CN106744802A - Compound duct carbon material of the one-dimensional micropore macropore of bio-based and preparation method thereof - Google Patents
Compound duct carbon material of the one-dimensional micropore macropore of bio-based and preparation method thereof Download PDFInfo
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Abstract
The compound duct carbon material of the one-dimensional micropore macropore of bio-based of the invention belongs to supercapacitor technologies field, the microscopic appearance of the compound duct carbon material of the one-dimensional micropore macropore of bio-based is tubulose, states the compound duct carbon material of the one-dimensional micropore macropore of bio-based and is made up of agraphitic carbon and graphitized carbon；The preparation method of the compound duct carbon material of the one-dimensional micropore macropore of bio-based is that trailing plants Japonica is carried out into the carbon material that carbonization-activation obtains one-dimensional micropore macropore compound pore passage structure.The compound duct carbon material of the one-dimensional micropore macropore of bio-based of the invention achieves that processing procedure is simple and convenient, and raw material green is cheap and easy to get, environmentally friendly, the good beneficial effect of chemical property.The compound duct carbon material of the one-dimensional micropore macropore of gained bio-based has huge potentiality application in terms of super capacitor material.
Description
Technical field
The present invention relates to super capacitor material technical field, and in particular to a kind of one-dimensional micropore-macropore of bio-based is combined
Duct carbon material and preparation method thereof.
Background technology
With the development of mankind's science and technology, increasing instrument and equipment needs portable energy storage device, such as wind-driven generator,
Mobile phone, notebook computer, unmanned plane and lithium battery automobile etc..The ultracapacitor not only specific surface area, extra small with super large
Electric charge gap and itself do not occur chemical reaction etc. feature, also with the advantage better than other energy storage devices：(1) charging rate
Hurry up, charging can reach more than the 95% of its rated capacity in 10 seconds~10 minutes；(2) service life cycle is long, depth discharge and recharge
Number of times is recycled up to 1~500,000 times；(3) energy conversion efficiency is high, and process losses are small, and high current energy circulation efficiency >=
90%；(4) power density is high, up to 300W/kg~5000W/kg, equivalent to 5~10 times of battery；(5) product raw material structure
Into, production, using, store and disassemble process and do not pollute, be preferable environmental protection power supply；(6) safety coefficient is high, makes for a long time
With can be non-maintaining；(7) easy to detect, dump energy can directly read.At present, the predecessor for preparing ultracapacitor has polypyrrole
(European Polymer Journal.2013,49,3651-3656), graphene oxide (Nanoscale Research
) and MnO Letters.2014,9,535-5452(ACS Appl.Mater.Interfaces,2014 6(13),10506-
10515) etc., these methods are cumbersome, relatively costly.And at the aspect of biomass carbonization, one-dimensional carbon material product report compared with
Few, pattern is destroyed most of biomass after treatment, and one-dimensional microstructure is conducive to the transmission of electric charge to spread.Separately
Outward, from environmental protection from the point of view of cost, it is desired to prepare the predecessor used by product is with low cost, preferably waste is sharp
With.Therefore, suitable, the with low cost biomass material of pattern is found, by the good electrochemistry of simple treatment processability
Material is significant.
The content of the invention
The technical problem to be solved in the present invention is, biomass carbonization material feedstock high cost.To solve this problem, this hair
It is bright to be combined duct carbon material there is provided a kind of one-dimensional micropore-macropore of bio-based, while providing the one-dimensional micropore of the bio-based-big
The preparation method of the compound duct carbon material in hole.The technical solution adopted by the present invention is that the one-dimensional micropore-macropore of bio-based is combined
Duct carbon material is made up of agraphitic carbon and graphitized carbon；The system of the compound duct carbon material of the one-dimensional micropore-macropore of bio-based
Preparation Method is that trailing plants Japonica is carried out into the carbon material that carbonization-activation obtains one-dimensional micropore-macropore compound pore passage structure.
The concrete technical scheme that the present invention is used is that a kind of one-dimensional micropore-macropore of bio-based is combined duct carbon material, by nothing
Sizing carbon and graphitized carbon composition, it is characterized in that, the compound duct carbon material of the one-dimensional micropore-macropore of bio-based is one-dimensional tubulose
Structure, length is 100~300 μm, and about 2~8 μm of caliber, 0.2~0.5 μm of thickness of pipe wall has a large amount of micropores in tube wall；Wherein without
The mass ratio of sizing carbon and graphitized carbon is about 3.5~4.5:1.
The preparation method of the compound duct carbon material of the one-dimensional micropore-macropore of bio-based, building-up process is as follows：
Trailing plants Japonica is peeled off remove seed, is washed with deionized water and net is obtained within 12~24 hours trailing plants Japonica silk after 100~140 DEG C of dryings；
Under nitrogen protection, trailing plants Japonica silk is carbonized 0.5~3 hour in 500~700 DEG C, obtains carbonization trailing plants Japonica silk；Carbonization trailing plants Japonica silk is put
In the distilled water dissolved with NaOH, heated 1~5 hour in 100~140 DEG C, be washed with deionized after 100~140
DEG C drying 12~24 hours, obtains the carbonization trailing plants Japonica silk without metallic element, with the mistake for avoiding metallic element from being circulated in electrochemistry
The unstable of material is caused in journey；The mass ratio of carbonization trailing plants Japonica silk, NaOH and water is 1:4~30:200~400；
Stirred 30~90 minutes in distilled water by the carbonization trailing plants Japonica silk immersion without metallic element dissolved with potassium hydroxide, taken out
Filter, in 100~140 DEG C to drying 12~24 hours, obtains loading the carbonization trailing plants Japonica silk of potassium hydroxide；Under nitrogen protection, will
The carbonization trailing plants Japonica silk for loading potassium hydroxide is activated 0.5~2 hour in 600~1000 DEG C；Washed with boiling water after 100~140 DEG C
Dry 12~24 hours, obtain the compound duct carbon material of one-dimensional micropore-macropore；Wherein without metallic element carbonization trailing plants Japonica silk,
The mass ratio of potassium hydroxide and water is 1:4~8:200~600.
One-dimensional micropore-the macropore of bio-based of the invention is combined duct carbon material, and its microscopic appearance is tubulose, and length is 100 μ
M~300 μm, about 2~8 μm of caliber, 0.2~0.5 μm of thickness of pipe wall, 1385~1395m of specific surface area2/ g, capacitance reaches 245~
265F/g, equivalent series resistance only has 0.16~0.18 Ω；By controlling the pattern of product, make with good charge-transporting
Can, there is huge potentiality application in terms of super capacitor material.It is one-dimensional micro- prepared by the present invention for prior art
Hole-macropore is combined duct carbon material, and its synthetic method is simple, and morphology controllable, synthesis cycle is short, and capacitance is higher and equivalent series
Resistance very little, with low cost, raw material is easy to get, green non-pollution.Experimentation only needs to calcine twice, centre potassium hydroxide solution
Immersion, you can obtain final product.The one-dimensional micropore of bio-based-macropore compound pore passage structure carbon material, on the one hand can provide compared with
Big specific surface area, allows substantial amounts of electric charge to be attached to the surfaces externally and internally of carbon material, so as to reach larger capacitance, another aspect one
The structure of dimension is again in itself good electric charge transmission bridge, is conducive to the quick transmission of electric charge, be greatly reduced material etc.
Effect series resistance.Whole technical process is simple, and low cost, effect is good, twice laid, environmental protection, beneficial to industrialization production.
Brief description of the drawings
The undressed optical photograph of Fig. 1 trailing plants Japonica (A) and transmission electron microscope photo (B).
The scanning electricity of the different amplification of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 2 embodiments 1
Sub- microphotograph.
The nitrogen adsorption curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 3 embodiments 1.
The pore size distribution curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 4 embodiments 1.
The cyclic voltammetry curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 5 embodiments 1.
The impedance curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 6 embodiments 1.
The Raman curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of Fig. 7 embodiments 1.
Specific embodiment
The present invention is illustrated with specific embodiment below, its purpose is only that and is best understood from present disclosure and unrestricted
Protection scope of the present invention.
Embodiment 1
Trailing plants Japonica is peeled off remove seed, is washed with deionized water and net is obtained within 12 hours trailing plants Japonica silk after 100 DEG C of dryings；In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 0.5 hour in 500 DEG C, obtain 250mg carbonization trailing plants Japonica silks；250mg carbonization trailing plants Japonica silks are placed in
In dissolved with the 100g distilled water of 1g NaOH, heated 1 hour in 100 DEG C, be washed with deionized small after 100 DEG C of dryings 12
When, carbonization trailing plants Japonica silks of the 250mg without metallic element is obtained, to avoid metallic element from causing material during electrochemistry is circulated
That expects is unstable；
The 50g stirrings 0.5 in distilled water of the carbonization trailing plants Japonica silk immersion without metallic element dissolved with 1g potassium hydroxide by 250mg
Hour, suction filtration, in 100 DEG C of dryings 12 hours, obtains the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide；Under nitrogen protection, will
The carbonization trailing plants Japonica silk of 120mg load potassium hydroxide is activated 0.5 hour in 800 DEG C；Wash small after 120 DEG C of dryings 24 with boiling water
When, obtain the compound duct carbon material 1 of one-dimensional micropore-macropore.
Fig. 1 (A) provides the optical photograph of undressed trailing plants Japonica, and trailing plants Japonica has a shell, and there is very thin hair surface inside of splitting
Silk spills, and a sheet seed is arranged at the bottom per Shu Maosi, and Fig. 1 (B) is that the transmission electron microscope of untreated trailing plants Japonica silk shines
Piece, it is seen then that trailing plants Japonica silk is tubular structure, 29 μm of external diameter, 25 μm of internal diameter, 2 μm of tube wall.
Fig. 2 is the electron scanning micrograph of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based of embodiment 1.
From Figure 2 it can be seen that the compound duct carbon material 1 of the one-dimensional micropore-macropore of the gained bio-based of embodiment 1 is one-dimensional tubular structure, compared to not
The material for the treatment of has obvious contraction, about 4 μm of caliber, thickness of pipe wall about 250nm, 100 μm of length；It is one-dimensional micro- that Fig. 3 provides bio-based
The nitrogen adsorption curve of the compound duct carbon material 1 of hole-macropore, is I type adsorption curve, and specific surface area (BET) is 1394m2/g.Figure
4 pore-size distributions for providing the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based, from fig. 4, it can be seen that duct is main contained by material
It is micropore, also has an obvious peak in big porose area.Fig. 5 provides following for the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based
Ring volt-ampere curve, is typical electric double layer capacitance cyclic voltammetry curve, and the capacitance for calculating product according to Fig. 5 is 265F/
g.Fig. 6 provides the impedance curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based, and the radius of the semicircle of high frequency region is represented
Charge transfer resistance, the slope of the straight line of low frequency range represents electrolyte diffusion resistance, and it is one-dimensional micro- to calculate bio-based according to Fig. 6
The equivalent series resistance of the compound duct carbon material 1 of hole-macropore is 0.16 Ω；Fig. 7 provides the one-dimensional micropore of bio-based-macropore composite holes
The Raman spectrum of road carbon material 1, primitive curve can be divided into D bands and G bands, wherein, D bands represent agraphitic carbon in material, G band generations
Graphitized carbon in table material, is fitted by swarming, and the ratio that can calculate agraphitic carbon and graphitized carbon is 64:18.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based is one-dimensional tubulose knot
Structure, length is 100 μm, 4 μm of caliber, 0.25 μm of thickness of pipe wall；The mass ratio of wherein agraphitic carbon and graphitized carbon is about 64:18.
Embodiment 2
Trailing plants Japonica is peeled off remove seed, is washed with deionized water and net is obtained within 24 hours trailing plants Japonica silk after 120 DEG C of dryings；In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 1 hour in 600 DEG C, obtain 250mg carbonization trailing plants Japonica silks；250mg carbonization trailing plants Japonica silks are placed in molten
Have in the 50mL distilled water of 2.5g NaOH, heated 5 hours in 120 DEG C, be washed with deionized small after 120 DEG C of dryings 24
When, carbonization trailing plants Japonica silks of the 250mg without metallic element is obtained, to avoid metallic element from causing material during electrochemistry is circulated
That expects is unstable；
250mg is stirred in 100mL distilled water of the carbonization trailing plants Japonica silk immersion without metallic element dissolved with 2g potassium hydroxide
60 minutes；Suction filtration, in 120 DEG C of dryings 24 hours, obtains the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide；Under nitrogen protection,
The carbonization trailing plants Japonica silk of 120mg load potassium hydroxide is activated 1 hour in 600 DEG C；Wash small after 100 DEG C of dryings 12 with boiling water
When, obtain the compound duct carbon material 2 of the one-dimensional micropore-macropore of bio-based.
The compound duct carbon material 2 of the one-dimensional micropore-macropore of the gained bio-based of embodiment 2 is one-dimensional tubular structure compared to untreated
Material have obvious contraction, about 2 μm of caliber, about 0.230 μm of thickness of pipe wall, 200 μm of length；One-dimensional micropore-the macropore of bio-based is multiple
The nitrogen adsorption curve for closing duct carbon material 1 is similar with Fig. 3, is I type adsorption curve, and specific surface area (BET) is 1385m2/g；It is raw
The pore-size distribution of the compound duct carbon material 2 of the one-dimensional micropore-macropore of thing base is similar with Fig. 4, and duct is mainly micropore contained by material,
Big porose area also has an obvious peak.The cyclic voltammetry curve and Fig. 5 of the compound duct carbon material 2 of the one-dimensional micropore-macropore of bio-based
It is similar, it is typical electric double layer capacitance cyclic voltammetry curve, the capacitance for calculating product is 255F/g；Bio-based is one-dimensional micro-
The impedance curve of the compound duct carbon material 2 of hole-macropore is similar with Fig. 6, and the radius of the semicircle of high frequency region represents charge transfer resistance,
The slope of the straight line of low frequency range represents electrolyte diffusion resistance, calculates the compound duct carbon materials of the one-dimensional micropore-macropore of bio-based
The equivalent series resistance of material 2 is 0.17 Ω；The Raman spectrum and Fig. 7 classes of the compound duct carbon material 2 of the one-dimensional micropore-macropore of bio-based
Seemingly, primitive curve can be divided into D bands and G bands, wherein, D bands represent agraphitic carbon in material, and G bands represent graphitized carbon in material,
It is fitted by swarming, the ratio that can calculate agraphitic carbon and graphitized carbon is about 62：15.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based is one-dimensional tubulose knot
Structure, length is 200 μm, and caliber is 2 μm, 0.23 μm of thickness of pipe wall；The mass ratio of wherein agraphitic carbon and graphitized carbon is about 62:
15。
Embodiment 3
Trailing plants Japonica is peeled off remove seed, is washed with deionized water and net is obtained within 18 hours trailing plants Japonica silk after 140 DEG C of dryings；In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 3 hours in 700 DEG C, obtain 250mg carbonization trailing plants Japonica silks；250mg carbonization trailing plants Japonica silks are placed in molten
Have in the 75mL distilled water of 7.5g NaOH, heated 3 hours in 140 DEG C, be washed with deionized small after 140 DEG C of dryings 18
When, carbonization trailing plants Japonica silks of the 250mg without metallic element is obtained, to avoid metallic element from causing material during electrochemistry is circulated
That expects is unstable；
250mg is stirred in 150mL distilled water of the carbonization trailing plants Japonica silk immersion without metallic element dissolved with 1.5g potassium hydroxide
Mix 90 minutes, suction filtration, in 140 DEG C of dryings 18 hours, obtain the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide；In nitrogen protection
Under, the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide is activated 2 hours in 1000 DEG C；Washed with boiling water after 140 DEG C of dryings 18
Hour, obtain the compound duct carbon material 3 of one-dimensional micropore-macropore.
The electron scanning micrograph and Fig. 2 of the compound duct carbon material 3 of the one-dimensional micropore-macropore of bio-based of embodiment 3
Similar, the compound duct carbon material 3 of the one-dimensional micropore-macropore of the gained bio-based of embodiment 3 is one-dimensional tubular structure compared to untreated
Material has obvious contraction, about 8 μm of caliber, about 0.450 μm of thickness of pipe wall, 300 μm of length；One-dimensional micropore-the macropore of bio-based is combined
The nitrogen adsorption curve of duct carbon material 3 is similar with Fig. 3, is I type adsorption curve, and specific surface area (BET) is 1395m2/g；It is biological
The pore-size distribution of the compound duct carbon material 3 of the one-dimensional micropore-macropore of base is similar with Fig. 4, and duct is mainly micropore contained by material, big
Porose area also has an obvious peak.The cyclic voltammetry curve and Fig. 5 classes of the compound duct carbon material 3 of the one-dimensional micropore-macropore of bio-based
Seemingly, it is typical electric double layer capacitance cyclic voltammetry curve, the capacitance for calculating product is 245F/g；Bio-based is one-dimensional micro-
The impedance curve of the compound duct carbon material 3 of hole-macropore is similar with Fig. 6, and the radius of the semicircle of high frequency region represents charge transfer resistance,
The slope of the straight line of low frequency range represents electrolyte diffusion resistance, calculates the compound duct carbon materials of the one-dimensional micropore-macropore of bio-based
The equivalent series resistance of material 1 is 0.18 Ω；The Raman spectrum and Fig. 7 classes of the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based
Seemingly, primitive curve can be divided into D bands and G bands, wherein, D bands represent agraphitic carbon in material, and G bands represent graphitized carbon in material,
It is fitted by swarming, the ratio that can calculate agraphitic carbon and graphitized carbon is about 64:17.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of bio-based is one-dimensional tubulose knot
Structure, length is 300 μm, and caliber is 8 μm, 0.45 μm of thickness of pipe wall；The mass ratio of wherein agraphitic carbon and graphitized carbon is about 64:
17。
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
Specific implementation of the invention is confined to these explanations.For the person of ordinary skill of the art, can be according to the present invention
Technical scheme and inventive concept, make it is corresponding change and substitute, and performance or purposes are identical, should all be considered as of the invention
Protection domain.
Claims (2)
1. a kind of compound duct carbon material of the one-dimensional micropore-macropore of bio-based, is made up of, its feature agraphitic carbon and graphitized carbon
It is that the compound duct carbon material of the one-dimensional micropore-macropore of bio-based is one-dimensional tubular structure, length is 100~300 μm, caliber
About 2~8 μm, there are a large amount of micropores in 0.2~0.5 μm of thickness of pipe wall in tube wall；Wherein the mass ratio of agraphitic carbon and graphitized carbon is about
It is 3.5~4.5:1.
2. a kind of one-dimensional micropore-macropore of bio-based of claim 1 is combined the preparation method of duct carbon material, and building-up process is such as
Under：
Trailing plants Japonica is peeled off remove seed, is washed with deionized water and net is obtained within 12~24 hours trailing plants Japonica silk after 100~140 DEG C of dryings；In nitrogen
Under gas shielded, trailing plants Japonica silk is carbonized 0.5~3 hour in 500~700 DEG C, obtains carbonization trailing plants Japonica silk；Carbonization trailing plants Japonica silk is placed in molten
Have in the distilled water of NaOH, heated 1~5 hour in 100~140 DEG C, be washed with deionized dry after 100~140 DEG C
Dry 12~24 hours, obtain without metallic element carbonization trailing plants Japonica silk, with avoid metallic element electrochemistry circulate during
Cause the unstable of material；The mass ratio of carbonization trailing plants Japonica silk, NaOH and water is 1:4~30:200~400；
Stirred 30~90 minutes in distilled water by the carbonization trailing plants Japonica silk immersion without metallic element dissolved with potassium hydroxide, suction filtration,
In 100~140 DEG C to drying 12~24 hours, obtain loading the carbonization trailing plants Japonica silk of potassium hydroxide；Under nitrogen protection, will load
The carbonization trailing plants Japonica silk of potassium hydroxide is activated 0.5~2 hour in 600~1000 DEG C；Washed with boiling water after 100~140 DEG C of dryings
12~24 hours, obtain the compound duct carbon material of one-dimensional micropore-macropore；Carbonization trailing plants Japonica silk wherein without metallic element, hydrogen-oxygen
The mass ratio for changing potassium and water is 1:4~8:200~600.
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| CN113648966A (en) * | 2021-08-10 | 2021-11-16 | 南京航空航天大学 | Biomass porous carbon material and preparation method and application thereof |
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| CN102745689A (en) * | 2012-07-30 | 2012-10-24 | 重庆工商大学 | Method for preparing activated carbon by catalyzing and activating microorganism white-rot fungi or enzymes |
| CN103950918A (en) * | 2014-03-10 | 2014-07-30 | 苏州科技学院相城研究院 | Method using hypha as template for preparation of graphene tube with controllable aperture |
| CN105110314A (en) * | 2015-07-28 | 2015-12-02 | 大连理工大学 | Metal oxide hollow nanometer particle-embedded nitrogen-doped nanometer foamy carbon synthesis method |
| CN106185918A (en) * | 2016-07-19 | 2016-12-07 | 句容市百诚活性炭有限公司 | A kind of preparation method of the activated carbon of hierarchical porous structure |
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