CN110255561A - A kind of N doping biomass porous carbon and preparation method thereof - Google Patents
A kind of N doping biomass porous carbon and preparation method thereof Download PDFInfo
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- CN110255561A CN110255561A CN201910692104.6A CN201910692104A CN110255561A CN 110255561 A CN110255561 A CN 110255561A CN 201910692104 A CN201910692104 A CN 201910692104A CN 110255561 A CN110255561 A CN 110255561A
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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
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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
It is to be casted off a skin with Chinese parasol tree tree for raw material the invention discloses a kind of N doping biomass porous carbon and preparation method thereof, after activation of potassium hydroxide, the lower calcining of argon atmosphere protection, then through pickling, drying, i.e. acquisition N doping biomass porous carbon.Present invention process is simple and convenient to operate, and resulting materials can be used as the electrode material of supercapacitor, specific capacity height, good cycle.
Description
Technical field
The invention belongs to biomass porous technical field of carbon material preparation, and in particular to a kind of to be casted off a skin with Chinese parasol tree tree for forerunner
Body, the method for preparing N doping biomass porous carbon.
Background technique
In recent years, due to the exhaustion of fossil fuel and global warming, the exploitation of renewable and sustainable energy storage equipment
It becomes increasingly conspicuous.Since supercapacitor has many advantages, such as that energy density height, power density is big, has extended cycle life, safe and reliable, quilt
It is widely used in hybrid vehicle and portable electronic product.The energy storage of supercapacitor is based on ionic adsorption (double electricity
Layer capacitor, EDLCs) or Rapid reversible faraday's reaction (pseudocapacitors).Carbonaceous nano material has biggish electrode/electro
Matter interface and shorter diffusion path are solved, is the research hotspot for preparing electrochemical capacitor high-performance capacitor electrode.Carbon based material
Such as electrode material of active carbon, carbon nanotube, Carbon fibe, templated porous charcoal, graphene as super capacitor device has and leads
The capacitive properties such as electrical property is good, large specific surface area, pore-size distribution is suitable, surface functional group is abundant.
Double layer capacitor (EDLC) is with active carbon (ACs) for electrode material, and with power density height, capacity is big, leaks electricity
It flows that small, charge and discharge process is simple, the advantages that having extended cycle life, is acknowledged as a kind of efficient electrical energy storage device.Active carbon
Electrode has the excellent performances such as easy processing, at low cost, corrosion-resistant, high temperature resistant, and is widely used.The desired activities of EDLC electrode
Carbon Materials require high specific surface area and optimal pore-size distribution, this is extremely important to the Fabrication of High Specific Capacitance of EDLC.It is especially former
Material and activation method are two key factors for influencing active carbon final structure and cost.
In recent years, many scholars feature cheap, from a wealth of sources, renewable and environmentally friendly because of biological material, by it
As the various biomass waste materials such as the raw material for preparing active carbon, such as cocoanut shell, walnut shell, corn stover, rice husk all by conduct
The presoma of biomass carbon material, to prepare the Carbon Materials of electrochemical performance.These raw materials are considered in traditional sense
It is biological waste, but in terms of biomass carbon, these waste materials are renewable, inexpensive and rapid regeneration resource, are had
Huge availability, therefore biomass is considered as a kind of carbon precursor of environmental protection, biomass castoff prepares Carbon Materials and also draws
The extensive concern of people is played.But the existing active carbon prepared with biological material, when being used as electrode of super capacitor,
The poor problem of generally existing performance.Therefore, continue to explore suitable biomass material and suitable preparation method, to be made
The porous carbon material of specific capacity height, good cycle, has great importance.
Summary of the invention
The present invention provides a kind of N doping biomass porous carbons and preparation method thereof, it is therefore intended that suitable by screening
Biomass material and suitable preparation method, to obtain the electrode material for super capacitor of specific capacity height, good cycle.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of N doping biomass porous carbon, it is characterized in that: it is casted off a skin with Chinese parasol tree tree for raw material, through hydrogen
After potassium oxide activation, the lower calcining of argon atmosphere protection, then through pickling, drying, i.e. acquisition N doping biomass porous carbon.Specific packet
Include following steps:
1) Chinese parasol tree tree husking deionized water is cleaned by ultrasonic completely, is then dried, then be broken into powder with wall-breaking machine, obtained
Chinese parasol tree tree husking powder;
2) potassium hydroxide is mixed with Chinese parasol tree tree husking powder and is placed in beaker, appropriate deionization is then added
Water stirs 8-12h, then dries;
3) product obtained in step 2) is pulverized, is then placed in tube furnace, carried out under argon atmosphere protection
Calcining, is down to room temperature after calcining, take out;
4) product for obtaining step 3), which is placed in hydrochloric acid solution, stirs 8-12h, is then centrifuged for separating, and gained precipitating is spent
Ionized water eccentric cleaning is to neutrality, then dries, i.e. acquisition N doping biomass porous carbon.
Further, in step 2), potassium hydroxide, Chinese parasol tree tree husking powder, deionized water amount ratio be 2~4g:
10g:50mL。
Further, in step 3), calcination temperature is 800 DEG C, and heating rate is 5-10 DEG C of min-1.Further, institute
Stating calcining is first with 5 DEG C of min-1Heating rate be warming up to 400 DEG C and keep the temperature 2h, then again with 10 DEG C of min-1Heating speed
Rate is warming up to 800 DEG C and keeps the temperature 2h.
Further, in step 4), the concentration of the hydrochloric acid solution is 1mol/L, the revolving speed of centrifuge separation be 3500rpm,
Centrifugation time is 5min.
Further, the drying in step 1), step 2) and step 4) is dried in 80 DEG C of baking oven.
Present invention N doping biomass porous carbon obtained is used as the electrode material of supercapacitor.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, by using the husking of Chinese parasol tree tree as raw material and preparation process is rationally arranged in the present invention, including activation method, forges
Burning condition etc., gained N doping biomass porous carbon pattern is uniformly, aperture is mostly micropore and has that part is mesoporous, large specific surface area;
Using N doping biomass porous carbon obtained by the present invention as the electrode material of supercapacitor, specific capacity height, good cycle, phase
Than showing superior performance in existing biomass porous carbon.
2, the raw materials used in the present invention Chinese parasol tree tree casts off a skin, and is renewable resource, from a wealth of sources, has practical, at low cost
Advantage.
3, preparation process of the invention is simple and convenient to operate, and is a kind of method that situ Nitrogen Doping may be implemented, and is not necessarily to
Additionally introduce other nitrogen sources.
Detailed description of the invention
Fig. 1 is the SEM figure of N doping biomass porous carbon prepared by embodiment 1;
Fig. 2 is the SEM figure of N doping biomass porous carbon prepared by embodiment 2;
Fig. 3 is the SEM figure of N doping biomass porous carbon prepared by embodiment 3;
Fig. 4 is the SEM figure of N doping biomass porous carbon prepared by embodiment 4;
Fig. 5 is the SEM figure of N doping biomass porous carbon prepared by embodiment 5;
Fig. 6 is the TEM figure of N doping biomass porous carbon prepared by embodiment 5;
Fig. 7 is the XPS figure of N doping biomass porous carbon prepared by embodiment 5;
Fig. 8 is the SEM figure of N doping biomass porous carbon prepared by embodiment 6;
Fig. 9 is bent for the constant current charge-discharge of electrode prepared by the N doping biomass porous carbon using Examples 1 to 6
Line.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.The following contents is affiliated only to design example of the invention and explanation
Those skilled in the art make various modifications or additions to the described embodiments or using similar sides
Formula substitution, as long as it does not deviate from the concept of invention or beyond the scope defined by this claim, should belong to of the invention
Protection scope.
Embodiment 1
The present embodiment prepares N doping biomass porous carbon as follows:
1) it takes 10g Chinese parasol tree tree to cast off a skin, places it in beaker after being soaked with deionized water and be cleaned by ultrasonic completely, be then put into
It is dried in 80 DEG C of baking oven, then is broken into powder with wall-breaking machine, obtain Chinese parasol tree tree husking powder;
2) 2g potassium hydroxide is mixed with 10g Chinese parasol tree tree husking powder and is placed in beaker, 50mL deionization is then added
Water stirs 8h, then is placed in 80 DEG C of baking ovens and dries;
3) product obtained in step 2) is ground into powder in mortar, takes appropriate powder to be placed in and burn in boat, then
It is put into tube furnace, is calcined under argon atmosphere protection, calcination temperature is 800 DEG C, and heating rate is 5 DEG C of min-1, heat preservation
Time is 2h, is cooled to room temperature taking-up to tube furnace after calcining;
4) powder for obtaining step 3) be placed in concentration be 1mol/L hydrochloric acid solution stir 12h, be then centrifuged for separation (from
Heart revolving speed is 3500rpm, centrifugation time 5min), gained precipitating deionized water eccentric cleaning to neutrality, then it is placed in 80 DEG C
It is dried in baking oven, i.e. acquisition N doping biomass porous carbon.
Fig. 1 is that the SEM of the present embodiment products therefrom schemes, and as can be seen from the figure porous structure has preliminarily formed, but simultaneously
Unevenly.
Embodiment 2
The present embodiment prepares N doping biomass porous carbon by the identical method of embodiment 1, and difference is only that: in step 2)
Potassium hydroxide quality is 3g.
Fig. 2 is that the SEM of the present embodiment products therefrom schemes, and as can be seen from the figure sample has formed uniform porous structure.
Embodiment 3
The present embodiment prepares N doping biomass porous carbon by the identical method of embodiment 1, and difference is only that: in step 2)
Potassium hydroxide quality is 4g.
Fig. 3 is that the SEM of the present embodiment products therefrom schemes, and as can be seen from the figure with the increase of KOH amount, porous structure is opened
Beginning gradually collapses.
Embodiment 4
The present embodiment prepares N doping biomass porous carbon by the identical method of embodiment 1, and difference is only that: in step 3)
Calcining be first with 5 DEG C of min-1Heating rate be warming up to 400 DEG C and keep the temperature 2h, then again with 10 DEG C of min-1Heating speed
Rate is warming up to 800 DEG C and keeps the temperature 2h.
Fig. 4 is that the SEM of the present embodiment products therefrom schemes, and has as can be seen from the figure formed a small amount of porous structure, but
And it is uneven.
Embodiment 5
The present embodiment prepares N doping biomass porous carbon by the identical method of embodiment 2, and difference is only that: in step 3)
Calcining be first with 5 DEG C of min-1Heating rate be warming up to 400 DEG C and keep the temperature 2h, then again with 10 DEG C of min-1Heating speed
Rate is warming up to 800 DEG C and keeps the temperature 2h.
Fig. 5 is that the SEM of the present embodiment products therefrom schemes, as can be seen from the figure the resulting sample of the present embodiment and embodiment
2 compare, and pore size distribution is more uniform, and porous structure has formed.
Fig. 6 is that the TEM of the present embodiment products therefrom schemes, as can be seen from the figure comprising micro- in the resulting sample of the present embodiment
The pore structures such as hole, mesoporous, it is corresponding with Fig. 5.
Fig. 7 is that the XPS of the present embodiment products therefrom schemes, and as can be seen from the figure C is main in sample obtained by the present embodiment
A small amount of O element is contained on element, surface, while can be seen that the method can form the doping of N element in situ.
Embodiment 6
The present embodiment prepares N doping biomass porous carbon by the identical method of embodiment 3, and difference is only that: in step 3)
Calcining be first with 5 DEG C of min-1Heating rate be warming up to 400 DEG C and keep the temperature 2h, then again with 10 DEG C of min-1Heating speed
Rate is warming up to 800 DEG C and keeps the temperature 2h.
Fig. 8 is that the SEM of the present embodiment products therefrom schemes, and as can be seen from the figure pore structure is collapsed more obvious.
Embodiment 7
Porous carbon material can be applied to a variety of energy storage devices, such as supercapacitor.To test electricity obtained by above-described embodiment
The capacitive property of pole material does following test: by the various embodiments described above N doping biomass porous carbon obtained and gathering inclined fluorine
Ethylene (PVDF) 9:1 in mass ratio, adds 1-Methyl-2-Pyrrolidone (NMP) that slurry is made, and is 1cm*2cm's coated in area
On carbon paper, coated area 1*1cm2, electrode is made.Electro-chemical test uses three-electrode system, and saturated calomel electrode is as ginseng
Than electrode, Pt as to electrode, in 6mol/L KOH solution, in -1~0V potential range, current density 1Ag-1Under into
The test of row constant current charge-discharge.
Fig. 9 is bent for the constant current charge-discharge of electrode prepared by the N doping biomass porous carbon using Examples 1 to 6
Line.Comparison is it is found that the specific capacity of Examples 1 to 6 sample is followed successively by 182.7Fg-1、266.3Fg-1、233.3Fg-1、264.3Fg-1、
337Fg-1、292Fg-1, the biomass porous carbon material compared to existing public reporting is significantly improved.Especially embodiment 5
The specific capacity of resulting materials is the 1.85 of embodiment 1,2,3,4,6,1.27,1.44,1.28,1.15 times respectively, and best performance can
As ideal electrode material.
Claims (8)
1. a kind of preparation method of N doping biomass porous carbon, it is characterised in that: casted off a skin with Chinese parasol tree tree for raw material, through hydrogen-oxygen
After changing potassium activation, the lower calcining of argon atmosphere protection, then through pickling, drying, i.e. acquisition N doping biomass porous carbon.
2. the preparation method of N doping biomass porous carbon according to claim 1, which is characterized in that including following step
It is rapid:
1) Chinese parasol tree tree husking deionized water is cleaned by ultrasonic completely, is then dried, then be broken into powder with wall-breaking machine, obtain Chinese parasol tree
Tree husking powder;
2) potassium hydroxide is mixed with Chinese parasol tree tree husking powder and is placed in beaker, appropriate amount of deionized water is then added, stirs
8-12h is mixed, then is dried;
3) product obtained in step 2) is pulverized, is then placed in tube furnace, calcined under argon atmosphere protection,
It is down to room temperature after calcining, takes out;
4) product for obtaining step 3), which is placed in hydrochloric acid solution, stirs 8-12h, is then centrifuged for separating, and gained precipitating uses deionization
Water eccentric cleaning is to neutrality, then dries, i.e. acquisition N doping biomass porous carbon.
3. preparation method according to claim 2, it is characterised in that: in step 2), potassium hydroxide, Chinese parasol tree tree husking powder
Last, deionized water amount ratio is 2~4g:10g:50mL.
4. preparation method according to claim 2, it is characterised in that: in step 3), calcination temperature is 800 DEG C, heating speed
Rate is 5-10 DEG C of min-1。
5. the preparation method according to claim 4, it is characterised in that: in step 3), the calcining is first with 5 DEG C of min-1
Heating rate be warming up to 400 DEG C and keep the temperature 2h, then again with 10 DEG C of min-1Heating rate be warming up to 800 DEG C and keep the temperature 2h.
6. preparation method according to claim 2, it is characterised in that: in step 4), the concentration of the hydrochloric acid solution is
1mol/L, the revolving speed of centrifuge separation is 3500rpm, centrifugation time 5min.
7. preparation method according to claim 2, it is characterised in that: the drying in step 1), step 2) and step 4) is all
It is to be dried in 80 DEG C of baking oven.
8. the N doping biomass porous carbon obtained of preparation method described in a kind of any one of claim 1~7.
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Application publication date: 20190920 |