CN106698418A - Self-templated fibrous biomass-based porous carbon material and preparation method and application thereof - Google Patents
Self-templated fibrous biomass-based porous carbon material and preparation method and application thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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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 belongs to the field of material science, and discloses a self-templated fibrous biomass-based porous carbon material and a preparation method and application thereof. The preparation method comprises the following steps: (1) washing, drying and crushing fibrous biomass; (2) carbonizing the crushed biomass raw material at low temperature first, then adding a solid activator, then adding water, soaking, activating, taking out and drying; (3) carbonizing the dried product at high temperature in an inert gas atmosphere, washing the carbonized product by using acid, then washing by using water until the carbonized product is neutral, and drying the washed product to obtain the biomass-based porous carbon material. By the preparation method, the self-templated biomass-based porous carbon material is prepared through two-step carbonization, and the structure of biomass itself is effectively utilized; the preparation method is simple and cheap. The prepared biomass-based porous carbon material is excellent in performance and wide in application; the porous carbon material can be used as an electrode of a supercapacitor and is large in capacity and good in stability, and the efficient utilization of biomass resources is achieved.
Description
Technical field
The present invention relates to self-template method fiber biomass base porous carbon materials with and preparation method thereof, and by prepare it is many
Hole carbon material is applied to ultracapacitor, belongs to material science.
Background technology
With developing rapidly for global industry, the non-renewable resources such as substantial amounts of coal, oil are constantly consumed, and cause money
The shortage in source.Therefore the consumption that we have to look for a kind of new energy to reduce or substitute non-renewable resources.Using can
The biomass of regeneration replace the fossil fuel of increasingly depleted as carbon source, are the directions of the following whole nation or even global evolution.By
In biomass are cheap, wide material sources, so being led as the raw material future porous carbon materials of porous carbon materials using biomass
Important component in domain.
Biomass are considered as a kind of excellent carbon materials material precursor, had prepare carbon material using biomass at present
Report.The carbon source of activated carbon can be prepared due to not only containing in biomass, and there is natural institutional framework, these structures
Multi-stage artery structure can be converted into.Therefore, biological material can turn into the raw material for preparing multistage pore canal activated carbon.But,
In current research, most of researchs only focus on the structure in destruction biomass to obtain porous carbon, cause biomass in itself
Structure be not fully utilized.Compared with presoma with artificial template, biomass material is more environment-friendly.This
Research can prepare the more excellent activated carbon of performance, will have the high-performance super capacitor material of upgrade cost advantage to prepare,
Realize that the high-valued application of biomass provides new thinking.
The content of the invention
It is an object of the invention to provide a kind of biomass-based porous carbon materials of self-template method and preparation method thereof.In order to be able to
Biomass design feature in itself, the present invention is enough made full use of directly using the biomass material of fiber-like, to be activated by two steps
The method of carbonization, prepares porous carbon materials, and the porous carbon of preparation is used as the electrode material of super capacitor, realizes biological material
The high-valued application of material.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of the biomass-based porous carbon materials of self-template, comprises the following steps：
(1) fiber biomass washed, dry and crush；
(2) by the biomass material elder generation low-temperature carbonization of broken mistake, solid activating agent is subsequently adding, is added water at immersion activation
Drying is taken out after reason；
(3) by dried product under atmosphere of inert gases high temperature cabonization, by the product acid elution after carbonization, then use
Water washing, until neutrality, the product after washing is dried, and obtains biomass-based porous carbon materials.
Step (1) described biomass material is first washed, then is dried or dried process, and dry temperature is 50~80
DEG C, it is also possible to dry naturally.Described crushing can be ground into bulk with shearing method or pulverizer.
Described biomass are bagasse, cajeputtree or the ganoderma lucidum dregs of a decoction.
The condition of the low-temperature carbonization described in step (2) is that carburizing temperature is 200 DEG C~500 DEG C, and process time is 1~3 small
When, the heating rate of low-temperature carbonization is 1~10 DEG C/min.
Described activator is NaOH, KOH, ZnCl2And H3PO4In one or more.
The mass ratio of the activator and biomass is 0.25~4.
The activation process time is 5~12h.
The method of step (2) activation process is to add activator in the raw material that low temperature is carbonized in advance, is added water, and stirring makes it
It is well mixed, soak 6~12h；Dry temperature is 80~100 DEG C, and the time is 6~20h.
The condition of the high temperature cabonization is first to be warming up to 300~400 DEG C of 0.5~2h of carbonization, then is warming up to 650~850 DEG C
1~3h of carbonization, the front and rear heating rate twice is 3~10 DEG C/min, and the inert gas is nitrogen or argon gas, gas stream
Speed is 0.5~1L/min.
Step (2) dry temperature is 80~100 DEG C, and the time is 6~20h；The dried strip of step (3) described final product
Part is dry 3~12h at 50~100 DEG C.
Washing methods described in step (3) is, first with the salt acid elution 3~5 times of 1~5M, is washed with water, until neutrality.
Biomass-based porous carbon materials prepared by the above method, its specific surface area is：1000~3000m2/g。
Described biomass-based porous carbon materials are used to prepare the electrode material of ultracapacitor or for adsorbing or being catalyzed.
The present invention has the advantage that relative to existing technology：
(1) present invention is cheap with natural biomass as raw material, and amount is big, is the reason for preparing biomass-based carbon material
Think presoma.
(2) present invention adds the mode of activator different, specifically first weighs sample and activator by a certain percentage,
Then soak.Using substantial amounts of heat is released during adding water, the activation efficiency of activator is substantially increased.
(3) present invention is by two step carbonization, and first low-temperature carbonization fixes biomass structure in itself, then high by a step
Warm carbonizatin method prepares porous carbon materials, efficiently utilizes biomass structure in itself, prepares the work with multi-stage artery structure
Property charcoal, and realize the higher value application of biomass resource.
(4) processing procedure is simple, it is only necessary to add a small amount of activator just to obtain the porous carbon materials of high-specific surface area, greatly
Corrosion of the activator to equipment is reduced greatly, is conducive to large-scale production.Corncob base porous carbon materials prepared by the present invention
Excellent performance, is widely used, and porous carbon materials can act as the electrode of ultracapacitor, and capacity is big, good stability.
Brief description of the drawings
Fig. 1 is the SEM figures of the bagasse product of pre- carbonization prepared by embodiment 1.
Fig. 2 (a), (b) be embodiment 2 in be prepare bagasse base porous carbon under different amplification SEM figure.
Fig. 3 (a), (b) are SEM figure of the cajeputtree base porous carbon materials of the preparation of embodiment 2 under different amplification.
Fig. 4 is the SEM figures of ganoderma lucidum dregs of a decoction base porous carbon materials prepared by embodiment 3.
Fig. 5 is the SEM figures of cajeputtree base porous carbon materials prepared by embodiment 4.
Specific embodiment
The present invention is more specifically described in detail with reference to specific embodiment, but embodiments of the present invention are not limited
In this, for especially not dated technological parameter, can refer to routine techniques is carried out.
Embodiment 1
(1) bagasse is put into boat-shaped sample cell, and is placed in atmosphere tube type stove, burner hearth vacuumized, in argon
Low-temperature carbonization is carried out under the atmosphere of gas, the flow velocity of argon gas is 0.5L/min, and heating rate is 5 DEG C/min, is warming up to 200 DEG C, place
The reason time is 3h.Then the product grinding that will be obtained is stand-by.
(2) bagasse that 1g is carbonized in advance is put into beaker, adds the KOH solids of 2g, add a small amount of water (with just
Dipped reactant is advisable), soak 8h.It is dried into 6h for 80 DEG C in baking oven, by dried residue in the atmosphere of argon gas, first
300 DEG C of carbonization 1h are warmed up to, then proceed to be warmed up to 750 DEG C of carbonization 1.5h, gas flow rate is 0.5L/min, and heating rate is 5
℃/min.The product that will the be obtained salt acid elution 5 times of 2M, is washed with water neutrality, and 12h is dried at 80 DEG C, obtains bagasse
Base porous carbon materials.
From figure 1 it appears that the bagasse of pre- carbonization remains its original fibre structure, and fiber surface light
It is sliding.
Figure it is seen that obtained bagasse base porous carbon materials have what is enriched on the fibre structure of itself
Hole, the specific surface area of porous carbon materials is：1749.34m2/g。
Embodiment 2
(1) cajeputtree is put into boat-shaped sample cell, and is placed in atmosphere tube type stove, burner hearth vacuumized, in argon
Low-temperature carbonization is carried out under the atmosphere of gas, the flow velocity of argon gas is 0.5L/min, and heating rate is 5 DEG C/min, is warming up to 300 DEG C, place
The reason time is 1.5h.Then the product grinding that will be obtained is stand-by.
The cajeputtree that 1g is carbonized in advance is put into beaker, in mass ratio 2:1 ratio mixes with KOH solids, and the leaching that adds water
Bubble 10h, then 100 DEG C dry 10h.Dried sample is put into boat-shaped sample cell, in the atmosphere of nitrogen, is first warming up to
300 DEG C of low-temperature carbonization 2h, then be warming up to 750 DEG C of high temperature cabonization 1.5h, gas flow rate is 0.5L/min, heating rate is 5 DEG C/
min.The product that will the be obtained salt acid elution 5 times of 2M, is washed with water neutrality, and 12h is dried at 80 DEG C, obtains cajeputtree Quito
Hole carbon material.
From figure 3, it can be seen that obtained cajeputtree base porous carbon materials have abundant hole in the structure of itself,
The specific surface area of porous carbon materials is：1731.5m2/g.Self-template method is successfully passed by the method and has prepared cajeputtree Quito
Hole carbon material.
Embodiment 3
(1) the ganoderma lucidum dregs of a decoction are put into boat-shaped sample cell, and are placed in atmosphere tube type stove, burner hearth is vacuumized,
Low-temperature carbonization is carried out under the atmosphere of argon gas, the flow velocity of argon gas is 0.5L/min, and heating rate is 5 DEG C/min, is warming up to 300 DEG C,
Process time is 1.5h.Then the product grinding that will be obtained is stand-by.
(2) ganoderma lucidum dregs of a decoction 1g being carbonized in advance are put into beaker, and in mass ratio 3:1 ratio mixes with KOH solids, and adds
Water soaks 10h, and then 100 DEG C dry 8h.Dried sample is put into boat-shaped sample cell, in the atmosphere of argon gas, is first risen
To 300 DEG C, be carbonized temperature 1h, and heating rate is 5 DEG C/min, then is warming up to 750 DEG C of carbonization 1.5h, and gas flow rate is 0.5L/min,
Heating rate is 3 DEG C/min.The product that will the be obtained salt acid elution 5 times of 2M, is washed with water neutrality, and 12h is dried at 80 DEG C,
Ganoderma lucidum dregs of a decoction base porous carbon materials are obtained, its specific surface area is：1363.2m2/g。
Embodiment 4
(1) cajeputtree is put into boat-shaped sample cell, and is placed in atmosphere tube type stove, burner hearth vacuumized, in argon
Low-temperature carbonization is carried out under the atmosphere of gas, the flow velocity of argon gas is 0.5L/min, and heating rate is 5 DEG C/min, is warming up to 400 DEG C, place
The reason time is 1h.Then the product grinding that will be obtained is stand-by.
(2) cajeputtree that 1g is carbonized in advance is put into beaker, by dried residue in mass ratio 2:1 ratio with prepare
KOH solution mixing, activate 10h, then 100 DEG C dry 10h.In the atmosphere of argon gas, 750 DEG C of carbonization 2h, gas flow rate is
0.5L/min, heating rate is 5 DEG C/min.The product that will the be obtained salt acid elution 5 times of 2M, is washed with water neutrality, 80 DEG C
Under dry 12h, obtain cajeputtree base porous carbon materials.
Embodiment 5
(1) bagasse is put into boat-shaped sample cell, and is placed in atmosphere tube type stove, burner hearth vacuumized, in argon
Low-temperature carbonization is carried out under the atmosphere of gas, the flow velocity of argon gas is 0.5L/min, and heating rate is 5 DEG C/min, is warming up to 300 DEG C, place
The reason time is 1h.
(2) by the bagasse of 1g with being put into beaker, by dried residue in mass ratio 3:1 ratio and ZnCl2Gu
Body mixes, and in the atmosphere of nitrogen, 850 DEG C of carbonization 2h, gas flow rate is 0.5L/min, and heating rate is 5 DEG C/min.To obtain
The product salt acid elution 5 times of 2M, be washed with water neutrality, dry 12h at 80 DEG C, obtain bagasse base porous carbon materials.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. the preparation method of the biomass-based porous carbon materials of a kind of self-template, it is characterised in that comprise the following steps：
(1) fiber biomass washed, dry and crush；
(2) by the biomass material elder generation low-temperature carbonization of broken mistake, solid activating agent is subsequently adding, after adding water immersion activation process
Take out drying；
(3) by dried product under atmosphere of inert gases high temperature cabonization, the product acid elution after carbonization is washed with water
Wash until neutrality, the product after washing is dried, obtain biomass-based porous carbon materials.
2. method according to claim 1, it is characterised in that described biomass are bagasse, cajeputtree or ganoderma lucidum medicine
Slag.
3. method according to claim 1 and 2, it is characterised in that the condition of the low-temperature carbonization described in step (2) is carbonization
Temperature is 200 DEG C~500 DEG C, and process time is 1~3 hour, and the heating rate of low-temperature carbonization is 1~10 DEG C/min.
4. method according to claim 1 and 2, it is characterised in that described activator is NaOH, KOH, ZnCl2With
H3PO4In one or more.
5. method according to claim 1 and 2, it is characterised in that the mass ratio of the activator and biomass is 0.25
~4.
6. method according to claim 1 and 2, it is characterised in that the activation process time is 5~12h.
7. method according to claim 1 and 2, it is characterised in that the condition of the high temperature cabonization be first be warming up to 300~
400 DEG C carbonization 0.5~2h, then be warming up to 650~850 DEG C carbonization 1~3h, it is described before and after twice heating rate be 3~10 DEG C/
Min, the inert gas is nitrogen or argon gas, and gas flow rate is 0.5~1L/min.
8. method according to claim 1 and 2, it is characterised in that step (2) dry temperature is 80~100 DEG C, time
It is 6~20h；The drying condition of step (3) described final product is dry 3~12h at 50~100 DEG C.
9. the biomass-based porous carbon materials that any one of claim 1~8 method is prepared.
10. the biomass-based porous carbon materials described in claim 9 are used to prepare the electrode material of ultracapacitor or for inhaling
Attached or catalysis.
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| CN107519855A (en) * | 2017-07-18 | 2017-12-29 | 武汉工程大学 | Bagasse base Pd/carbon catalyst and its production and use |
| CN107754760A (en) * | 2017-09-30 | 2018-03-06 | 四会市启德信息咨询服务有限公司 | A kind of porous carbon materials of purifying formaldehyde and preparation method thereof |
| CN107758660A (en) * | 2017-10-27 | 2018-03-06 | 武汉工程大学 | A kind of method that bagasse matrix activated carbon is prepared using zinc chloride as activator |
| CN108163852A (en) * | 2018-01-03 | 2018-06-15 | 湖南农业大学 | A kind of ganoderma lucidum base two-dimensional sheet carbon material and preparation method thereof and the application as secondary cell negative pole material |
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