CN105948042A - Preparation method of activated carbon for supercapacitors - Google Patents
Preparation method of activated carbon for supercapacitors Download PDFInfo
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- CN105948042A CN105948042A CN201610300981.0A CN201610300981A CN105948042A CN 105948042 A CN105948042 A CN 105948042A CN 201610300981 A CN201610300981 A CN 201610300981A CN 105948042 A CN105948042 A CN 105948042A
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- activated carbon
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- presoma
- super capacitors
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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Abstract
The invention discloses a preparation method of activated carbon for supercapacitors. The method comprises the steps of: crushing a pre-configured biomass material; subjecting the crushed biomass material to alkali treatment, then performing filtration to remove impurities from the alkali treated biomass material so as to obtain a precursor; then immersing the precursor in a potassium hydroxide solution to conduct supersonic vibration and stirring, and then performing filtering to obtain a modified precursor; heating the modified precursor, and pre-activating the modified precursor; adding a hydroxide of alkali into the modified precursor and conducting heating activation. The preparation method has a simple process, solves the problem of uneven pore distribution of carbon materials, and improves the structural consistency of carbon materials. The prepared carbon material has abundant pores, high specific surface area, and excellent capacitance characteristics, significantly improves the supercapacitor capacity and high-rate charge-discharge capacity, has good circulation performance, prolongs the supercapacitor life, and has very good economical efficiency and adaptability.
Description
Technical field
The present invention relates to electrode material preparation field, particularly to the preparation method of a kind of activated carbon for super capacitors.
Background technology
The ultracapacitor grown up in recent years, both there is high-specific-power and the cyclicity of conventional physical electric capacity, there is again the high-energy-density characteristic of electrochmical power source, so, it can meet the use condition requiring high-specific-power, can meet again the use condition requiring high-energy-density.Due to the Large Copacity energy-storage property that ultracapacitor has an excellent pulse charge-discharge performance and conventional physical electric capacity does not has, the application at high energy pulse laser has caused the extensive concern of people.Meanwhile, because its storage energy is big, light weight, can unlimited discharge and recharge and be used as computer system and the stand-by power supply without communication apparatus of rationing the power supply by people.Along with the rise of environmental-protecting type electric automotive research, ultracapacitor independently or can combine the power-supply system as electric automobile with secondary cell (such as lead-acid battery or lithium ion battery), and be widely used prospect.
In the various electrode materials of ultracapacitor, cheap absorbent charcoal material be most widely used general be also the class that technology is the most ripe.Absorbent charcoal material has excellent heat conductivility and electric conductivity, and its density is low, and resist chemical performance is good, and thermal coefficient of expansion is little, and elastic modelling quantity is the highest.The variforms such as powder, bulk, fiber, cloth can be prepared by distinct methods, the most also have multiple allotrope (such as graphite, diamond, fullerene), also can have different space structures because of the difference of degree of graphitization, therefore be widely used in electrochemical field and make electrode material.
Through retrieval, have a kind of with petroleum coke as raw material disclosed in prior art, through grinding, prepare activated carbon for super capacitors with potassium hydroxide for activator；Being also disclosed a kind of with the hard fruit shells such as Fructus Pruni shell, peach shell or corn cob as raw material, with a certain amount of phosphoric acid as activator, potassium dihydrogen phosphate or sodium dihydrogen phosphate are that expanding agent is prepared specific capacitance and reached the activated carbon of 200F/g；One being also disclosed with starch (oxidative crosslinked starch, Semen Maydis cationic starch, graft copolymerization starch, soluble starch or tapioca) as raw material, potassium hydroxide is the method that activator produces activated carbon for super capacitors.
But the activated carbon specific surface area that said method is prepared and capacitance are the most relatively low, and material with carbon element distribution of pores is uneven, can affect the service life of ultracapacitor, its performance need to be improved further.
So, develop a kind of method for preparation of active carbon that can improve activated carbon specific surface area and capacitance, be insider's urgent problem.
Summary of the invention
In view of this, the present invention provides the preparation method of a kind of activated carbon for super capacitors.This preparation method can prepare the material with carbon element abundant, that specific surface area is high, capacitance characteristic is excellent that portals, and significantly improves capacity of super capacitor and high-rate charge-discharge capability.
In order to realize foregoing invention purpose, the present invention provides techniques below scheme:
The preparation method of a kind of activated carbon for super capacitors, comprises the steps:
Pulverize the biological material being pre-configured with；
Described biological material after pulverizing processes through alkali, then by being filtrated to get presoma, to get rid of the impurity in the biological material after alkali processes；
The leaching of described presoma is put in potassium hydroxide solution, carries out supersonic vibration and stirring, then by being filtrated to get modified presoma；
Described modified presoma is heated, makes described modified presoma carry out pre-activate；
The hydroxide of alkali, and heat-activated is added in described modified presoma.
Preferably, described biological material includes starch, lignin, corn cob, rice husk, the wheat head, trees, coconut husk, shell, leaves or straw.
Further, in one embodiment, the concentration of the described potassium hydroxide solution putting described presoma for leaching is 0.01-5 mol/L.
Further, in one embodiment, the particle mean size of described biological material after crushed is 0.1-0.5 cm.
Further, in one embodiment, when the leaching of described presoma is put in potassium hydroxide solution, through the supersonic vibration that frequency is 20-50 KHz.
Further, in one embodiment, when the leaching of described presoma is put in potassium hydroxide solution, through the stirring that speed is 100-1800 r/min.
Further, in one embodiment, the leaching of described presoma puts that to carry out time of supersonic vibration and stirring in potassium hydroxide solution be 0.1-72 h.
Further, in one embodiment, heating-up temperature when described modified presoma carries out pre-activate is 100-300 DEG C or 700-900 DEG C.
Further, in one embodiment, heat time heating time when described modified presoma carries out pre-activate is 0.1-10 h.
Beneficial effect: this preparation method technique is simple, and environmental benefit is good, and the pre-activate time is short, reduces energy consumption；On the one hand the biomass such as straw can be recycled, on the other hand can prepare ultracapacitor material with carbon element, the problem uneven in order to solve material with carbon element distribution of pores, make the structural integrity of material with carbon element improve；The material with carbon element hole prepared is abundant, specific surface area is high, capacitance characteristic is excellent, significantly improves capacity of super capacitor and high-rate charge-discharge capability, and cyclicity is good, extends the ultracapacitor life-span, has good economy and adaptability.
Detailed description of the invention
The invention discloses the preparation method of a kind of activated carbon for super capacitors, those skilled in the art can use for reference present disclosure, is suitably modified technological parameter and realizes.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are considered as being included in the present invention.Method and the application of the present invention are described by preferred embodiment, method described herein and application substantially can be modified in without departing from present invention, spirit and scope or suitably change and combine by related personnel, realizes and applies the technology of the present invention.
This application provides the preparation method of a kind of activated carbon for super capacitors, comprise the steps: to pulverize the biological material being pre-configured with；Described biological material after pulverizing processes through alkali, then by being filtrated to get presoma, to get rid of the impurity in the biological material after alkali processes；The leaching of described presoma is put in potassium hydroxide solution, carries out supersonic vibration and stirring, then by being filtrated to get modified presoma；Described modified presoma is heated, makes described modified presoma carry out pre-activate；The hydroxide of alkali, and heat-activated is added in described modified presoma.Preferably, described biological material includes starch, lignin, corn cob, rice husk, the wheat head, trees, coconut husk, shell, leaves or straw.
Further, in one embodiment, the concentration of the described potassium hydroxide solution putting described presoma for leaching is 0.01-5 mol/L.
Further, in one embodiment, the particle mean size of described biological material after crushed is 0.1-0.5 cm.
Further, in one embodiment, when the leaching of described presoma is put in potassium hydroxide solution, through the supersonic vibration that frequency is 20-50 KHz.
Further, in one embodiment, when the leaching of described presoma is put in potassium hydroxide solution, through the stirring that speed is 100-1800 r/min.
Further, in one embodiment, the leaching of described presoma puts that to carry out time of supersonic vibration and stirring in potassium hydroxide solution be 0.1-72 h.
Further, in one embodiment, heating-up temperature when described modified presoma carries out pre-activate is 100-300 DEG C or 700-900 DEG C.
Further, in one embodiment, heat time heating time when described modified presoma carries out pre-activate is 0.1-10 h.
Compared with the activated carbon of ultracapacitor in prior art, the activated carbon that preparation method set forth herein prepares has the advantage that
(1) using biological material to prepare material with carbon element, it is possible to biomass to be recycled, technique is simple, and the suitability is extensive, and good in economic efficiency, environmental benefit is good.
(2) in the pre-activate stage, presoma leaching is put in potassium hydroxide solution, by supersonic vibration and the method for modifying of stirring, compares traditional direct method by presoma with potassium hydroxide mechanical mixture and have the advantage that
Activated carbon pre-activate pore size distribution is uniform, and the activated carbon specific surface area after activation is high；
Can save in a large number the pre-activate time, reduce energy consumption；
The activated carbon concordance prepared is good, is used for making ultracapacitor specific energy high, good cycle.
Below in conjunction with embodiment, technical scheme it is expanded on further:
Embodiment
1
Weigh 10g corn straw, be put in pulverizer pulverizing, mean diameter 1mm.It is in 0.1mol/L potassium hydroxide solution that corn straw powder after pulverizing is placed in containing 300ml concentration, stirs 20min.Filtration washing obtains pure biomass.Pure biomass are placed in the beaker of the potassium hydroxide solution that 500ml concentration is 1mol/L, ultrasound wave dispersion 25
Min, supersonic frequency 50KHz, stir speed (S.S.) is 400
R/min, mixing time is 25 min, and filtration washing obtains alkali modification biomass.Being placed in tube furnace by 5g alkali modification activated carbon, arrange heating parameters, temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, be incubated 30min, cooling obtains pre-activate activated carbon.Mix by the mass ratio of 100:7 with potassium hydroxide crystal with pre-activate activated carbon, be placed on Muffle furnace, be warming up to 800 DEG C, temperature retention time 2h.Obtain activated carbon.
Prepared material with carbon element is carried out electro-chemical test discovery, prepares specific surface area 2700m2/g, the activated carbon for super capacitors of specific capacity 272g/F.
Embodiment
2
Weigh 10g coconut husk, be put in pulverizer pulverizing, mean diameter 1mm.It is in 0.1mol/L potassium hydroxide solution that corn straw powder after pulverizing is placed in containing 300 ml concentration, stirs 20min.Filtration washing obtains pure biomass.Pure biomass being placed in the beaker that 500ml concentration is 1mol/L potassium hydroxide solution, ultrasound wave dispersion 25min, supersonic frequency 50 KHz, stir speed (S.S.) 400 r/min, mixing time 25 min, filtration washing obtains alkali modification biomass.Being placed in tube furnace by 5g alkali modification activated carbon, arrange heating parameters, temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, be incubated 30 min, cooling obtains pre-activate activated carbon.Mix by the mass ratio of 100:7 with potassium hydroxide crystal with pre-activate activated carbon, be placed on Muffle furnace, be warming up to 800 DEG C, temperature retention time 2h.Obtain activated carbon.
Prepared material with carbon element is carried out electro-chemical test discovery, prepares specific surface area 2720m2/g, the activated carbon for super capacitors of specific capacity 282g/F.
Embodiment
3
Weigh 10g lignin, be put in pulverizer pulverizing, mean diameter 1mm.It is in 0.1mol/L potassium hydroxide solution that corn straw powder after pulverizing is placed in containing 300ml concentration, mixing time 20min.Filtration washing obtains pure biomass.Pure biomass are placed in 500
Ml concentration is in the beaker of 1 mol/L potassium hydroxide solution, ultrasonic dispersing time 25min, supersonic frequency 50KHz, stir speed (S.S.) 400 r/min, mixing time 25min, and filtration washing obtains alkali modification biomass.Being placed in tube furnace by 5g alkali modification activated carbon, arrange heating parameters, temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, be incubated 30 min, cooling obtains pre-activate activated carbon.Mix by the mass ratio of 100:7 with potassium hydroxide crystal with pre-activate activated carbon, be placed on Muffle furnace, be warming up to 800 DEG C, temperature retention time 2h.Obtain activated carbon.
Prepared material with carbon element is carried out electro-chemical test discovery, prepares specific surface area 2710m2/g, the activated carbon for super capacitors of specific capacity 275g/F.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of an activated carbon for super capacitors, it is characterised in that comprise the steps:
Pulverize the biological material being pre-configured with；
Described biological material after pulverizing processes through alkali, then by being filtrated to get presoma, to get rid of the impurity in the biological material after alkali processes；
The leaching of described presoma is put in potassium hydroxide solution, carries out supersonic vibration and stirring, then by being filtrated to get modified presoma；
Described modified presoma is heated, makes described modified presoma carry out pre-activate；
The hydroxide of alkali, and heat-activated is added in described modified presoma.
The preparation method of activated carbon for super capacitors the most according to claim 1, it is characterised in that described biological material includes starch, lignin, corn cob, rice husk, the wheat head, trees, coconut husk, shell, leaves or straw.
The preparation method of activated carbon for super capacitors the most according to claim 2, it is characterised in that the concentration being used for the described potassium hydroxide solution that described presoma is put in leaching is 0.01-5 mol/L.
The preparation method of activated carbon for super capacitors the most according to claim 3, it is characterised in that the particle mean size of described biological material after crushed is 0.1-0.5 cm.
The preparation method of activated carbon for super capacitors the most according to claim 4, it is characterised in that when the leaching of described presoma is put in potassium hydroxide solution, through the supersonic vibration that frequency is 20-50 KHz.
The preparation method of activated carbon for super capacitors the most according to claim 4, it is characterised in that when the leaching of described presoma is put in potassium hydroxide solution, through the stirring that speed is 100-1800 r/min.
7. according to the preparation method of the activated carbon for super capacitors described in claim 5 or 6, it is characterised in that the leaching of described presoma puts that to carry out time of supersonic vibration and stirring in potassium hydroxide solution be 0.1-72 h.
The preparation method of activated carbon for super capacitors the most according to claim 7, it is characterised in that heating-up temperature when described modified presoma carries out pre-activate is 100-300 DEG C or 700-900 DEG C.
The preparation method of activated carbon for super capacitors the most according to claim 8, it is characterised in that heat time heating time when described modified presoma carries out pre-activate is 0.1-10 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629652A (en) * | 2016-12-29 | 2017-05-10 | 华南农业大学 | Biomass-based carbon material having high specific surface area and activation-free preparation method and application thereof |
| CN108117074A (en) * | 2016-11-28 | 2018-06-05 | 北京化工大学 | The method of the circulating and recovering of the preparation method of super-activated carbon and produced waste liquid and by-product carbonate |
| CN110902675A (en) * | 2019-10-28 | 2020-03-24 | 广西科学院 | Method for preparing special-shaped activated carbon and capacitance carbon by using lignin-modified inferior biomass |
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| CN101525132A (en) * | 2009-04-15 | 2009-09-09 | 广西师范大学 | Active carbon for super capacitor and a preparation method thereof |
| CN103539119A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for electrochemical energy storage device |
| CN105469999A (en) * | 2015-11-20 | 2016-04-06 | 浙江农林大学 | Method of preparing electrode material for carbon-based supercapacitor by taking bamboo powder as raw material |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525132A (en) * | 2009-04-15 | 2009-09-09 | 广西师范大学 | Active carbon for super capacitor and a preparation method thereof |
| CN103539119A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for electrochemical energy storage device |
| CN105469999A (en) * | 2015-11-20 | 2016-04-06 | 浙江农林大学 | Method of preparing electrode material for carbon-based supercapacitor by taking bamboo powder as raw material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117074A (en) * | 2016-11-28 | 2018-06-05 | 北京化工大学 | The method of the circulating and recovering of the preparation method of super-activated carbon and produced waste liquid and by-product carbonate |
| CN108117074B (en) * | 2016-11-28 | 2020-04-28 | 北京化工大学 | Preparation method of super activated carbon and method for recycling produced waste liquid and producing by-product carbonate |
| CN106629652A (en) * | 2016-12-29 | 2017-05-10 | 华南农业大学 | Biomass-based carbon material having high specific surface area and activation-free preparation method and application thereof |
| CN110902675A (en) * | 2019-10-28 | 2020-03-24 | 广西科学院 | Method for preparing special-shaped activated carbon and capacitance carbon by using lignin-modified inferior biomass |
| CN110902675B (en) * | 2019-10-28 | 2022-08-23 | 广西科学院 | Method for preparing special-shaped activated carbon and capacitance carbon by using lignin-modified inferior biomass |
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