CN107403698B - A kind of application preparing the method for activated carbon and its active carbon of preparation using biomass - Google Patents
A kind of application preparing the method for activated carbon and its active carbon of preparation using biomass Download PDFInfo
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- CN107403698B CN107403698B CN201710810743.9A CN201710810743A CN107403698B CN 107403698 B CN107403698 B CN 107403698B CN 201710810743 A CN201710810743 A CN 201710810743A CN 107403698 B CN107403698 B CN 107403698B
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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
The invention discloses a kind of applications that the method for activated carbon and its active carbon of preparation are prepared using biomass.This method is by biomass drying and crushing; it is put into certain density acid solution and impregnates 1-2h, be subsequently placed in open hydrothermal system, be placed in Muffle furnace and be heated to 180-250 DEG C; heat preservation 5-8h reacts to obtain carbon matrix precursor; washing is placed in high-temperature activation under protective atmosphere with a certain proportion of alkali activator powder mixed grinding after suction filtration is dry to neutrality after carbon matrix precursor natural cooling; after cooled to room temperature; washing to neutrality, it is dry to get.Gained active carbon material epigranular, large specific surface area, supercapacitor obtained have height ratio capacity and good cyclical stability.This method utilizes agriculture waste biomass raw material, prepares supercapacitor carbon electrode material by simple and quick method, turns waste into wealth, make full use of resource, reduce environmental pollution, good in economic efficiency, is beneficial to industrialized production.
Description
Technical field:
The present invention relates to the preparation technical fields of absorbent charcoal material, in particular to a kind of to prepare activity using biological material
The new method of carbon, and its application on electrode of super capacitor.
Background technique:
Global warming and the increasingly depleted of fossil fuel force people to greatly develop sustainable and renewable energy.Currently,
Increasingly short energy problem is solved, is still one of huge challenge of facing mankind.Finding cleaning, efficient and renewable energy
While, energy stores also can not be ignored.Such as be considered as the solar energy and wind energy of new energy most with prospects, all by
The influence of the factors such as time, place, weather, is unable to steady operation.Therefore, especially energy-storage system is needed to deposit energy
Chu Houzai is used.In recent years, supercapacitor played the part of more and more important role as energy storage device, in particular with letter
The rapid development of new technology in the fields such as breath technology, electronic product and vehicle used energy, people focus more on grinding for supercapacitor
Study carefully and develops.
Biomass, especially agriculture and forestry organic waste material and food residue object, cellulose, hemicellulose and wood containing very high degree
Quality, these ingredients can be obtained carbon-rich material by high-temperature process.China is large agricultural country, every to generate a large amount of agriculture every year
Woods waste, the current method for cleaning of these substances predominantly burn, and not only cause serious pollution to environment, or to resource
Significant wastage therefore how biomass castoff to be carried out harmless treatment and realizing recycling, is scientific research circle now, work
The key issues of the common concerns such as industry.However, due to still containing plurality of impurities such as metal etc. in biomass, it is straight on the market at present
Connecing has the shortcomings that ingredient is impure, performance is poor by the carbon electrode material of biomass preparation, to residual with agriculture and forestry organic waste material and food
Staying the biomass based on object to carry out, green high-purity carbonization recycles and exploitation is then applied to energy storage field, has very big
Economic value and Practical significance.
Summary of the invention:
The purpose of the present invention is to provide a kind of novel to be made under acidic environment effect using high microsteping content biomass
Application of the active carbon that the method and this method of standby activated carbon are prepared on the electrode material of production supercapacitor.
Method provided by the invention can not only make biomass dead meal resource be effectively used, and slow down eco-environmental pressure, simultaneously
Activated carbon obtained has preferable chemical property, may be used as the electrode material of supercapacitor, is conducive to push new energy
The development of source domain.
A method of activated carbon being prepared using biomass, is that raw material is opened under acid solution effect using biomass
The hydro-thermal reaction of formula prepares carbon matrix precursor, carbon matrix precursor and alkali activator powder mixed grinding, high-temperature activation to get.
As a further preference, the biomass after drying and crushing is mixed with certain density acid solution, after immersion, is set
In open hydrothermal reaction kettle, at 180-250 DEG C, heat preservation 5-8h reacts to obtain carbon matrix precursor.
As a further preference, the biomass dries 24-48h in convection oven at 80 DEG C.It is crushed to 30-50
Mesh.
As a further preference, the biomass after drying and crushing is pressed into solid and liquid weight volume with certain density acid solution
Than mixing for 1g:15-30ml, the certain density acid solution is the phosphoric acid or 60-80% that mass concentration is 70-85%
The concentrated sulfuric acid is placed in open hydrothermal reaction kettle after impregnating 1-2h, and at 180-250 DEG C, heat preservation 5-8h reacts to obtain carbon forerunner
Body.
As a further preference, the biomass after drying and crushing is mixed with certain density acid solution, impregnates postposition
It in the hydrothermal reaction kettle of open type, is placed in Muffle furnace and heats, insulation reaction obtains carbon matrix precursor.
As a further preference, open hydrothermal reaction kettle volume is 50-300ml, and liquid amount is that reaction kettle holds when reaction
Long-pending 60-70%.
As a further preference, open hydro-thermal reaction pot systems are high-temperature resistant polytetrafluoroethylmelt liner, and flange form can live
Dynamic steel bushing.
The method for preparing activated carbon using biomass, washing filters dry to neutrality after carbon matrix precursor natural cooling
With a certain proportion of alkali activator mixed grinding after dry, alkali activator is preferably KOH, NaOH, K2CO3、Na2CO3、NaHCO3
One or more of；Be placed in high-temperature activation under protective atmosphere, after cooled to room temperature, washing to neutrality, it is dry to get.
As a further preference, use washing up to neutral after carbon matrix precursor natural cooling, after filtering drying, carbon forerunner
The ratio of body and alkali activator is 1:1-5 mixed grinding, and 700 DEG C -1200 DEG C of tubular type being placed under nitrogen atmosphere protection is high
Keep the temperature 1-8h in warm Muffle furnace, after cooled to room temperature, washed respectively using deionized water, 1MHCl solution, then spend from
Sub- water washing to neutrality, after vacuum filtration in 80 DEG C of dry 12h to get.
The nitrogen atmosphere is the nitrogen that purity is 99% or more；The flow velocity that is passed through of the nitrogen atmosphere is 3-8ml/
min；The heating rate of tubular type high temperature Muffle furnace is 3-10 DEG C/min.
The method for preparing activated carbon using biomass, biomass have cellulose high-content agriculture and forestry organic waste material and
Food residue object, comprising: one or more of stalk, Chinese silvergrass, tendril, pericarp.
Active carbon material after weighing the above-mentioned grinding of 0.8g, is ground after mixing with acetylene black by weight 8:1,
Then the polytetrafluoroethyl-ne aqueous solution that a small amount of concentration is 10% is added, wherein activated carbon: acetylene black: polytetrafluoroethylene (PTFE)=8:1:1
(mass ratio) is added a small amount of alcohol as solvent, continues to grind after mixing, rolls piece, prepare carbon electrode material.By carbon electricity obtained
Pole piece is pressed on stainless steel collector, is electrolysis with the KOH aqueous solution of 6mol/L after being then dried in vacuo 12h at 110 DEG C
Liquid is assembled into supercapacitor, tests chemical property.
Using active carbon material epigranular obtained by the method for the present invention, specific surface area is about 875m2/ g, electrode group obtained
After dressing up supercapacitor, specific discharge capacity 405.34F/g has good cyclical stability, can be used for energy storage neck
Domain.This method utilizes trade waste carbon felt leftover pieces, prepares supercapacitor carbon electrode material by simple and quick method
Material, turns waste into wealth, makes full use of resource, reduce environmental pollution, good in economic efficiency, is beneficial to industrialized production.
Detailed description of the invention:
Fig. 1: using the scanning electron microscope (SEM) photograph of supercapacitor activated carbon prepared by the embodiment of the present invention 2；
Fig. 2: it is assembled into after supercapacitor using activated carbon prepared by the embodiment of the present invention 2 in the case where 100mV/s sweeps speed
Cyclic voltammogram；
Fig. 3: it is assembled into after supercapacitor under 1A/g current density using activated carbon prepared by the embodiment of the present invention 2
Charging and discharging curve figure；
Fig. 4: it is assembled into after supercapacitor using activated carbon prepared by the embodiment of the present invention 2 and is filled in 10A/g current density
Cyclical stability under discharging condition.
Specific embodiment:
Feature of the invention is described below, illustrated embodiment for explaining only the invention, is not intended to limit this
The range of invention.It should be understood by those skilled in the art that the equivalent replacement that the technical characteristic of the content of present invention is done, or it is corresponding
Improvement, still fall within protection scope of the present invention.
Embodiment 1: it can be used for the preparation side of the active carbon material of electrode of super capacitor using the preparation of biomass dead meal
Method the following steps are included:
It is crushed after stalk is dried in convection oven to constant weight, it is pressed into solid and liquid weight volume ratio with 75% sulfuric acid solution
For 1g:30ml mixing, impregnates in the opening hydro-thermal reaction pot systems after 1h is placed on improvement, be placed in Muffle furnace and add in air
For heat to 220 DEG C, heat preservation 5h reacts to obtain carbon matrix precursor, using washing until neutral after natural cooling, filter it is dry after with KOH powder
End keeps the temperature 2h in 800 DEG C of tubular type high temperature Muffle furnace being placed under nitrogen atmosphere protection with 1:1 ratio mixed grinding, naturally cold
But it to after room temperature, is washed, is then washed with deionized to neutrality respectively using deionized water, 1MHCl solution, after vacuum filtration
In 80 DEG C of dry 12h, the activity that can be used as electrode material for super capacitor with good chemical property can be obtained after grinding
Carbon material.
Embodiment 2: it can be used for the preparation side of the active carbon material of electrode of super capacitor using the preparation of biomass dead meal
Method the following steps are included:
It is crushed after Chinese silvergrass is dried in convection oven to constant weight, it is pressed into solid and liquid weight volume ratio with 85% phosphoric acid solution
For 1g:20ml mixing, impregnates in the opening hydro-thermal reaction pot systems after 1h is placed on improvement, be placed in Muffle furnace and add in air
For heat to 200 DEG C, heat preservation 5h reacts to obtain carbon matrix precursor, using washing until neutral after natural cooling, filter it is dry after with KOH powder
End keeps the temperature 2h in 800 DEG C of tubular type high temperature Muffle furnace being placed under nitrogen atmosphere protection with 1:1 ratio mixed grinding, naturally cold
But it to after room temperature, is washed, is then washed with deionized to neutrality respectively using deionized water, 1MHCl solution, after vacuum filtration
In 80 DEG C of dry 12h, the activity that can be used as electrode material for super capacitor with good chemical property can be obtained after grinding
Carbon material.
Embodiment 3: it can be used for the preparation side of the active carbon material of electrode of super capacitor using the preparation of biomass dead meal
Method the following steps are included:
It is crushed after pericarp is dried in convection oven to constant weight, it is pressed into solid and liquid weight volume ratio with 75% sulfuric acid solution
For 1g:30ml mixing, impregnates in the opening hydro-thermal reaction pot systems after 1h is placed on improvement, be placed in Muffle furnace and add in air
For heat to 220 DEG C, heat preservation 8h reacts to obtain carbon matrix precursor, using washing until neutral after natural cooling, filter it is dry after with KOH powder
End keeps the temperature 2h in 700 DEG C of tubular type high temperature Muffle furnace being placed under nitrogen atmosphere protection with 1:1 ratio mixed grinding, naturally cold
But it to after room temperature, is washed, is then washed with deionized to neutrality respectively using deionized water, 1MHCl solution, after vacuum filtration
In 80 DEG C of dry 12h, the activity that can be used as electrode material for super capacitor with good chemical property can be obtained after grinding
Carbon material.
Comparative example:
It is crushed after taking pericarp to dry in convection oven to constant weight, it is pressed into solid and liquid weight volume ratio with 75% sulfuric acid solution
For 1g:30ml mixing, impregnates 1h and be placed in common closed hydro-thermal reaction system, be placed in Muffle furnace and be heated in air
220 DEG C, heat preservation 8h reacts to obtain carbon matrix precursor, using washing until neutral after natural cooling, filter it is dry after with KOH powder with
1:1 ratio mixed grinding, be placed in nitrogen atmosphere protection under 700 DEG C of tubular type high temperature Muffle furnace in keep the temperature 2h, naturally cool to
It after room temperature, is washed, is then washed with deionized to neutrality respectively using deionized water, 1MHCl solution, in 80 after vacuum filtration
Carbon material is obtained after DEG C dry 12h, adopts and prepares electrode slice in a like fashion, be fitted into capacitor device and test, electrochemistry
Performance can not show a candle to it is treated by the present method after active carbon product.
It uses the method for the present invention to prepare gained activated carbon with biomass dead meal, is packed into super capacitor after being prepared into electrode slice
It is tested in device device, wherein scanning electron microscope (SEM) photograph such as Fig. 1 institute of electrode of super capacitor activated carbon obtained in embodiment 2
Show, every chemical property such as Fig. 2, shown in 3,4, the experimental results of embodiment 1-3 and comparative example are as shown in table 1.From reality
It tests from the point of view of result, the active carbon material obtained of embodiment 2 has uniform particle size, 875m2The specific surface area of/g is made
Supercapacitor have 405.34F/g specific discharge capacity, have good cyclical stability.
Table 1
In conclusion use it is provided by the present invention with acid solution impregnate biomass dead meal after in open system solvent
The method of thermal response: on the one hand, it is process object with biomass dead meal, realizes the recycling of resource, effectively reduce ring
Border pollution, reduces production cost；On the other hand, preparation process is simple, simple flow, at low cost, obtained activation carbon product tool
There is good chemical property, can be used for energy storage field；Raw material sources are extensive, simple production process, are suitble to industrialization
It promotes and applies.
Claims (10)
1. a kind of method for preparing activated carbon using biomass, which is characterized in that acted on for raw material in acid solution using biomass
It is lower to carry out open hydro-thermal reaction and prepare carbon matrix precursor, carbon matrix precursor and alkali activator powder mixed grinding, high-temperature activation,
To obtain the final product.
2. the method according to claim 1 for preparing activated carbon using biomass, which is characterized in that after drying and crushing
Biomass is mixed with certain density acid solution, after immersion, is placed in open hydrothermal reaction kettle, at 180-250 DEG C, keeps the temperature 5-
8h reacts to obtain carbon matrix precursor.
3. the method according to claim 2 for preparing activated carbon using biomass, which is characterized in that after drying and crushing
Biomass is that 1g:15-30ml is mixed by solid and liquid weight volume ratio with certain density acid solution, and the certain density acid is molten
Liquid is that the phosphoric acid that mass concentration is 70-85% or the concentrated sulfuric acid of 60-80% are placed in open hydrothermal reaction kettle after impregnating 1-2h
In, at 180-250 DEG C, heat preservation 5-8h reacts to obtain carbon matrix precursor.
4. the method according to claim 2 for preparing activated carbon using biomass, which is characterized in that after drying and crushing
Biomass is mixed with certain density acid solution, and immersion is placed in the hydrothermal reaction kettle of open type, is placed in Muffle furnace and is heated,
Insulation reaction obtains carbon matrix precursor.
5. the method according to claim 1 for preparing activated carbon using biomass, which is characterized in that open hydrothermal reaction kettle
Volume is 50-300ml, and liquid amount is the 60-70% of reactor volume when reaction.
6. the method according to claim 1 for preparing activated carbon using biomass, which is characterized in that carbon matrix precursor is naturally cold
But wash afterwards to neutrality, filter it is dry after with a certain proportion of alkali activator powder mixed grinding, alkali activator KOH,
NaOH、K2CO3、Na2CO3、NaHCO3One or more of；It is placed in high-temperature activation under protective atmosphere, after cooled to room temperature,
Washing to neutrality, it is dry to get.
7. the method according to claim 6 for preparing activated carbon using biomass, which is characterized in that carbon matrix precursor is naturally cold
But afterwards using washing until neutral, after suction filtration is dry, the ratio of carbon matrix precursor and alkali activator is 1:1-5 mixed grinding, is set
1-8h is kept the temperature in 700 DEG C -1200 DEG C of the tubular type high temperature Muffle furnace under nitrogen atmosphere protection, after cooled to room temperature, is adopted
It is washed, is then washed with deionized to neutrality respectively with deionized water, 1MHCl solution, in 80 DEG C of dryings after vacuum filtration
12h to get.
8. the method according to claim 1 for preparing activated carbon using biomass, which is characterized in that biomass has fiber
The agriculture and forestry organic waste material and food residue object of plain high-content, comprising: one or more of stalk, Chinese silvergrass, tendril, pericarp.
9. the activated carbon of the described in any item method preparations of claim 1-8.
10. the application of active carbon as claimed in claim 9, which is characterized in that be used to prepare supercapacitor active carbon electrode
Material.
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| CN108328597B (en) * | 2018-01-08 | 2022-12-06 | 石河子大学 | Carbon material prepared from printing and dyeing wastewater |
| CN108840378A (en) * | 2018-06-29 | 2018-11-20 | 张家港江苏科技大学产业技术研究院 | Iron-absorbent charcoal composite material, method and application is prepared in situ in a kind of metallurgical dust |
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| CN112138699A (en) * | 2020-09-25 | 2020-12-29 | 拉萨波玛拉生物科技有限公司 | Preparation method of N-rich hydrothermal carbon material |
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| CN114906847A (en) * | 2022-05-16 | 2022-08-16 | 内蒙古科技大学 | Wet activation method for gasification slag carbon residue and application thereof |
| CN115387028A (en) * | 2022-08-22 | 2022-11-25 | 湖南理工学院 | Porous Si/C composite material packaged by conductive fiber network and preparation method and application thereof |
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