CN109704332A - A kind of porous active carbon and its preparation method and application by the preparation of single carbon source one-step method - Google Patents
A kind of porous active carbon and its preparation method and application by the preparation of single carbon source one-step method Download PDFInfo
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- CN109704332A CN109704332A CN201910176568.1A CN201910176568A CN109704332A CN 109704332 A CN109704332 A CN 109704332A CN 201910176568 A CN201910176568 A CN 201910176568A CN 109704332 A CN109704332 A CN 109704332A
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- 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 belongs to super capacitor material technical field more particularly to a kind of porous active carbons and its preparation method and application by the preparation of single carbon source one-step method.The described method includes: by fulvic acid or potassium fulvate at 600-750 DEG C, be carbonized 1-6 hour, the product that carbonization is obtained is through washing, cooled to room temperature, carbonizing production be put into drying box after washing drying to get.Porous active carbon material preparation technology provided by the invention, process flow is simple, and carbon yield is high, and can largely prepare high performance carbon material without be further activated.Meanwhile electrode material of the porous active carbon prepared by the present invention as supercapacitor, show excellent chemical property.
Description
Technical field
The invention belongs to super capacitor material technical field more particularly to it is a kind of for supercapacitor by single carbon
The porous active carbon and preparation method thereof of source one-step method preparation.
Background technique
It is only intended to increase understanding of the overall background of the invention for information disclosed in background of invention, without
It is existing well known to persons skilled in the art so to be considered as recognizing or imply that information composition has become in any form
Technology.
No matter porous material is still industrially all widely used in daily life.Especially contain micropore or mesoporous
Porous carbon materials, be more widely applied, such as adsorbent, the electrode material of catalyst carrier, supercapacitor.
The customary preparation methods of activated carbon include physically activated and chemical activation.Physically activated includes two steps: raw material
It carbonizes and is activated using carbon dioxide or steam.Raw material carbonization is the continuous pyrolytic process of complexity, and physically activated
It then needs and oxidant carries out at 700-1100 DEG C.In chemical activating process, carbonization and activation simultaneously carry out, presoma and
KOH、NaOH、H3PO4And ZnCl2Equal activators are mixed in a certain proportion, and prepare porous carbon materials.Chemical activation, which can be prepared, to be had
The activated carbon of high surface area, but preparation process is cumbersome, higher cost.
Carbon material is the electrode material of symmetrical supercapacitor and the common negative electrode material of Asymmetric Supercapacitor,
Its performance is to supercapacitor using particularly important.It is main using chemistry currently used for the porous carbon materials of supercapacitor
Prepared by activation or steam activation processing, need to control activation condition.With moral great waves in the " preparation of the spherical porous carbon of humic acidic group
And its research of chemical property " in disclose with weathering coal measures fulvic acid (LFA) after purification be presoma, system research
Influence of the appearance structure and particle diameter distribution of porous carbon material to chemical property.Charcoal is prepared for using simple solvent evaporated method
Then microballoon is further prepared for spherical activated charcoal by alkali activation, by changing alkali charcoal than regulating and controlling its pore distribution, compare
The difference of spherical activated charcoal and powdered active carbon on electrochemical behavior.As a result, it has been found that spherical activated charcoal is in electric conductivity and hole
It is superior to powdered active carbon in terms of road structure distribution, and shows excellent electrochemical performance.
However, it is considered herein that the above method there are the problem of one of be: preparation process is complicated, the period is long, energy consumption is big, at
This height, low yield are easily introduced other impurity in activation process, and the porous carbon materials capacity and energy density that prepare are lower；
And Fulvic Acid From Weathered Coal content is low, causes to optimize purifying technique complexity and low efficiency.
Summary of the invention
In view of the above problems, the preparation cost of carbon material how is reduced, high-performance is simply and efficiently largely prepared
Porous carbon materials be one of current supercapacitor industry urgent problem.Therefore, the present invention is intended to provide it is a kind of by
The porous active carbon and its preparation method and application of single carbon source one-step method preparation.Porous active carbon material system provided by the invention
Standby technology, process flow is simple, and carbon yield is high, and can largely prepare high-performance carbon materials without be further activated
Material.Meanwhile electrode material of the porous active carbon prepared by the present invention as supercapacitor, show excellent electrochemistry
Energy.
An object of the present disclosure is to provide a kind of method for preparing porous active carbon by single carbon source one-step method.
Second purpose of the invention, is to provide the porous active carbon of above method preparation.
Third purpose of the present invention, is to provide the application of above-mentioned porous active carbon.
For achieving the above object, the invention discloses following technical proposals:
Firstly, the present invention discloses a kind of method for preparing porous active carbon by single carbon source one-step method, include the following steps:
Fulvic acid is carbonized, will the obtained product of carbonization washed to get.
Secondly, the present invention discloses another method for preparing porous active carbon by single carbon source one-step method, including walk as follows
It is rapid: potassium fulvate is carbonized, will the obtained product of carbonization washed to get.
Optionally, the temperature of the charing is 600-750 DEG C, and carbonization time is 1-6 hours.
Fulvic acid and potassium fulvate are broad-spectrum plant growth regulators, not only cheap, but also no pollution to the environment.Its
Middle fulvic acid is extracted from low-grade coal, and composed structure is relatively simple, mainly aromatic hydroxy-carboxylic substance, and yellow rotten
Sour potassium is the condensation polymer of multivalence phenolic aromatic compound and nitrogen compound.Have since fulvic acid and potassium fulvate belong to aromatic series
Machine object and containing nitrogen, steady chemical structure is high, therefore, after fulvic acid and potassium fulvate cracking, nitrogenous carbon material can be formed,
And carbon yield with higher, it is to prepare the suitable carbon source of high conductivity carbon material, and the carbon material prepared can have and answer extensively
With.
Optionally, in the method for preparing porous active carbon further include the steps that the product after washing is dried.
Optionally, the temperature of the drying is 90-115 DEG C, and drying time is 2-5 hours.
Optionally, the washing can also be acid washed and wash replacement, i.e., wash again after first pickling；The acid includes dilute salt
Acid, dilute sulfuric acid or dust technology etc..
Again, the present invention discloses the porous active carbon and preparation method thereof by the preparation of single carbon source one-step method and is adsorbing
Application in the fields such as agent, catalyst carrier, supercapacitor.
Finally, the present invention discloses a kind of capacitor, the electrode material of the capacitor is the single carbon source one-step method system
Standby porous active carbon.
Compared with prior art, the present invention achieve it is following the utility model has the advantages that
(1) carbon source fulvic acid and potassium fulvate that the present invention uses, cheap, stable structure, no pollution to the environment.
(2) present invention by single carbon source fulvic acid or potassium fulvate can one-step method prepare porous active carbon, the by-product Yishui River
It washes away and removes, not only energy saving and process is simple.
(3) porous active carbon technology of preparing proposed by the present invention, carbonization temperature is low, and the time is short, and carbon yield is high, is suitable for a large amount of
Production.
(4) porous active carbon material prepared by the present invention, purity and structural stability are high, are used for electrode of super capacitor material
Excellent chemical property is shown when material.
Detailed description of the invention
The Figure of description for constituting a part of the invention is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Fig. 1 is the x-ray diffraction pattern of porous carbon negative pole material made from the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope shape appearance figure of porous carbon negative pole material made from the embodiment of the present invention 1.
Fig. 3 be porous carbon negative pole material made from the embodiment of the present invention 1 N2 adsorption/desorption isotherm and corresponding aperture
Distribution map.
Fig. 4 is porous carbon negative pole material and commercial activated carbon made from the embodiment of the present invention 1 in 10mvs-1Under sweep speed
Cyclic voltammetry curve comparison diagram.
Fig. 5 is porous carbon negative pole material and commercial activated carbon made from the embodiment of the present invention 1 in 1Ag-1Under current density
Constant current charge-discharge curve comparison figure.
Fig. 6 is porous carbon negative pole material made from the embodiment of the present invention 1 in 8Ag-1Long circulating stability under current density
Figure.
Fig. 7 is porous carbon negative pole material made from the embodiment of the present invention 5 in 1Ag-1Constant current charge-discharge under current density
Curve graph.
Fig. 8 is porous carbon negative pole material made from the embodiment of the present invention 6 in 1Ag-1Constant current charge-discharge under current density
Curve graph.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As described in background, the existing technology for preparing active carbon not only preparation process is complicated, the period is long, energy consumption is big,
At high cost, low yield is easily introduced other impurity in activation process, and the porous carbon materials capacity for preparing and energy density compared with
It is low.Therefore, the preparation cost of carbon material how is reduced, simply and efficiently largely preparing porous carbon materials is current supercapacitor
One of industry urgent problem.Therefore, the present invention propose it is a kind of by single carbon source one-step method preparation porous active carbon and
Preparation method and application；The present invention is further illustrated now in conjunction with the drawings and specific embodiments.
Embodiment 1
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid, is heated to 700 DEG C in tube furnace under nitrogen atmosphere, keeps the temperature 3 hours.Heating furnace is closed, cooled to room temperature obtains
To the grey black powder 12.6g of bulk multi-hole.After the washing of grey black powder, it is put into drying box and is dried 3 hours at 110 DEG C.
Performance test: relevant characterization has been carried out to porous active carbon material manufactured in the present embodiment.Spread out by the X-ray of Fig. 1
Penetrating result can see, and other impurities are free of in the carbon material being prepared；It can see, produce by the transmission electron microscope tissue of Fig. 2
Object has fluffy porous structure, reaches 518.3m by the specific surface area that the adsorption-desorption curve of Fig. 3 obtains product2g-1, average hole
Diameter 1.43nm.
Porous carbon 0.2g made from the present embodiment is weighed, with 9%PVDF and carbon black with the ratio of 8:1:1 in 1 methyl, 2 pyrrole
It mixes in pyrrolidone solution, is applied in nickel sheet after mixing evenly, be put into vacuum oven and obtained after 12 hours after 120 DEG C of drying
To electrode material, it is expressed as FA.
Constant current charge-discharge and cyclic voltammetry carry out in the KOH solution of 1M at room temperature.Using three-electrode system,
Using platinized platinum as to electrode, saturated calomel electrode is as reference electrode, and FA is as working electrode.
Using the electrode for the porous active carbon preparation that the present embodiment obtains, in 10mv s-1Circulation volt is carried out under sweep speed
Peace test, and compared with commercial activated carbon, as shown in Figure 4.The porous active carbon that the present embodiment obtains is shown typically
Fake capacitance feature, being computed its capacity is 275F g-1.It is calculated by the constant current charge-discharge curve of Fig. 5, in 1A g-1Current density
Under, the porous active carbon specific capacity that the present embodiment obtains is 139F g-1, the specific capacity than commercial activated carbon is higher by 90%.Fig. 6 is
The porous active carbon that the present embodiment obtains, in 8Ag-1The curve that constant current charge-discharge is carried out under current density, after recycling 10000 times
Capacity retention ratio is 93.4%, shows excellent cyclical stability.
Compared to " preparation of the spherical porous carbon of humic acidic group and its research of chemical property " referred in background technique
Report prepares spherical activated charcoal by humic acid, and not only method is simple by the present invention, but also the porous carbon pore-size distribution prepared is more
Uniformly.Active carbon prepared by the present invention is using the KOH of 1M as electrolyte, in 1A g-1Capacity under current density is 139F g-1, and
The spherical activated charcoal of report is using the KOH of 6M as electrolyte, in 0.05A g-1Specific capacity 320F g under current density-1, in 0.1A g-1Specific capacity 193F g under current density-1.As can be seen that active carbon prepared by the present invention obviously shows superior electrochemistry
Performance and higher cost performance.
Embodiment 2
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid potassium, is heated to 600 DEG C under nitrogen atmosphere in tube furnace, keeps the temperature 3 hours.Closing heating furnace, cooled to room temperature,
Obtain the grey black powder 12.1g of bulk multi-hole.After the grinding washing of grey black powder, it is put into drying box and dries 4 at 110 DEG C
Hour.
Embodiment 3
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid potassium, is heated to 650 DEG C under nitrogen atmosphere in tube furnace, keeps the temperature 2 hours.Closing heating furnace, cooled to room temperature,
Obtain the grey black powder 12.5g of bulk multi-hole.After the washing of grey black powder, it is put into drying box small in 110 DEG C of drying 3.0
When.
Embodiment 4
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid potassium, is heated to 750 DEG C under nitrogen atmosphere in tube furnace, keeps the temperature 4 hours.Closing heating furnace, cooled to room temperature,
Obtain the grey black powder 12.3g of bulk multi-hole.By grey black powder after the cleaning of 200mL water, it is put into drying box at 110 DEG C
Drying 3.5 hours.
Embodiment 5
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid, is heated to 280 DEG C in tube furnace under air atmosphere, keeps the temperature 1 hour.750 DEG C are warming up in nitrogen atmosphere, heat preservation
5 hours.Heating furnace is closed, cooled to room temperature obtains the grey black powder 12.3g of bulk multi-hole.By grey black powder water
After washing, it is put into drying box and is dried 5 hours at 90 DEG C.The porous active carbon constant current charge-discharge curve that the present embodiment obtains is as schemed
Shown in 7, in 1A g-1Under current density, specific capacity is 117F g-1。
Embodiment 6
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid, is heated to 280 DEG C in tube furnace under nitrogen atmosphere, keeps the temperature 1 hour, 650 DEG C is warming up in nitrogen atmosphere, heat preservation
6 hours.Heating furnace is closed, cooled to room temperature obtains the grey black powder 12.3g of bulk multi-hole.By grey black powder water
After washing, it is put into drying box and is dried 2 hours at 115 DEG C.The porous active carbon constant current charge-discharge curve that the present embodiment obtains is such as
Shown in Fig. 8, in 1A g-1Under current density, specific capacity is 132F g-1。
Embodiment 7
A method of porous active carbon is prepared by single carbon source one-step method, includes the following steps: to weigh 30g Huang in the balance
Rotten acid, is heated to 700 DEG C in tube furnace under air atmosphere, keeps the temperature 1 hour.Heating furnace is closed, cooled to room temperature obtains
To the grey black powder 12.1g of bulk multi-hole.After the washing of grey black powder, it is put into drying box and is dried 3 hours at 110 DEG C.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for preparing porous active carbon by single carbon source one-step method, which comprises the steps of: will be yellow rotten
Acid is carbonized, will the obtained product of carbonization washed to get.
2. the method as described in claim 1, which is characterized in that the temperature of the charing is 600-750 DEG C, carbonization time 1-
6 hours.
3. a kind of method for preparing porous active carbon by single carbon source one-step method, which comprises the steps of: will be yellow rotten
Sour potassium is carbonized, will the obtained product of carbonization washed to get.
4. the method as described in claim 1, which is characterized in that the temperature of the charing is 600-750 DEG C, carbonization time 1-
6 hours.
5. method according to any of claims 1-4, which is characterized in that further include that the product after washing is dried
Step.
6. method as claimed in claim 5, which is characterized in that the temperature of the drying is 90-115 DEG C, drying time 2-5
Hour.
7. method according to any of claims 1-4, which is characterized in that the washing can also be acid washed and wash generation
It replaces, i.e., is washed again after first pickling.
8. the method for claim 7, which is characterized in that the acid includes dilute hydrochloric acid, dilute sulfuric acid or dust technology.
9. porous active carbon of the method according to claim 1 preparation and preparation method thereof is in adsorbent, catalysis
Application in agent carrier, supercapacitor field.
10. a kind of capacitor, which is characterized in that the electrode material of the capacitor is the described in any item sides of claim 1-8
The porous active carbon of method preparation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110339817A (en) * | 2019-07-29 | 2019-10-18 | 安徽工业大学 | A kind of preparation method of N doping fulvic acid base porous charcoal adsorbent material |
| CN113277510A (en) * | 2021-05-31 | 2021-08-20 | 中国科学技术大学 | Synthetic method for preparing porous carbon material by using small molecules |
| CN115010128A (en) * | 2022-05-26 | 2022-09-06 | 江西省科学院应用化学研究所 | Method for preparing carbon material by taking potassium cinnamate as raw material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103373728A (en) * | 2012-04-16 | 2013-10-30 | 河南理工大学 | Method for preparing active carbon for super-capacitor from potassium humate in one-step carbonization way |
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2019
- 2019-03-08 CN CN201910176568.1A patent/CN109704332A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103373728A (en) * | 2012-04-16 | 2013-10-30 | 河南理工大学 | Method for preparing active carbon for super-capacitor from potassium humate in one-step carbonization way |
Non-Patent Citations (1)
| Title |
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| 杨燕飞: "多孔炭的一步制备及在无机盐电解液中电化学性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110339817A (en) * | 2019-07-29 | 2019-10-18 | 安徽工业大学 | A kind of preparation method of N doping fulvic acid base porous charcoal adsorbent material |
| CN113277510A (en) * | 2021-05-31 | 2021-08-20 | 中国科学技术大学 | Synthetic method for preparing porous carbon material by using small molecules |
| CN115010128A (en) * | 2022-05-26 | 2022-09-06 | 江西省科学院应用化学研究所 | Method for preparing carbon material by taking potassium cinnamate as raw material |
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Application publication date: 20190503 |