CN108046254A - A kind of corncob derives active carbon electrode material and preparation method thereof - Google Patents
A kind of corncob derives active carbon electrode material and preparation method thereof Download PDFInfo
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- CN108046254A CN108046254A CN201711441936.8A CN201711441936A CN108046254A CN 108046254 A CN108046254 A CN 108046254A CN 201711441936 A CN201711441936 A CN 201711441936A CN 108046254 A CN108046254 A CN 108046254A
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Abstract
The invention discloses a kind of corncobs to derive active carbon electrode material and preparation method thereof.Specific step of preparation process is as follows：First, agricultural wastes corncob is soaked in the potassium hydroxide solution of various concentration, high-temperature calcination after drying；Then, the product of gained and potassium hydroxide are subjected to second of mixed grinding, high-temperature calcination according to different ratios, and then corncob is made and derives classifying porous absorbent charcoal material.The corncob of the present invention, which derives classifying porous absorbent charcoal material, has micropore and mesoporous double grading structure.Electrode material for super capacitor is used as, shows good specific capacity and excellent high rate performance.This preparation method has the advantages that novel, easy to operate, manufacturing cost is low etc..
Description
Technical field
The present invention relates to a kind of preparation methods of electrode material more particularly to a kind of corncob to derive classifying porous activated carbon
Electrode material for super capacitor and preparation method；Belong to new energy materials field.
Background technology
Biomass carbon material is subject to the extensive concern of scientific research personnel as electrode material for super capacitor.Common biomass
Mainly traditional agriculture and forestry biomass, including various crop stalks, timber, shell, fruit stone, rice husk etc..Wherein, agricultural is useless
Biomass derived carbon material is abandoned due to having many advantages, such as of low cost, environmental-friendly, flourishing porous structure, made
Become current research hotspot for electrode material for super capacitor.But agriculture waste biomass derived carbon material preparation process is numerous
Trivial, condition is harsh, and specific surface area is smaller, and easy-regulating does not limit its application in ultracapacitor to pore-size distribution.
For agriculture waste biomass derived carbon material there are the problem of, Ding (Chem Eng Journal, 2013,
225:Sulfuric acid catalysis hydrolysis of corncob 300-305) et al. is used, hydrothermal carbonization is finally activated, and then synthesizes and have height
Specific surface area（3611 m2/g）Spherical porous charcoal.But the preparation process of the porous carbon material is complicated, condition requirement is harsh,
Repeatability is low.Li et al. people (Energy Environ. Sci. 2016, 9, 102-106) by activation of potassium hydroxide and after
Continuous ammonia nitrating is prepared for the classifying porous activated carbon of nitrating, and good electrification is showed as electrode material for super capacitor
Learn performance.Although the preparation process of the porous active Carbon Materials is simple, the stronger ammonia environmental pollution of corrosivity is more
Seriously.Therefore, finding a kind of controllable porous carbon preparation method for material in simple environmentally protective aperture, there is great science to anticipate
Justice and social benefit.
The content of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned existing technology of preparing, a kind of simple, safety high ratio is provided
Surface area corncob derives classifying porous activated carbon electrode material for super capacitor, while has micropore and mesoporous double-hole knot
Structure, while the pore size of activated carbon can carry out Effective Regulation；Corncob prepared by this method derives classifying porous activated carbon and surpasses
When grade capacitor electrode material is used as electrode material for super capacitor, its specific capacity and high rate performance can be greatly improved.
The preparation method of the present invention, preparation process is simple, and safety coefficient is high, without template and with high specific surface.
The present invention is realized by following measures：
The invention discloses a kind of corncobs to derive active carbon electrode material, it is characterized in that being made of following methods：
（1）Agricultural wastes corncob is soaked in the potassium hydroxide solution that concentration is 15%~50%, controls corncob and hydrogen
The ratio of potassium oxide is 1:1~6, take out drying after abundant impregnate, and carry out high-temperature calcination, calcining heat for 600 DEG C~
1000 DEG C, soaking time is 1~6 h；Substance after calcining is washed, centrifuge and drying process after, obtain living for the first time
Change product；
（2）It is 1 by weight by step 1 products therefrom and potassium hydroxide：0.5~4 carries out being fully ground mixing, carries out high temperature and forges
It burns, calcining heat is 600 DEG C~1000 DEG C, and soaking time is 1~6 h, is then washed, centrifuged and drying process obtains jade
Rice core derives active carbon electrode material.
The electrode material, it is preferred that the absorbent charcoal material has the dual pore structure of micropore-mesopore, wherein micropore
Size is 0.1~2 nm, and macropore range is about 2~10 nm, and specific surface area is 1000~3000 m2/g.
The electrode material, it is preferred that in step 1, the concentration of the potassium hydroxide solution is 25%~30%；Step 2
In, the product is 1 by weight proportion with potassium hydroxide:1~3.
The electrode material, it is preferred that the wash solution is dilute hydrochloric acid and deionized water；The PH of solution after washing
It is worth for 7；The temperature of the drying process is 50 DEG C~120 DEG C, and drying time is 6~24 h.
The invention also discloses the preparation sides that a kind of corncob derives classifying porous activated carbon electrode material for super capacitor
Method, it is characterized in that being as follows：
（1）Agricultural wastes corncob is soaked in concentration in 15%~50% potassium hydroxide solution, fully to be taken out after immersion dry
After dry, high-temperature calcination is carried out, calcining heat is 600 DEG C~800 DEG C, and soaking time is 2~4 h；Substance after calcining is carried out
After washing, centrifugation and drying process, the product activated for the first time is obtained；
（2）It is 1 by weight proportion by step 1 products therefrom and potassium hydroxide:4~2:1 carries out being sufficiently mixed grinding, carries out high temperature
Calcining, calcining heat are 600 DEG C~800 DEG C, and soaking time is 2~4 h, is then washed, centrifuged and drying process obtains
Corncob derives classifying porous activated carbon electrode material for super capacitor.
The preparation method, it is preferred that in step 1, the concentration of the potassium hydroxide solution is 25%~30%；Step 2
In, the product is 1 by weight proportion with potassium hydroxide:1~5.
The preparation method, it is preferred that the wash solution is dilute hydrochloric acid and deionized water；The PH of solution after washing
It is worth for 7；The temperature of the drying process is 50 DEG C~70 DEG C, and drying time is 8~12 h.
Compared with prior art, beneficial effects of the present invention are：
（1）Corncob prepared by the method for the present invention derives classifying porous activated carbon has micropore and mesoporous dual pore structure simultaneously,
The pore size of activated carbon can carry out Effective Regulation simultaneously.
（2）The present invention effectively make use of agricultural wastes corncob, significantly increase the added value of discarded object, and
Corncob only need to be carried out dual activation using potassium hydroxide and can obtain classifying porous activated carbon by the preparation process of the present invention, no
Need to be by the mould material with hierarchical porous structure and the experimental provision of complexity, condition is easily-controllable, and simple process and low cost is honest and clean,
Solve the problems, such as that conventional manufacturing process is complicated and mould material is not easy to find.
（3）Corncob prepared by the present invention derives classifying porous activated carbon electrode material for super capacitor as super capacitor
During device electrode material, high specific capacity and good high rate performance are shown.
Below with reference to attached drawing to the conceiving of the present invention, the technique effect of specific material structure and generation is made furtherly
It is bright, to be fully understood from the purpose of the present invention, feature and effect.
Description of the drawings
Fig. 1 is the graph of pore diameter distribution that corncob prepared by the embodiment of the present invention 1 derives active carbon electrode material；It is horizontal in figure
Coordinate is aperture, and ordinate is pore volume.
Fig. 2 is the scanning electron microscope (SEM) photograph that corncob prepared by the embodiment of the present invention 1 derives active carbon electrode material；
Fig. 3 is the transmission electron microscope picture that corncob prepared by the embodiment of the present invention 1 derives active carbon electrode material；
Fig. 4 is that constant current of the corncob derivative active carbon electrode material of the preparation of the embodiment of the present invention 1 under different current densities is filled
Discharge curve.In figure, abscissa is the time, and ordinate is voltage.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out in fact lower premised on the technology of the present invention
It applies, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to the spy being exemplified below
Determine embodiment.
Embodiment 1
Corncob is immersed in the potassium hydroxide solution that concentration is 25%, the ratio of corncob and potassium hydroxide is 1:3, fully
It is dry after immersion, 2 h are then calcined at 800 DEG C, then wash products therefrom with dilute hydrochloric acid and deionized water, until
The pH value of solution is 7, and by gained sediment, dry 12 hours obtain the product activated for the first time under conditions of 70 DEG C.
The product of first time activation and potassium hydroxide are pressed 1:3 are fully ground mixing in mortar, and are calcined at 800 DEG C
2 h wash products therefrom with dilute hydrochloric acid and deionized water, and until the pH value of solution is 7, gained is deposited in 70 DEG C
Under conditions of dry 12 hours obtain corncob and derive active carbon electrode material.
Obtained corncob derives the pore-size distribution of active carbon electrode material as shown in Figure 1, prepared as shown in Figure 1
Active carbon electrode material has micropore and mesoporous dual pore structure, and micropore average-size is about 2 nm, and mesoporous average-size is about
For 4 nm.
Fig. 2 and 3 is respectively the scanning electron microscope (SEM) photograph and transmission electron microscope picture that prepared corncob derives active carbon electrode material,
It can be seen that activated carbon prepared after re-activation has developed pore structure and while with micropore and mesoporous.
By the electrode material, binding agent and conductive charcoal according to 8:1:Nickel foam is coated to after 1 ratio grinding uniformly（1×1
cm）On be dried（70℃）, working electrode is made, under three-electrode system（Platinized platinum is used as to electrode, and Ag/AgCl electrodes are made
For reference electrode, the aqueous sodium persulfate solution of 1 M is as electrolyte）, its chemical property is tested.The combination electrode is in electricity
Current density is under 0.5 A/g, and specific capacitance is up to 298.1 F/g；When current density increases to 10 A/g, capability value is
253.2 F/g, capacitance fade is smaller, can retain 84.9% capacitance, shows excellent high rate performance.(Fig. 4).
Embodiment 2
Corncob is immersed in the potassium hydroxide solution that concentration is 15%, the ratio of corncob and potassium hydroxide is 1:1, fully
It is dry after immersion, 6 h are then calcined at 600 DEG C, then wash products therefrom with dilute hydrochloric acid and deionized water, until
The pH value of solution is 7, and by gained sediment, dry 24 hours obtain the product activated for the first time under conditions of 50 DEG C.
The product of first time activation and potassium hydroxide are pressed 1:0.5 is fully ground mixing in mortar, and is forged at 600 DEG C
6 h are burnt, products therefrom is washed with dilute hydrochloric acid and deionized water, until the pH value of solution is 7, gained is deposited in 50
Dry 24 hours obtain corncob derivative active carbon electrode material under conditions of DEG C.
Obtained corncob derives in active carbon electrode material, and micropore average-size is about 0.1 nm, mesoporous average
Size is about 10 nm.
Its chemical property is tested using method same as Example 1.The combination electrode is in current density
Under 0.5 A/g, specific capacitance is up to 272.6 F/g；When current density increases to 10 A/g, capability value is 265.5 F/g,
Capacitance fade is smaller, can retain 97.4% capacitance, shows excellent high rate performance.
Embodiment 3
Corncob is immersed in the potassium hydroxide solution that concentration is 50%, the ratio of corncob and potassium hydroxide is 1:6, fully
It is dry after immersion, 1 h is then calcined at 1000 DEG C, is then washed products therefrom with dilute hydrochloric acid and deionized water, directly
PH value to solution is 7, and by gained sediment, dry 6 hours obtain the product activated for the first time under conditions of 120 DEG C.
The product of first time activation and potassium hydroxide are pressed 1:6 are fully ground mixing in mortar, and are forged at 1000 DEG C
1 h is burnt, products therefrom is washed with dilute hydrochloric acid and deionized water, until the pH value of solution is 7, by being deposited in for gained
Dry 6 hours obtain corncob derivative active carbon electrode material under conditions of 120 DEG C.
Obtained corncob derives in active carbon electrode material, and micropore average-size is about 1 nm, mesoporous average ruler
Very little about 2 nm.
Its chemical property is tested using method same as Example 1.The combination electrode is in current density
Under 0.5 A/g, specific capacitance is up to 308.5 F/g；When current density increases to 10 A/g, capability value is 253.5 F/g,
Capacitance fade is smaller, can retain 82.1% capacitance, shows excellent high rate performance.
Embodiment 4
Corncob is immersed in the potassium hydroxide solution that concentration is 35%, the ratio of corncob and potassium hydroxide is 1:2, fully
It is dry after immersion, 1 h is then calcined at 1000 DEG C, is then washed products therefrom with dilute hydrochloric acid and deionized water, directly
PH value to solution is 7, and by gained sediment, dry 6 hours obtain the product activated for the first time under conditions of 120 DEG C.
The product of first time activation and potassium hydroxide are pressed 1:6 are fully ground mixing in mortar, and are calcined at 600 DEG C
6 h wash products therefrom with dilute hydrochloric acid and deionized water, and until the pH value of solution is 7, gained is deposited in 90 DEG C
Under conditions of dry 12 hours obtain corncob and derive active carbon electrode material.
Obtained corncob derives in active carbon electrode material, and micropore average-size is about 1.5 nm, mesoporous average
Size is about 5 nm.
Its chemical property is tested using method same as Example 1.The combination electrode is in current density
Under 0.5 A/g, specific capacitance is up to 327.6 F/g；When current density increases to 10 A/g, capability value is 285.3 F/g,
Capacitance fade is smaller, can retain 87.1% capacitance, shows excellent high rate performance.
Claims (7)
1. a kind of corncob derives active carbon electrode material, it is characterized in that being made of following methods：
（1）Agricultural wastes corncob is soaked in the potassium hydroxide solution that concentration is 15%~50%, controls corncob and hydrogen
The ratio of potassium oxide is 1:1~6, take out drying after abundant impregnate, and carry out high-temperature calcination, calcining heat for 600 DEG C~
1000 DEG C, soaking time is 1~6 h；Substance after calcining is washed, centrifuge and drying process after, obtain living for the first time
Change product；
（2）It is 1 by weight by step 1 products therefrom and potassium hydroxide：0.5~4 carries out being fully ground mixing, carries out high temperature and forges
It burns, calcining heat is 600 DEG C~1000 DEG C, and soaking time is 1~6 h, is then washed, centrifuged and drying process obtains jade
Rice core derives active carbon electrode material.
2. electrode material according to claim 1, it is characterized in that, the absorbent charcoal material has micropore-mesopore double-hole
Structure, wherein pore size are 0.1~2 nm, and macropore range is about 2~10 nm, and specific surface area is 1000~3000 m2/g.
3. electrode material according to claim 1 or 2, it is characterized in that, in step 1, the concentration of the potassium hydroxide solution
For 25%~30%；In step 2, the product is 1 by weight proportion with potassium hydroxide:1~3.
4. electrode material according to claim 1 or 2, it is characterized in that, the wash solution is dilute hydrochloric acid and deionized water；
The pH value of solution after washing is 7；The temperature of the drying process is 50 DEG C~120 DEG C, and drying time is 6~24 h.
5. a kind of corncob derives the preparation method of classifying porous activated carbon electrode material for super capacitor, it is characterized in that specific step
It is rapid as follows：
（1）Agricultural wastes corncob is soaked in concentration in 15%~50% potassium hydroxide solution, fully to be taken out after immersion dry
After dry, high-temperature calcination is carried out, calcining heat is 600 DEG C~800 DEG C, and soaking time is 2~4 h；Substance after calcining is carried out
After washing, centrifugation and drying process, the product activated for the first time is obtained；
（2）It is 1 by weight proportion by step 1 products therefrom and potassium hydroxide:4~2:1 carries out being sufficiently mixed grinding, carries out high temperature
Calcining, calcining heat are 600 DEG C~800 DEG C, and soaking time is 2~4 h, is then washed, centrifuged and drying process obtains
Corncob derives classifying porous activated carbon electrode material for super capacitor.
6. preparation method according to claim 1, it is characterized in that, in step 1, the concentration of the potassium hydroxide solution is
25%~30%；In step 2, the product is 1 by weight proportion with potassium hydroxide:1~5.
7. preparation method according to claim 1, it is characterized in that, the wash solution is dilute hydrochloric acid and deionized water；It washes
The pH value of solution after washing is 7；The temperature of the drying process is 50 DEG C~70 DEG C, and drying time is 8~12 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109110756A (en) * | 2018-10-24 | 2019-01-01 | 济南大学 | Derivative carbon electrode material of a kind of homogeneous corncob and preparation method thereof |
| CN109850866A (en) * | 2019-01-30 | 2019-06-07 | 青岛大学 | A kind of classifying porous carbon material and preparation method thereof for flexible super capacitor |
| CN112441581A (en) * | 2020-11-25 | 2021-03-05 | 华南理工大学 | Purple-root water hyacinth-based graded porous carbon material, preparation method thereof and application thereof in super capacitor |
| CN113800515A (en) * | 2021-10-29 | 2021-12-17 | 哈尔滨工业大学 | Preparation method of nitrogen-doped activated carbon and multi-hydroxide/biomass porous carbon nano composite electrode material |
| CN113880085A (en) * | 2021-11-17 | 2022-01-04 | 常州大学 | Preparation method of biomass activated carbon for supercapacitor and supercapacitor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109110756A (en) * | 2018-10-24 | 2019-01-01 | 济南大学 | Derivative carbon electrode material of a kind of homogeneous corncob and preparation method thereof |
| CN109850866A (en) * | 2019-01-30 | 2019-06-07 | 青岛大学 | A kind of classifying porous carbon material and preparation method thereof for flexible super capacitor |
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| CN112441581A (en) * | 2020-11-25 | 2021-03-05 | 华南理工大学 | Purple-root water hyacinth-based graded porous carbon material, preparation method thereof and application thereof in super capacitor |
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| CN113800515B (en) * | 2021-10-29 | 2022-12-20 | 哈尔滨工业大学 | Preparation method of nitrogen-doped activated carbon and multi-hydroxide/biomass porous carbon nano composite electrode material |
| CN113880085A (en) * | 2021-11-17 | 2022-01-04 | 常州大学 | Preparation method of biomass activated carbon for supercapacitor and supercapacitor |
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