CN105948042B - A kind of preparation method of activated carbon for super capacitors - Google Patents
A kind of preparation method of activated carbon for super capacitors Download PDFInfo
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- CN105948042B CN105948042B CN201610300981.0A CN201610300981A CN105948042B CN 105948042 B CN105948042 B CN 105948042B CN 201610300981 A CN201610300981 A CN 201610300981A CN 105948042 B CN105948042 B CN 105948042B
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- presoma
- activated carbon
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- super capacitors
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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
- C01P2006/12—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 kind of preparation method of activated carbon for super capacitors, comprise the following steps：Crush the biological material being pre-configured with；By the biological material after crushing through alkali process, then by being filtrated to get presoma, to get rid of the impurity in the biological material after alkali process；Presoma leaching is put ultrasonic vibration and stirring are carried out in potassium hydroxide solution, then by being filtrated to get modified presoma；The modified presoma is heated, the modified presoma is carried out pre-activate；The hydroxide of alkali, and heat-activated are added in the modified presoma.The preparation method technique is simple, solves the problems, such as carbon material distribution of pores inequality, improves the structural integrity of carbon material；The carbon material hole prepared is enriched, specific surface area is high, capacitance characteristic is excellent, significantly improves capacity of super capacitor and high-rate charge-discharge capability, cyclicity is good, extends the ultracapacitor life-span, has good economy and adaptability.
Description
Technical field
The present invention relates to electrode material preparation field, more particularly to a kind of preparation method of activated carbon for super capacitors.
Background technology
The ultracapacitor to grow up in recent years, high-specific-power and cyclicity both with conventional physical electric capacity, have again
There is the high-energy-density characteristic of electrochmical power source, so, it can meet the use condition for requiring high-specific-power, and and can meets to require high
Than the use condition of energy.By there is ultracapacitor excellent pulse charge-discharge performance and conventional physical electric capacity not to have
Some Large Copacity energy-storage properties, the extensive concern of people is caused in the application of high energy pulse laser.Meanwhile because it is deposited
Energy storage capacity is big, light weight, can infinitely discharge and recharge and be used as computer system and without the standby electricity of communication apparatus of rationing the power supply by people
Source.With the rise of environmental-protecting type electric automotive research, ultracapacitor can independently or and secondary cell（Such as lead-acid battery or lithium
Ion battery）The power-supply system as electric automobile is combined, be widely used prospect.
In the various electrode materials of ultracapacitor, cheap absorbent charcoal material is most widely used and technology
Most ripe one kind.Absorbent charcoal material has excellent heat conductivility and electric conductivity, and its density is low, resist chemical performance
Good, thermal coefficient of expansion is small, and modulus of elasticity is not high.The variforms such as powder, bulk, fiber, cloth can be made by distinct methods, together
When also possess a variety of allotropes（Such as graphite, diamond, fullerene）, also can have difference because of the difference of degree of graphitization
Space structure, therefore be widely used in electrochemical field and make electrode material.
Through retrieval, one kind is disclosed in the prior art using petroleum coke as raw material, by grinding, using potassium hydroxide as activator
Prepare activated carbon for super capacitors；One kind has been also disclosed using the hard fruit shells such as apricot shell, peach shell or corncob as raw material, with certain
Amount phosphoric acid is activator, and potassium dihydrogen phosphate or sodium dihydrogen phosphate are that expanding agent prepares the activated carbon that specific capacitance reaches 200F/g；Also
One kind is disclosed with starch（Oxidative crosslinked starch, corn cationic starch, graft copolymerization starch, soluble starch or para arrowroot
Powder）For raw material, potassium hydroxide is the method that activator produces activated carbon for super capacitors.
But the activated carbon specific surface area prepared of the above method and capacitance are all relatively low, carbon material distribution of pores is uneven
It is even, the service life of ultracapacitor can be influenceed, need to further improve its performance.
It is in the industry so developing a kind of method for preparation of active carbon that can improve activated carbon specific surface area and capacitance
Personage's urgent problem.
The content of the invention
In view of this, the present invention provides a kind of preparation method of activated carbon for super capacitors.The preparation method can be made
The standby carbon material that abundant, specific surface area is high, capacitance characteristic is excellent that portals, significantly improves capacity of super capacitor and high magnification fills
Discharge performance.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of preparation method of activated carbon for super capacitors, comprises the following steps：
Crush the biological material being pre-configured with；
By the biological material after crushing through alkali process, then by being filtrated to get presoma, to get rid of through at alkali
The impurity in biological material after reason；
Presoma leaching is put ultrasonic vibration and stirring are carried out in potassium hydroxide solution, then by being filtrated to get modification
Presoma；
The modified presoma is heated, the modified presoma is carried out pre-activate；
The hydroxide of alkali, and heat-activated are added in the modified presoma.
Preferably, the biological material includes starch, lignin, corncob, rice husk, the wheat head, trees, coconut husk, fruit
Shell, leaf or stalk.
Further, in one embodiment, the concentration for soaking the potassium hydroxide solution for putting the presoma is
0.01-5 mol/L。
Further, in one embodiment, the particle mean size of the biological material after crushed is 0.1-0.5
cm。
Further, in one embodiment, it is 20- through frequency when the presoma leaching is put in potassium hydroxide solution
50 KHz ultrasonic vibration.
Further, in one embodiment, it is 100- through speed when the presoma leaching is put in potassium hydroxide solution
1800 r/min stirring.
Further, in one embodiment, presoma leaching put carried out in potassium hydroxide solution ultrasonic vibration and
The time of stirring is 0.1-72 h.
Further, in one embodiment, heating-up temperature during the modified presoma progress pre-activate is 100-300
DEG C or 700-900 DEG C.
Further, in one embodiment, heat time during the modified presoma progress pre-activate is 0.1-10
h。
Beneficial effect：The preparation method technique is simple, and environmental benefit is good, and the pre-activate time is short, reduces energy consumption；One side energy
It is enough to recycle the biomass such as stalk, ultracapacitor carbon material on the other hand can be prepared, to solve carbon materials
The problem of expecting distribution of pores inequality, improves the structural integrity of carbon material；The carbon material hole prepared is enriched, specific surface area
Height, capacitance characteristic are excellent, significantly improve capacity of super capacitor and high-rate charge-discharge capability, cyclicity is good, extends super
Level capacitor life-span, has good economy and adaptability.
Embodiment
The invention discloses a kind of preparation method of activated carbon for super capacitors, those skilled in the art can use for reference this
Literary content, it is suitably modified technological parameter realization.In particular, all similar replacements and change are to art technology
It is it will be apparent that they are considered as being included in the present invention for personnel.The method of the present invention and application are by preferable
Embodiment is described, related personnel substantially can not depart from present invention, in spirit and scope to side as described herein
Method and application are modified or suitably changed with combining, to realize and using the technology of the present invention.
This application provides a kind of preparation method of activated carbon for super capacitors, comprise the following steps：Crushing is matched somebody with somebody in advance
The biological material put；By the biological material after crushing through alkali process, then by being filtrated to get presoma, to get rid of
The impurity in biological material after alkali process；By the presoma leaching put in potassium hydroxide solution carry out ultrasonic vibration and
Stirring, then by being filtrated to get modified presoma；The modified presoma is heated, carries out the modified presoma pre-
Activation；The hydroxide of alkali, and heat-activated are added in the modified presoma.Preferably, the biological material includes
There are starch, lignin, corncob, rice husk, the wheat head, trees, coconut husk, shell, leaf or stalk.
Further, in one embodiment, the concentration for soaking the potassium hydroxide solution for putting the presoma is
0.01-5 mol/L。
Further, in one embodiment, the particle mean size of the biological material after crushed is 0.1-0.5
cm。
Further, in one embodiment, it is 20- through frequency when the presoma leaching is put in potassium hydroxide solution
50 KHz ultrasonic vibration.
Further, in one embodiment, it is 100- through speed when the presoma leaching is put in potassium hydroxide solution
1800 r/min stirring.
Further, in one embodiment, presoma leaching put carried out in potassium hydroxide solution ultrasonic vibration and
The time of stirring is 0.1-72 h.
Further, in one embodiment, heating-up temperature during the modified presoma progress pre-activate is 100-300
DEG C or 700-900 DEG C.
Further, in one embodiment, heat time during the modified presoma progress pre-activate is 0.1-10
h。
Compared with the activated carbon of ultracapacitor in the prior art, preparation method set forth herein prepares
Activated carbon have the following advantages that：
（1）Carbon material is prepared using biological material, biomass can be recycled, technique is simple, applicability
Extensively, good in economic efficiency, environmental benefit is good.
（2）In the pre-activate stage, presoma leaching is put in potassium hydroxide solution, passes through ultrasonic vibration and the modification of stirring
Method, direct presoma and the method for potassium hydroxide mechanical mixture are had the following advantages that compared to traditional：
Activated carbon pre-activate pore size distribution is uniform, and the activated carbon specific surface area after activation is high；
It can largely save the pre-activate time, reduce energy consumption；
The activated carbon uniformity prepared is good, for, the good cycle higher than energy that make ultracapacitor.
With reference to embodiment, technical scheme is expanded on further：
Embodiment 1
10g maize straws are weighed, is put into pulverizer and crushes, average grain diameter 1mm.Maize straw powder after crushing is put
In being in 0.1mol/L potassium hydroxide solutions containing 300ml concentration, 20min is stirred.Filtration washing obtains pure biomass.Will
Pure biomass is placed in the beaker for the potassium hydroxide solution that 500ml concentration is 1mol/L, and ultrasonic wave disperses 25 min, supersonic frequency
Rate 50KHz, stir speed (S.S.) are 400 r/min, and mixing time is 25 min, and filtration washing obtains alkali modification biomass.By 5g alkali
Modified activated carbon is placed in tube furnace, is set heating parameters, the temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, is incubated
30min, cooling obtain pre-activate activated carbon.100 are pressed with pre-activate activated carbon and potassium hydroxide crystal:7 mass ratio mixing, puts
In Muffle furnace, 800 DEG C are warming up to, soaking time 2h.Obtain activated carbon.
Electro-chemical test discovery is carried out to prepared carbon material, prepares specific surface area 2700m2/g, specific capacity 272g/
F activated carbon for super capacitors.
Embodiment 2
10g coconut husks are weighed, is put into pulverizer and crushes, average grain diameter 1mm.Maize straw powder after crushing is placed in and contained
It is in 0.1mol/L potassium hydroxide solutions to have 300 ml concentration, stirs 20min.Filtration washing obtains pure biomass.Will be pure
Biomass is placed in the beaker that 500ml concentration is 1mol/L potassium hydroxide solutions, and ultrasonic wave disperses 25min, supersonic frequency 50
KHz, the r/min of stir speed (S.S.) 400, the min of mixing time 25, filtration washing obtain alkali modification biomass.By 5g alkali modifications activity
Charcoal is placed in tube furnace, is set heating parameters, the temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, is incubated 30 min, cooling
Obtain pre-activate activated carbon.100 are pressed with pre-activate activated carbon and potassium hydroxide crystal:7 mass ratio mixing, is placed on Muffle furnace,
800 DEG C are warming up to, soaking time 2h.Obtain activated carbon.
Electro-chemical test discovery is carried out to prepared carbon material, prepares specific surface area 2720m2/g, specific capacity 282g/
F activated carbon for super capacitors.
Embodiment 3
10g lignin is weighed, is put into pulverizer and crushes, average grain diameter 1mm.Maize straw powder after crushing is placed in
It is mixing time 20min in 0.1mol/L potassium hydroxide solutions containing 300ml concentration.Filtration washing obtains pure biomass.Will
Pure biomass is placed in the beaker that 500 ml concentration are 1 mol/L potassium hydroxide solutions, ultrasonic dispersing time 25min, is surpassed
Acoustic frequency 50KHz, stir speed (S.S.) 400 r/min, mixing time 25min, filtration washing obtain alkali modification biomass.5g alkali is changed
Property activated carbon be placed in tube furnace, set heating parameters, the temperature rise period 1,3 DEG C/min of heating rate, to 150 DEG C, insulation 30
Min, cooling obtain pre-activate activated carbon.100 are pressed with pre-activate activated carbon and potassium hydroxide crystal:7 mass ratio mixing, is placed on
Muffle furnace, 800 DEG C are warming up to, soaking time 2h.Obtain activated carbon.
Electro-chemical test discovery is carried out to prepared carbon material, prepares specific surface area 2710m2/g, specific capacity 275g/
F activated carbon for super capacitors.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of activated carbon for super capacitors, it is characterised in that comprise the following steps：
Crush the biological material being pre-configured with；
By the biological material after crushing through alkali process, then by being filtrated to get presoma, to get rid of after alkali process
Biological material in impurity；
Presoma leaching is put ultrasonic vibration and stirring are carried out in potassium hydroxide solution, then by being filtrated to get modified forerunner
Body；
The modified presoma is heated, the modified presoma is carried out pre-activate；
The hydroxide of alkali, and heat-activated are added in the modified presoma.
2. the preparation method of activated carbon for super capacitors according to claim 1, it is characterised in that the biological material
Material includes starch, lignin, corncob, rice husk, the wheat head, trees, coconut husk, shell, leaf or stalk.
3. the preparation method of activated carbon for super capacitors according to claim 2, it is characterised in that put for leaching described
The concentration of the potassium hydroxide solution of presoma is 0.01-5 mol/L.
4. the preparation method of activated carbon for super capacitors according to claim 3, it is characterised in that institute after crushed
The particle mean size for stating biological material is 0.1-0.5 cm.
5. the preparation method of activated carbon for super capacitors according to claim 4, it is characterised in that the presoma leaching
When putting in potassium hydroxide solution, through the ultrasonic vibration that frequency is 20-50 KHz.
6. the preparation method of activated carbon for super capacitors according to claim 4, it is characterised in that the presoma leaching
When putting in potassium hydroxide solution, through the stirring that speed is 100-1800 r/min.
7. the preparation method of the activated carbon for super capacitors according to claim 5 or 6, it is characterised in that the forerunner
It is 0.1-72 h that body leaching, which is put and carries out ultrasonic vibration in potassium hydroxide solution with the time stirred,.
8. the preparation method of activated carbon for super capacitors according to claim 7, it is characterised in that the modified forerunner
Heating-up temperature when body carries out pre-activate is 100-300 DEG C or 700-900 DEG C.
9. the preparation method of activated carbon for super capacitors according to claim 8, it is characterised in that the modified forerunner
Heat time during body progress pre-activate is 0.1-10 h.
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| 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 |
| CN106629652B (en) * | 2016-12-29 | 2018-07-27 | 华南农业大学 | The biomass-based Carbon Materials of high-specific surface area and its exempt from process for preparing activated and application |
| 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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| CN101525132A (en) * | 2009-04-15 | 2009-09-09 | 广西师范大学 | Active carbon for super capacitor and a preparation method thereof |
| CN103539119B (en) * | 2013-10-30 | 2015-05-06 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for electrochemical energy storage device |
| CN105469999B (en) * | 2015-11-20 | 2017-11-17 | 浙江农林大学 | Bamboo powder is the method that raw material prepares Carbon-based supercapacitor electrode material |
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