, but still can not effectively control the formation of pore structure, for pore structure still based on micropore, structure is more single
One.
Summary of the invention
At high cost for existing absorbent charcoal material preparation process, there are environmental pollutions, and pore structure is single, as electrode material
The lower above problem of super capacitor specific capacitance of preparation, the present invention provide a kind of preparation method of porous carbon materials, adopt for the first time
The preceding pretreatment that is carbonized is carried out with selective surface's dissolution method, the porous active carbon of bigger serface, abundant pore structure is prepared
Material is prepared into supercapacitor as absolute electrode material (not needing to dose conductive agent and binder), and specific capacitance is reachable
To 488F/g.
One aspect of the present invention provides a kind of preparation method of porous carbon materials, comprising the following steps: (1) by cellulose fibre
30-60min is impregnated in the liquor zinci chloridi of 5wt%-40wt%, makes the dissolution of partial fiber surface of cellulose fibre；(2) go from
After solidifying a moment in sub- water, it is put into drying device and is dried；(3) it is carbonized using argon gas as protective atmosphere.
Further, cellulose fibre is impregnated 60min in the liquor zinci chloridi of 40wt% by the step (1).
Further, (2) 80 DEG C of the step dry 2h.
Further, (3) 650 DEG C of carbonization 2h of the step.
Further, the step (3) is carbonized using vacuum tube furnace.
Another aspect of the present invention also provides application of the above-mentioned porous carbon materials as electrode material.
Further, ultracapacitor device is made directly as two electrodes of button cell in porous carbon materials.
Further, by porous carbon materials and metal oxide or the compound obtained electrode material of conducting polymer, it is used for method
Draw fake capacitance supercapacitor.
The present invention also provides a kind of supercapacitor, which includes porous active carbon electrode, the porous work
Property carbon electrode material be claim 1 prepare porous carbon materials.
Above-mentioned porous carbon materials are also used as adsorbent material or catalyst carrier.
Present invention firstly provides completely new process, that is, selective surface's dissolution methods using a kind of simple possible, to fiber
High temperature cabonization again after cellulose fiber is pre-processed passes through the influence to various process parameters to pore structure and chemical property and carries out
Research, obtains optimal procedure parameters, the porous active carbon material of bigger serface, abundant pore structure is prepared, as only
Vertical electrode material (not needing to dose conductive agent and binder) is prepared into supercapacitor, and specific capacitance can reach 488F/g, much
More than existing similar supercapacitor, have a extensive future；Can have by adjusting liquor zinci chloridi concentration and soaking time
The formation of effect control pore structure；Preparation process does not need to consume a large amount of acid-base reagents and the energy, environmental-friendly；The porous carbon materials
It is widely used, it is alternatively arranged as adsorbent material and is adsorbed for liquid phase, or as catalyst carrier.
Detailed description of the invention
Fig. 1 is the porous carbon materials XRD diffraction pattern of embodiment 1-4 preparation；
Fig. 2 is the Raman spectrum of the porous carbon materials of embodiment 1-4 preparation；
Fig. 3 is the nitrogen Adsorption and desorption isotherms of the porous carbon materials of embodiment 1-6 preparation；
Fig. 4 is the specific surface area of the porous carbon materials of embodiment 1-6 preparation；
Fig. 5 is the porous carbon materials of embodiment 1-6 preparation using DFT as the graph of pore diameter distribution of model；
Fig. 6 is the scanning electron microscope (SEM) photograph of the porous carbon materials of embodiment 1-4 preparation；
Fig. 7 is the schematic diagram of selective surface's dissolution method.
In above-mentioned each figure, CF-0 indicates that the concentration of liquor zinci chloridi is 0；CF5-30 indicates that the concentration of liquor zinci chloridi is
5wt%, soaking time 30min；CF10-30 indicates that the concentration of liquor zinci chloridi is 10wt%, soaking time 30min；
CF20-30 indicates that the concentration of liquor zinci chloridi is 20wt%, soaking time 30min；CF40-30 indicates the dense of liquor zinci chloridi
Degree is 40wt%, soaking time 30min；CF10-60 indicates that the concentration of liquor zinci chloridi is 10wt%, and soaking time is
60min；CF40-60 indicates that the concentration of liquor zinci chloridi is 40wt%, soaking time 60min.
Specific embodiment
Combined with specific embodiments below and attached drawing is described in further details the present invention.
Embodiment 1-6 is the preparation of porous carbon materials, and embodiment 7 and 8 is the application of porous carbon materials.
Embodiment 1
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 5wt%, soaking time has
30 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 2
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 10wt%, soaking time has
30 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 3
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 20wt%, soaking time has
30 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 4
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 40wt%, soaking time has
30 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 5
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 10wt%, soaking time has
60 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 6
Filtering paper fiber (content of cellulose 90%) is impregnated using the liquor zinci chloridi of 40wt%, soaking time has
60 minutes, make the dissolution of partial fiber surface of cellulose fibre, after solidifying a moment in deionized water, is put into 650 DEG C of drying boxes
It is dried.Carbonisation carries out in 650 DEG C of vacuum tube furnace, and using argon gas as protective atmosphere, carbonization time is 2 small
When.Porous active carbon material is obtained after carbonization.
Embodiment 7
The present embodiment provides a kind of electric double layer super capacitor, the capacitor include button cell top cover, wave washer, gasket,
To electrode 1, diaphragm, to electrode 2, polypropylene seal pad and button cell box, to electrode 1 and to electrode 2 by identical in quality two
Part porous carbon materials are made under the premise of not dosing conductive agent and binder, and the diaphragm between two pairs of electrodes uses glass
Tunica fibrosa.
Embodiment 8
The present embodiment provides a kind of Faraday pseudo-capacitance supercapacitor, the electrode material of the capacitor is made by embodiment 6
Standby porous carbon materials and metal oxide or conducting polymer are compound obtained.
Detection and analysis
One, XRD diffraction is carried out to the material of embodiment 1-4 preparation, Fig. 1 is XRD diffraction pattern.The sample after high-temperature process
The XRD diffraction pattern of product shows the characteristic diffraction peak (002), (100) and (101) of carbon, shows the fiber after high-temperature process
Element is carbonized.
Two, the active carbon material of embodiment 1-4 preparation carries out Raman detection, and Raman spectrum is as shown in Figure 2.Raman spectrum is aobvious
Showing increases to 40%, I from 5% with solution concentrationD/IGAlso it correspondinglys increase, defect increases in sample, it should be due to selectivity
Caused by surface dissolution method causes micropore to increase.
Three, Fig. 3 is the nitrogen Adsorption and desorption isotherms of the active carbon material of embodiment 1-6 preparation；Fig. 4 is embodiment 1-6 system
Standby sample specific surface area, showing increases to 40% from 5% with solution concentration, and specific surface area significantly improves.From Fig. 3 and Fig. 4
It can be seen that the specific surface area ratio CF40-30's of CF40-60 is small, but the chemical property of CF40-60 is more preferable, because there is one
The effect for dividing micropore not have adsorption charge.
Four, Fig. 5 be using DFT as the sample graph of pore diameter distribution of model, Fig. 5 is shown as solution concentration increases, produce with
Based on micropore (aperture is less than 2 nanometers), the hierarchical porous structure of mesoporous (aperture is 2-50 nanometers) is had concurrently.
Five, Fig. 6 is the scanning electron microscopic picture of the porous carbon materials of embodiment 1-4 preparation, and Fig. 6 shows porous carbon materials
Microscopic appearance, it was confirmed that the presence of hierarchical porous structure.
By characterizing above, it was demonstrated that the available hierarchical porous structure abundant of method dissolved by selective surface, it is former
Reason figure is as shown in Figure 7.By being soaked for a period of time in the liquor zinci chloridi of certain solution concentration, the outer layer quilt of cellulose fibre
It is partly dissolved, by deionized water solidification, two fiber types element is recrystallized between residual fiber cellulose fiber
(Cellulose II) and interfibrous " bridge-type " membrane structure is formed, in the forming process of this membrane structure, on surface
Numerous micropores or mesoporous can be generated, are carbonized to cellulose fibre, this structure is still remained behind well, to be formed
The porous active carbon material of bigger serface, abundant pore structure, electrochemical property test show that material pore structure abundant has
Conducive to the quick diffusion and transmission of electrolyte ion when supercapacitor charge and discharge.
Six, by the immersion treatment before carbonization, the specific surface area of carbon material is significantly improved, from 244g/cm3(without chlorination
Zinc solution impregnates) it is increased to 1884g/cm3(embodiment 4), the specific surface area than Kuraray (Kurary) active carbon improve
35%.Seven, the carbon material prepared with embodiment 6 is that the specific capacitance for the button-shaped supercapacitor being made into electrode material is reachable
To 488F/g, the specific capacitance (175F/g) than Kurary activity charcoal super capacitor improves 179%.
Claims (9)
1. a kind of preparation method of porous carbon materials, which comprises the following steps: (1) cellulose fibre exists
60min is impregnated in the liquor zinci chloridi of 40wt%, makes the dissolution of partial fiber surface of cellulose fibre, the cellulose fibre is filtering
Paper fiber, the content of cellulose of the cellulose fibre are 90%；(2) after solidifying a moment in deionized water, it is put into drying
It is dried in device；(3) it is carbonized using argon gas as protective atmosphere.
2. preparation method according to claim 1, which is characterized in that (2) 80 DEG C of the step dry 2h.
3. preparation method according to claim 1, which is characterized in that (3) 650 DEG C of carbonization 2h of the step.
4. preparation method according to claim 3, which is characterized in that the step (3) is carbonized using vacuum tube furnace.
5. the application of porous carbon materials prepared by claim 1 as electrode material.
6. application according to claim 5, which is characterized in that porous carbon materials are right directly as two of button cell
Electrode is used for double electric layers supercapacitor.
7. application according to claim 5, which is characterized in that by porous carbon materials and metal oxide or conducting polymer
Compound obtained electrode material is used for Faraday pseudo-capacitance supercapacitor.
8. a kind of supercapacitor, which is characterized in that the supercapacitor includes porous active carbon electrode, the porous active carbon
The material of electrode is porous carbon materials prepared by claim 1.
9. porous carbon materials prepared by claim 1 are as adsorbent material or catalyst carrier.
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| CN201711452620.9A CN108198696B (en) | 2017-12-28 | 2017-12-28 | The preparation method and applications of porous carbon materials |
| PCT/CN2018/123612 WO2019129009A1 (en) | 2017-12-28 | 2018-12-25 | Preparation method for porous carbon material and use of same |
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| CN108198696B (en) * | 2017-12-28 | 2019-07-05 | 青岛大学 | The preparation method and applications of porous carbon materials |
| CN108987733B (en) * | 2018-09-11 | 2021-04-27 | 郑州大学 | Preparation method of active porous carbon @ FeS of lithium ion battery cathode material |
| CN112038107B (en) * | 2020-05-19 | 2021-10-15 | 延边大学 | Preparation and application of MnO/spore group double-doped porous carbon microsphere composite material |
| CN112563844B (en) * | 2020-12-03 | 2022-03-04 | 中国电力科学研究院有限公司 | Flexible graphite/continuous carbon fiber composite conductive grounding material and preparation method thereof |
| CN113149004A (en) * | 2021-04-26 | 2021-07-23 | 河北科技师范学院 | Preparation method of biomass porous carbon with high specific surface area |
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| CN106006630A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Method for preparing activated carbon materials |
| CN107424850A (en) * | 2016-05-23 | 2017-12-01 | 中国海洋大学 | It is a kind of to prepare the method for cellulose base porous carbon materials using hydro-thermal-activation-pyrolysismethod and be used for electrode of super capacitor |
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| CN101397135A (en) * | 2008-10-07 | 2009-04-01 | 东华大学 | Method for treating textile solid waste |
| CN105645410B (en) * | 2016-03-17 | 2017-11-14 | 中国林业科学研究院林产化学工业研究所 | 3D network pore structure Supercapacitor carbons and preparation method thereof |
| CN108198696B (en) * | 2017-12-28 | 2019-07-05 | 青岛大学 | The preparation method and applications of porous carbon materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006630A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Method for preparing activated carbon materials |
| CN107424850A (en) * | 2016-05-23 | 2017-12-01 | 中国海洋大学 | It is a kind of to prepare the method for cellulose base porous carbon materials using hydro-thermal-activation-pyrolysismethod and be used for electrode of super capacitor |
Non-Patent Citations (2)
| Title |
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| "Effect of ZnCl2 impregnation concentration on the microstructure and electrical performance of ramie-based activated carbon hollow fiber";Xuan Du, et al.;《IONICS》;20151112;第22卷;第545-553页 * |
| "纤维素多孔材料的制备与性能";崔莉等;《高分子材料科学与工程》;20131030;第29卷(第10期);第142-145页 * |
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