CN108074751A - A kind of flexible 3 D porous carbon materials and its preparation method and application - Google Patents
A kind of flexible 3 D porous carbon materials and its preparation method and application Download PDFInfo
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- CN108074751A CN108074751A CN201711297502.5A CN201711297502A CN108074751A CN 108074751 A CN108074751 A CN 108074751A CN 201711297502 A CN201711297502 A CN 201711297502A CN 108074751 A CN108074751 A CN 108074751A
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- flexible
- porous carbon
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- melamine sponge
- coal tar
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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
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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 a kind of flexible 3 D porous carbon materials and its preparation method and application.For the present invention using cheap business melamine sponge as three-dimension flexible carbon skeleton masterplate, coal tar pitch is carbon source, and with reference to KOH activation methods, a step obtains high conductivity, the flexible 3 D porous carbon materials of high-specific surface area；The preparation process of the material is simple, of low cost, suitable for commercial Application.The material is used as electrode material for super capacitor, has larger energy density, power density and excellent cyclical stability.
Description
Technical field
The present invention relates to a kind of flexible 3 D porous carbon materials and its preparation method and application, belong to novel energy resource material technology
Field.
Background technology
Ultracapacitor has high energy density, service life cycle length, body as a kind of electrochemical energy storage device
The series of advantages such as product is small, Simple portable, safety non-pollution, in mobile communication, information technology, consumer electronics, electric vehicle, boat
Empty space flight and science and techniques of defence etc. have broad application prospects, it is considered to be a kind of preferable electrochmical power source.At present, business
Change ultracapacitor mainly by the use of activated carbon as electrode material.The performance of ultracapacitor depends primarily upon electrode used therein material
Specific surface area, pore-size distribution, microstructure and electric conductivity etc..
Compared to other carbon materials, absorbent charcoal material has many advantages, such as that large specific surface area, raw material sources are enriched, are at low cost.But
The active carbon particle prepared due to conventional method is greatly and electric conductivity is poor, this increase electrolyte ion and charge diffusion length with
Resistance has severely impacted its fast charge/discharge ability, particularly at higher current densities, so as to cause the property of capacitor
It can reduce.
The content of the invention
The present invention provides a kind of low cost, high-specific surface area and highly conductive flexible 3 D porous carbon materials.The present invention
The preparation method and application of above-mentioned flexible 3 D porous carbon materials are additionally provided, the three-dimensional porous carbon material prepared by this method
Binder free is realized as electrode of super capacitor, there is high-energy density, high rate capability and excellent cycling stability, table
Reveal remarkable capacitive property, it is considered to be a kind of preferable electrode material for super capacitor.
The present invention provides a kind of flexible 3 D porous carbon materials, using cheap business melamine sponge conduct
Three-dimension flexible carbon skeleton masterplate, coal tar pitch are carbon source, and with reference to KOH activation methods, one-step method obtains high conductivity, high-specific surface area
Flexible 3 D porous carbon materials.
The mass fraction of raw material is：
Melamine sponge：5 ~ 10 parts
Coal tar pitch：20 ~ 60 parts
KOH：20 ~ 80 parts
Tetrahydrofuran：20 ~ 60 parts
Absolute ethyl alcohol：20 ~ 40 parts
The melamine sponge is the business melamine sponge without any processing.
The present invention provides the preparation methods of above-mentioned flexible 3 D porous carbon materials, comprise the following steps：
（1）It chooses business melamine sponge and is cut into the cm of the cm of 5 cm × 3 × 2, acetone is cleaned by ultrasonic 10 ~ 30 min,
Then dried in the range of temperature is 70 ~ 110 DEG C；
（2）20 ~ 60 parts of coal tar pitch is taken to be dissolved in the solution of 20 ~ 40 parts of tetrahydrofurans, stirring and dissolving；Take 20 ~ 80 parts of potassium hydroxide
It is dissolved in 20 ~ 40 parts of ethyl alcohol, stirring is until dissolving；
（3）By above two solution（Tetrahydrofuran and ethanol solution）It is stirred evenly after mixing, melamine sponge is put into it
In, it squeezes and is sufficiently impregnated repeatedly, 6 ~ 10 h are dried in the range of temperature is 70 ~ 110 DEG C after uniform adsorption；Form coal tar pitch/tri-
Poly cyanamid sponge compound；
In the step, the mass ratio of melamine sponge used and coal tar pitch is：Melamine sponge：Coal tar pitch=5 ~ 10：20~
60；
（4）Dried coal tar pitch/melamine sponge compound is taken, is transferred in ceramic crucible, is placed in tube furnace, N2Or
Under Ar gas shieldeds, at 700 DEG C ~ 1000 DEG C, a step is carbonized and activation, through pickling, filtering, vacuum drying (90 DEG C ~ 110 DEG C), obtains
Obtain flexible 3 D porous carbon materials.
The present invention provides application of the above-mentioned flexible 3 D porous carbon materials in ultracapacitor.
In above application, using flexible 3 D porous carbon materials direct slicing as the electrode material of ultracapacitor, normal
Rule three-electrode system evaluates its chemical property, and platinized platinum is to electrode, and saturation calomel is reference electrode, and electrolyte is 6 M KOH.
Beneficial effects of the present invention：
（1）The present invention selects business melamine sponge, and production cost is low as three-dimension flexible carbon skeleton masterplate.
（2）Compared with other porous carbon materials, product of the present invention has the carbon skeleton and pore passage structure of three-dimensional interconnection, favorably
In electronics and electrolyte ion in the conduction and diffusion of electrode interior, while the porous carbon material of foaming structure becomes storage charge
" reservoir ", so as to improve the energy density of the electrode material and power density.
Description of the drawings
Fig. 1 is（a）Comparative example 1,（b）The stereoscan photograph of embodiment 3；
Fig. 2 is the specific surface area and graph of pore diameter distribution of activated carbon prepared by comparative example 1 and embodiment 3 and three-dimensional porous carbon material；
Fig. 3 100 mV s under three-electrode system in 6 M KOH electrolyte for comparative example 1 and embodiment 3-1Cyclic voltammetric survey
Try graph；
Fig. 4 prepares activated carbon and three-dimensional porous carbon material in 1 A g for comparative example 1 and embodiment 3-1Charging and discharging curve figure；
Fig. 5 is 3 Nyquist impedance spectra of comparative example 1 and embodiment；
Fig. 6 is that prepare three-dimensional porous carbon material in current density be 5 A g to embodiment 3-1Following after the charge and discharge of 5000 cycles
Ring stability figure.
Specific embodiment
It is further illustrated the present invention below by embodiment, but is not limited to following embodiment.
Comparative example 1：Absorbent charcoal material is prepared by coal tar pitch and KOH, is not added with melamine masterplate
It weighs 20 parts of coal tar pitch and is dissolved in 20 parts of tetrahydrofurans；It weighs 40 parts of KOH and is dissolved in absolute ethyl alcohol, by above two solution
（Tetrahydrofuran and ethanol solution）Mixing, mixed solution 10 min of magnetic agitation, 70 DEG C of 6 h of drying at room temperature；By drying
Mixture afterwards is transferred in ceramic crucible, is placed in tube furnace, in N2Under protection, it is heated to 800 DEG C and is pyrolyzed；By gained
Carbon material is immersed in 10 h in 2 M HCl solutions, filtering, in 90 DEG C of vacuum drying, obtains absorbent charcoal material.
The absorbent charcoal material has block structure, and average grain diameter has reached 50 μm（See Fig. 1 a）, specific surface area is only
1132 m2g-1, pore volume is 0.599 cm3g-1.After testing, using the activated carbon as the electrode material of ultracapacitor, in 6 M
Specific capacitance is 100 F g in KOH electrolyte-1(current density is 1 A g-1), in 5 A g of current density-1Under, through 5000 cycles
After cycling, specific capacitance retention is 82.6%.
Comparative example 2：Absorbent charcoal material is prepared by coal tar pitch, is not added with KOH
One piece of the cm melamine foamed plastics sponge of the cm of 5 cm × 3 × 2 is cut, acetone is cleaned by ultrasonic 20 min, 90 DEG C of dryings；
It weighs 60 parts of coal tar pitch and is dissolved in 40 parts of tetrahydrofurans, at room temperature 20 min of magnetic agitation, be put into melamine sponge and be sufficiently impregnated
It is dry after uniform adsorption, dried coal tar pitch foam sponge compound is transferred in ceramic crucible, is placed in tube furnace,
N2Under protection, it is heated to 700 DEG C and is pyrolyzed；Gained carbon material is immersed in 10 h in 2 M HCl solutions, is filtered, at 90 DEG C
Vacuum drying, obtains three-dimensional porous carbon material.
The specific surface area of the three-dimensional porous carbon material of gained is 111.2 m2g-1, pore volume is 0.12 cm3g-1.After testing,
Using the three-dimensional porous carbon material as the electrode material of ultracapacitor, specific capacitance is 45.7F g in 6 M KOH electrolyte-1
(current density is 1 A g-1)；In 5 A g of current density-1Under, after 5000 loop cycles, specific capacitance retention is 79.6%.
Embodiment 1：Provide three-dimensional porous carbon material prepared according to the methods of the invention and its application
One piece of the cm melamine foamed plastics sponge of the cm of 5 cm × 3 × 2 is cut, acetone is cleaned by ultrasonic 30 min, and 100 DEG C dry
It is dry；It weighs 40 parts of coal tar pitch and is dissolved in 30 parts of tetrahydrofurans, weigh 20 parts of KOH and be dissolved in 20 parts of absolute ethyl alcohols, above two is molten
Liquid mixes, mixed solution 10 min of magnetic agitation at room temperature, is put into after melamine sponge is sufficiently impregnated uniform adsorption and does
It is dry；Dried coal tar pitch foam sponge compound is transferred in ceramic crucible, is placed in tube furnace, under Ar protections, is added
Heat is carbonized and is activated to 900 DEG C；Gained Carbon Materials are immersed in 10 h in 2 M HCl solutions, are filtered, it is true at 110 DEG C
Sky is dry, obtains three-dimensional porous carbon material.
The specific surface area of the three-dimensional porous carbon material of gained is 1146.9 m2g-1, pore volume is 0.78 cm3g-1.After testing,
Using the three-dimensional porous carbon material as the electrode material of ultracapacitor, specific capacitance is 142.7 F in 6 M KOH electrolyte
g-1(current density is 1 A g-1), in 5 A g of current density-1Under, after 5000 loop cycles, specific capacitance retention is
90.6%。
Embodiment 2：Provide three-dimensional porous carbon material prepared according to the methods of the invention and its application
Cutting one piece of the cm melamine foamed plastics sponge of the cm of 5 cm × 3 × 2, acetone is cleaned by ultrasonic 10 min, 70 DEG C of dryings,
It weighs 20 parts of coal tar pitch and is dissolved in 20 parts of tetrahydrofurans, weigh 80 parts of KOH and be dissolved in 40 parts of absolute ethyl alcohols, by above two solution（Four
Hydrogen furans and ethanol solution）Mixing, mixed solution 10 min of magnetic agitation at room temperature, is put into melamine sponge and fully soaks
It is dry after stain uniform adsorption；Dried coal tar pitch foam sponge compound is transferred in ceramic crucible, is placed in tube furnace,
In N2Under protection, it is heated to 800 DEG C and is pyrolyzed；Gained carbon material is immersed in 10 h in 2M HCl solutions, is filtered, 100
DEG C vacuum drying, obtain three-dimensional porous carbon material.
The specific surface area of the three-dimensional porous carbon material of gained is 2290 m2g-1, pore volume is 1.429 cm3g-1.After testing,
Using the three-dimensional porous carbon material as the electrode material of ultracapacitor, specific capacitance is 214F g in 6 M KOH electrolyte-1
(current density is 1 A g-1), in 5 A g of current density-1Under, after 5000 loop cycles, specific capacitance retention is 93.6%.
Embodiment 3：Provide three-dimensional porous carbon material prepared according to the methods of the invention and its application
One piece of the cm melamine foamed plastics sponge of the cm of 5 cm × 3 × 2 is cut, acetone is cleaned by ultrasonic 10 min, and 100 DEG C dry
It is dry, it weighs 40 parts of coal tar pitch and is dissolved in 30 parts of tetrahydrofurans, weigh 60 parts of KOH and be dissolved in 30 parts of absolute ethyl alcohols, above two is molten
Liquid（Tetrahydrofuran and ethanol solution）Mixing, mixed solution 10 min of magnetic agitation at room temperature, is put into melamine sponge
It is dried after being sufficiently impregnated uniform adsorption；Dried coal tar pitch foam sponge compound is transferred in ceramic crucible, is placed in pipe
In formula stove, in N2Under protection, it is heated to 800 DEG C and is pyrolyzed；Gained carbon material is immersed in 10 h, mistake in 2M HCl solutions
Filter in 110 DEG C of vacuum drying, obtains three-dimensional porous carbon material.
The three-dimensional porous carbon material of gained shows unique three-dimensional porous carbon nanosheet structure being connected with each other (see Fig. 1 b)
And high-specific surface area, specific surface area reach 3105 m2g-1, pore volume is 2.119 cm3g-1（See Fig. 2）.Unique structure
Effectively improve the diffusion and conduction of the electric conductivity of electrode material, electrolyte ion and charge in electrode and electrolyte interface.With
The electrode material of the three-dimensional porous carbon material as ultracapacitor, specific capacitance is 317.7 F g in 6 M KOH electrolyte-1
(current density is 1 A g-1), in 5 A g of current density-1Under, after 5000 loop cycles, specific capacitance retention is 97.2%.
Above-described embodiment explanation：The present invention is by the use of business melamine sponge as the masterplate of three-dimensional carbon skeleton, coal tar pitch
It for carbon source, is activated with reference to KOH, obtains high-specific surface area flexible 3 D porous carbon materials.With unused melamine sponge masterplate
It obtains traditional activated carbon to compare, apparent variation occurs for microstructure, becomes three-dimensional porous structure, specific surface from block structure
It accumulates from 1132 m2g-1Increase to 3105 m2g-1, pore volume is from 0.599 cm3g-1Increase to 2.119 cm3g-1.It is used as super electricity
During container electrode, capacitor is being 1 A g than electric current-1When, specific capacitance is from 100 F g-1Increase to 317 F g-1.Therefore, this hair
The three-dimensional porous carbon material of bright preparation has higher specific surface area, pore volume and excellent chemical property, and the present invention
Simple process and low cost is honest and clean, suitable for commercial Application.
Claims (6)
1. a kind of flexible 3 D porous carbon materials, it is characterised in that：Using melamine sponge as three-dimension flexible carbon skeleton mould
Version, coal tar pitch is carbon source, and with reference to KOH activation methods, a step obtains high conductivity, the flexible 3 D porous carbon of high-specific surface area
Material；Wherein, the mass fraction of raw material is：
Melamine sponge：5 ~ 10 parts
Coal tar pitch：20 ~ 60 parts
KOH：20 ~ 80 parts
Tetrahydrofuran：40 ~ 60 parts
Absolute ethyl alcohol：20 ~ 40 parts.
2. flexible 3 D porous carbon materials according to claim 1, it is characterised in that：The melamine sponge be without
The business melamine sponge of any processing.
3. the preparation method of the flexible 3 D porous carbon materials described in a kind of claim 1 or 2, it is characterised in that including following step
Suddenly：
（1）Business melamine sponge is taken to be cut into the cm of the cm of 5 cm × 3 × 2, it is 10 ~ 30 that acetone, which is cleaned by ultrasonic the time,
Then min is dried in temperature is 70 ~ 110 DEG C；
（2）20 ~ 60 parts of coal tar pitch is taken to be dissolved in the solution of 20 ~ 40 parts of tetrahydrofurans, stirring and dissolving；Take 20 ~ 80 parts of potassium hydroxide
It is dissolved in 20 ~ 40 parts of ethyl alcohol, stirring is until dissolving；
（3）It is stirred evenly after above-mentioned tetrahydrofuran and ethanol solution are mixed, melamine sponge is put into wherein, is squeezed repeatedly
It is sufficiently impregnated, 6 ~ 10 h is dried in temperature is 70 ~ 110 DEG C after uniform adsorption；It is compound to form coal tar pitch/melamine sponge
Object；
In the step, the mass ratio of melamine sponge used and coal tar pitch is：Melamine sponge：Coal tar pitch=5 ~ 10：20~
60；
（4）Dried coal tar pitch/melamine sponge compound is taken, is transferred in ceramic crucible, is placed in tube furnace, N2Or
Under Ar protections, at 700 ~ 1000 DEG C, direct carbonization and activation through pickling, filtering, vacuum drying, obtain flexible 3 D porous carbon
Material.
4. the preparation method of flexible 3 D porous carbon materials according to claim 3, it is characterised in that：The step（4）
In vacuum drying temperature be 90 ~ 110 DEG C.
5. a kind of application of the flexible 3 D porous carbon materials in ultracapacitor described in claim 1 or 2.
6. application according to claim 5, it is characterised in that：Using flexible 3 D porous carbon materials direct slicing as super
The electrode material of capacitor evaluates its chemical property in conventional three-electrode system, and platinized platinum is to electrode, and saturation calomel is reference
Electrode, electrolyte are 6 M KOH.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109473647A (en) * | 2018-11-01 | 2019-03-15 | 东莞市迈科新能源有限公司 | A kind of lithium sulfur battery anode material and preparation method thereof |
| CN109742405A (en) * | 2018-12-29 | 2019-05-10 | 中南林业科技大学 | Adjustable flexible electrode material in aperture and the preparation method and application thereof |
| CN109943066A (en) * | 2019-04-17 | 2019-06-28 | 河南科技大学 | Monomer cast nylon polymeric material with three dimensional network structure, preparation method and applications |
| CN110980719A (en) * | 2019-12-12 | 2020-04-10 | 太原科技大学 | Preparation method of porous graphitized hollow carbon microspheres |
| CN114053996A (en) * | 2021-10-29 | 2022-02-18 | 河南理工大学 | Integrally-formed nitrogen-containing blocky porous carbon material and preparation method and application thereof |
| CN114843118A (en) * | 2022-04-29 | 2022-08-02 | 武汉工程大学 | Electrode composite material GO-C @ M (OH) with hierarchical pores 2 And preparation method and application thereof |
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| CN114053996A (en) * | 2021-10-29 | 2022-02-18 | 河南理工大学 | Integrally-formed nitrogen-containing blocky porous carbon material and preparation method and application thereof |
| CN114843118A (en) * | 2022-04-29 | 2022-08-02 | 武汉工程大学 | Electrode composite material GO-C @ M (OH) with hierarchical pores 2 And preparation method and application thereof |
| CN114843118B (en) * | 2022-04-29 | 2024-04-09 | 武汉工程大学 | Electrode composite GO-C@M (OH) with hierarchical pores 2 Preparation method and application |
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