CN106098407A - A kind of method utilizing culture medium of edible fungus garbage to prepare ultracapacitor porous carbon electrode material - Google Patents
A kind of method utilizing culture medium of edible fungus garbage to prepare ultracapacitor porous carbon electrode material Download PDFInfo
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- CN106098407A CN106098407A CN201610651606.0A CN201610651606A CN106098407A CN 106098407 A CN106098407 A CN 106098407A CN 201610651606 A CN201610651606 A CN 201610651606A CN 106098407 A CN106098407 A CN 106098407A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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 method utilizing culture medium of edible fungus garbage to prepare ultracapacitor porous carbon electrode material, it includes the steps such as pre-treatment, carbonization, activation, pickling, the present invention utilizes the Organic substance in culture medium of edible fungus garbage to prepare super capacitor carbon electrode material as carbon source, achieve and turn waste into wealth, improve resource utilization, the specific surface area of material is high, uniform pore diameter, in the same size, demonstrate higher ratio electric capacity and good chemical property.
Description
Technical field
The present invention relates to the preparation method of super capacitor carbon electrode material, the invention still further relates to a kind of ultracapacitor work
Make electrode.
Background technology
Ultracapacitor as a kind of novel electrochemical energy storing device, have that storage energy is big, light weight, capable of circulation time
The advantageous feature such as number is long, non-maintaining.The combination property of ultracapacitor is closely related with electrode material, and at present, commercialization is super
Capacitor electrode material focuses primarily upon material with carbon element, and this material has the electrical conductance of excellence, higher theoretical surface is amassed, and chemistry is steady
The advantages such as qualitative good, aperture easily regulation and control.
Ultracapacitor industry belongs to energy intensive, and it produces or a non-renewable process.Therefore, electricity is improved
Pole material, it is achieved renewableization of production, has very important significance.Finding reproducible ultracapacitor carbon electrode material
During material, wide material sources, cheap biological material causes the broad interest of scientific research personnel, in recent years, multiple
Biological material has been used for preparing carbon electrode, but there is presently no and prepare ultracapacitor with culture medium of edible fungus garbage
The report of carbon electrode material.
Summary of the invention
It is an object of the invention to utilize culture medium of edible fungus garbage for raw material, prepare porous carbon electrode material and answered
For ultracapacitor working electrode.
The preparation method of the ultracapacitor porous carbon electrode material that the present invention provides is as follows:
1) pre-treatment: clean to neutral with water after culture medium of edible fungus garbage is first soaked 5～20h with dilute hydrochloric acid,
Again with acetone soak 5～20h, wash 3-4 time respectively with water and dehydrated alcohol the most successively, be finally put in oven for drying；
2) carbonization: will dry after culture medium of edible fungus garbage be placed in tube furnace, under argon atmosphere with 2～6 DEG C/
The ramp of min to 500～700 DEG C, and constant temperature carbonization 0.5～5h, take out carbonized product after temperature drops to room temperature；
3) activation: carbonized product and KOH mixed by the mass ratio of 1: 2～6 and is ground to uniform powder, being subsequently placed in
In tube furnace, with the ramp to 700～800 DEG C of 2～6 DEG C/min under argon atmosphere, and constant temperature activation 1～3h, treat temperature
Degree takes out activation products after dropping to room temperature；
4) pickling: activation products are first washed with dilute hydrochloric acid, is washed with water to neutrality, is finally placed on air dry oven
In be dried, i.e. obtain ultracapacitor porous carbon electrode material.
Preferably, step 2) in, described heating rate is 3 DEG C/min, and carburizing temperature is 700 DEG C, and carbonization time is 1h.
Preferably, step 3) in, described carbonized product is 1: 4 with the mass ratio of KOH.
Preferably, step 3) in, described heating rate is 3 DEG C/min, and activation temperature is 750 DEG C, and soak time is 3h.
The present invention further provides a kind of ultracapacitor working electrode, this electrode is by ultracapacitor porous carbon electrodes material
Material, conductive agent, binding agent form, and described ultracapacitor porous carbon electrode material is to prepare according to above-mentioned method.
Preferably, described conductive agent is Super P, binding agent is PTFE (politef), and described ultracapacitor is many
Hole carbon electrode material: conductive agent: the mass ratio of binding agent is 8: 1: 1.
The present invention compared with prior art has the advantage that
1) due in culture medium of edible fungus garbage rich in Organic substance, therefore can prepare electrode of super capacitor as carbon source
Material with carbon element, thus turn waste into wealth, improve resource utilization；
2) step is simple, and raw material sources is extensive, it is easy to accomplish industrialization, reproducible；
3) the electrode of super capacitor material with carbon element that prepared by the present invention has loose structure, and the specific surface area of material is up to
3439m2g-1, and uniform pore diameter, in the same size, demonstrate higher ratio electric capacity and good chemical property.
Accompanying drawing explanation
Fig. 1 is cyclic voltammetry curve figure (the 1M H of test under three-electrode system2SO4For electrolyte).
Fig. 2 is the cyclic voltammetry curve figure (6M KOH is electrolyte) of test under three-electrode system.
Detailed description of the invention
Embodiment 1
1. the preparation of ultracapacitor porous carbon electrode material
1) pre-treatment: culture medium of edible fungus garbage is first soaked 12h with the dilute hydrochloric acid that mass fraction is 10% and removes miscellaneous
Matter (mainly calcium carbonate impurity), is then washed with water to neutrality, then soaks 12h with acetone soln, the most successively by water and nothing
Water-ethanol washs 4 times respectively, is finally placed in 70 DEG C of oven drying 24h；
2) carbonization: take the culture medium of edible fungus garbage after drying and be placed in tube furnace, with 5 DEG C/min under argon atmosphere
Ramp to 500 DEG C, and constant temperature carbonization 1h, take out carbonized product after the temperature until tube furnace drops to room temperature afterwards；
3) activation: take carbonized product and mix by the mass ratio of 1: 4 with KOH, and be ground to uniform powder, then put
In tube furnace, with the ramp to 700 DEG C of 5 DEG C/min and 800 DEG C under argon atmosphere, respectively at 700 DEG C and 800 DEG C
Calcining 1h, 2h, 3h, i.e. can be taken off activation products after temperature drops to room temperature；
4) pickling: by activation products first with the dilute hydrochloric acid washing that mass fraction is 10%, remove alkalescence unnecessary in sample
Material (KOH), is washed with water to neutrality, is finally placed in 80 DEG C of air dry ovens and is dried, i.e. obtains ultracapacitor many
Hole carbon electrode material.
2. the preparation of ultracapacitor working electrode
Take the porous carbon electrode material of preparation, conductive agent (Super P), binding agent (PTFE), be in mass ratio 8: 1: 1 mix
Close, with mortar mix homogeneously and be modulated into pulpous state after adding appropriate ethanol, the homogenate made is dropped in stainless (steel) wire and foam
On nickel, (electrode slice prepared by stainless (steel) wire is for H2SO4Testing in electrolyte, electrode slice prepared by nickel foam is for KOH electrolyte
Middle test), it is then transferred to 80 DEG C of dry 12h in vacuum drying oven, finally takes out electrode slice, standby after weighing.
3. sample test
The working electrode prepared uses three-electrode system test, and with platinized platinum for electrode, Ag/AgCl is reference electrode, logical
Cross constant current charge-discharge to test than electric capacity (F/g) data.Wherein stainless (steel) wire electrode slice is used for H2SO4In electrolyte, nickel foam electricity
Pole piece is in KOH electrolyte.All of electro-chemical test is all in occasion China CHI660E (China, Shanghai) electrochemical workstation
Carry out.
Cyclic voltammetry curve (the 1M H of test under three-electrode system2SO4Electrolyte) illustrate: 1. cyclic voltammetry curve shows
Go out class rectangular shape, show typical electric double layer capacitance characteristic, even sweep greatly speed 500mV/s and still keep the song of similar rectangle
Line, illustrates that this material has good high rate performance.2. curve is all found that a pair obvious oxidoreduction peak, shows material
Charge and discharge process there occurs, faraday's redox reaction creates fake capacitance, thus improves and compare electric capacity.
Under three-electrode system, the cyclic voltammetry curve (6M KOH electrolyte) of test illustrates: cyclic voltammetry curve demonstrates class
Rectangular shape, shows typical electric double layer capacitance characteristic, when sweeping the curve still keeping similar rectangle when speed increases to 200mV/s
Figure, this result shows that this material not only shows good high rate performance in acid system, same in alkaline system
Also there is good high rate performance.
Table 1 embodiment 1 porous carbon materials is at 1M H2SO4Ratio electric capacity in electrolyte
Table 2 embodiment 1 porous carbon ratio electric capacity in 6M KOH electrolyte
As can be seen from the above data, super capacitor material prepared by the present invention has higher ratio electric capacity, Qi Zhong
The ratio electric capacity of the porous carbon materials of 700 DEG C of activation 3h is higher.
Embodiment 2
1. the preparation of ultracapacitor porous carbon electrode material
1) pre-treatment: by culture medium of edible fungus garbage first with mass fraction be 10% dilute hydrochloric acid soak 12h remove impurity,
Then it is washed with water to neutrality, then soaks 12h with acetone soln, wash 4 times respectively with water and dehydrated alcohol the most successively, finally
It is placed in 70 DEG C of oven drying 24h；
2) carbonization: take the culture medium of edible fungus garbage after drying and be placed in tube furnace, with 3 DEG C/min under argon atmosphere
Ramp to 700 DEG C and constant temperature carbonization 1h, after temperature drops to room temperature take out carbonized product；
3) activation: take carbonized product and mix by the mass ratio of 1: 4 with KOH, and be ground to uniform powder, then put
In tube furnace, with the ramp to 750 DEG C of 3 DEG C/min under argon atmosphere, and calcining at constant temperature 3h, treat that temperature drops to room temperature
Rear taking-up activation products；
4) pickling: by the dilute hydrochloric acid washing that activation products mass fraction is 10%, being then washed with water to pH value of solution is
Neutrality, is finally placed in 80 DEG C of air dry ovens and is dried, i.e. obtain porous carbon electrode material.
2. the preparation of ultracapacitor working electrode
Same as in Example 1.
3. sample test
Same as in Example 1, the results are shown in Table 3.
The ratio electric capacity of table 3 embodiment 2 porous carbon materials
Embodiment 3
1. the preparation of ultracapacitor porous carbon electrode material
1) pre-treatment: by culture medium of edible fungus garbage first with mass fraction be 5% dilute hydrochloric acid soak 20h remove impurity
(mainly calcium carbonate impurity), is then washed with water to neutrality, then soaks 5h with acetone soln, the most successively by water and anhydrous second
Alcohol washs 4 times respectively, is finally placed in 70 DEG C of oven drying 24h；
2) carbonization: take the culture medium of edible fungus garbage after drying and be placed in tube furnace, with 6 DEG C/min under argon atmosphere
Ramp to 700 DEG C, and constant temperature carbonization 0.5h, after temperature drops to room temperature, take out carbonized product；
3) activation: take carbonized product and KOH and mix by the mass ratio of 1: 2 and grind to form uniform powder, then put
In tube furnace, with the ramp to 700 DEG C of 2 DEG C/min under argon atmosphere, and calcining at constant temperature 3h, treat that temperature drops to room temperature
Rear taking-up；
4) pickling: by the dilute hydrochloric acid washing that activation products mass fraction is 10%, being then washed with water to pH value of solution is
Neutrality, is finally placed in 80 DEG C of air dry ovens and is dried, i.e. obtain porous carbon electrode material.
2. the preparation of ultracapacitor working electrode
Take prepared porous carbon electrode material, conductive agent (Super P), binding agent (PTFE), be to mix at 8: 2: 2 in mass ratio
Close, with mortar mix homogeneously and be modulated into pulpous state after adding appropriate ethanol, the homogenate made is dropped in stainless (steel) wire and foam
On nickel, (electrode slice prepared by stainless (steel) wire is for H2SO4Testing in electrolyte, electrode slice prepared by nickel foam is for KOH electrolyte
Middle test), it is then transferred to 80 DEG C of dry 12h in vacuum drying oven, finally takes out electrode slice, standby after weighing.
3. sample test
Same as in Example 1, the results are shown in Table 4.
The ratio electric capacity of table 4 embodiment 3 porous carbon materials
Embodiment 4
1. the preparation of ultracapacitor porous carbon electrode material
1) pre-treatment: by culture medium of edible fungus garbage first with mass fraction be 1% dilute hydrochloric acid soak 5h remove impurity, so
After be washed with water to neutrality, then soak 20h with acetone soln, wash respectively 4 times with water and dehydrated alcohol the most successively, the most rearmounted
In 70 DEG C of oven drying 24h；
2) carbonization: the culture medium of edible fungus garbage after drying is placed in tube furnace, with 2 DEG C/min under argon atmosphere
Ramp to 500 DEG C and constant temperature carbonization 5h, after temperature drops to room temperature take out；
3) activation: take carbonized product and KOH and mix by the mass ratio of 1: 6 and grind to form uniform powder, be subsequently placed in pipe
In formula stove, with the ramp to 800 DEG C of 6 DEG C/min under argon atmosphere, and constant temperature activation 1h, take after temperature drops to room temperature
Go out；
4) pickling: by the dilute hydrochloric acid washing that activation products mass fraction is 10%, then wash with water to neutrality, the most rearmounted
It is dried in 80 DEG C of air dry ovens, i.e. obtains porous carbon electrode material.
2. the preparation of ultracapacitor working electrode
Take ultracapacitor porous carbon electrode material, conductive agent (Super P), binding agent (PTFE), be 8 in mass ratio:
0.5: 0.5 mixing, with mortar mix homogeneously and be modulated into pulpous state after adding appropriate ethanol, drops in rustless steel by the homogenate made
On net and nickel foam, (electrode slice prepared by stainless (steel) wire is for H2SO4In electrolyte test, electrode slice prepared by nickel foam for
KOH electrolyte is tested), it is then transferred to 80 DEG C of dry 12h in vacuum drying oven, finally takes out electrode slice, standby after weighing.
3. sample test
Same as in Example 1, the results are shown in Table 5.
The ratio electric capacity of table 5 embodiment 4 porous carbon materials
Claims (6)
1. one kind utilizes the method that culture medium of edible fungus garbage prepares ultracapacitor porous carbon electrode material, it is characterised in that
Comprise the following steps:
1) pre-treatment: clean to neutral with water after culture medium of edible fungus garbage is first soaked 5～20h with dilute hydrochloric acid, then use
Acetone soak 5～20h, washs 3-4 time respectively with water and dehydrated alcohol the most successively, is finally put in oven for drying；
2) carbonization: the culture medium of edible fungus garbage after drying is placed in tube furnace, with 2～6 DEG C/min under argon atmosphere
Ramp to 500～700 DEG C, and constant temperature carbonization 0.5～5h, after temperature drops to room temperature, take out carbonized product；
3) activation: carbonized product and KOH mixed by the mass ratio of 1: 2～6 and is ground to uniform powder, being subsequently placed in tubular type
In stove, with the ramp to 700～800 DEG C of 2～6 DEG C/min under argon atmosphere, and constant temperature activation 1～3h, treat that temperature drops
Activation products are taken out after room temperature；
4) pickling: activation products first washed with dilute hydrochloric acid, be washed with water to neutrality, is finally placed in air dry oven dry
Dry, i.e. obtain ultracapacitor porous carbon electrode material.
The method preparing ultracapacitor porous carbon electrode material the most as claimed in claim 1, it is characterised in that: step 2)
In, the heating rate of described carbonization is 3 DEG C/min, and carburizing temperature is 700 DEG C, and carbonization time is 1h.
The method preparing ultracapacitor porous carbon electrode material the most as claimed in claim 1, it is characterised in that: step 3)
In, described carbonized product is 1: 4 with the mass ratio of KOH.
The method preparing ultracapacitor porous carbon electrode material the most as claimed in claim 1, it is characterised in that: step 3)
In, the heating rate of described activation is 3 DEG C/min, and activation temperature is 750 DEG C, and soak time is 3h.
5. a ultracapacitor working electrode, is made up of ultracapacitor porous carbon electrode material, conductive agent, binding agent, its
It is characterised by: described ultracapacitor porous carbon electrode material is to prepare according to the method described in Claims 1 to 4 any one
's.
6. ultracapacitor working electrode as claimed in claim 5, it is characterised in that: described conductive agent is Super P, bonding
Agent is PTFE, described ultracapacitor porous carbon electrode material: conductive agent: the mass ratio of binding agent is 8: 1: 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107424846A (en) * | 2017-06-14 | 2017-12-01 | 亿曼丰科技（深圳）有限公司 | Ultracapacitor based on inverse-excitation type switch power-supply low pass filter |
| CN107602126A (en) * | 2017-09-27 | 2018-01-19 | 张绍乙 | A kind of preparation method of porous carbon-silicon composite material |
| CN108022762A (en) * | 2016-11-11 | 2018-05-11 | 南京大学 | The method that nitrating porous carbon electrode material for super capacitor is prepared based on peanut shell |
| CN108109853A (en) * | 2017-12-25 | 2018-06-01 | 武汉大学 | The preparation method and application of superelevation specific surface porous carbon biomass electrode material |
| CN110112003A (en) * | 2019-04-01 | 2019-08-09 | 中国矿业大学 | A method of recycling industrial waste Oil Paint Slag prepares electrode material for super capacitor |
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| CN105244178A (en) * | 2015-10-28 | 2016-01-13 | 王彦博 | Super capacitor and preparation method thereof |
| CN105731452A (en) * | 2016-01-22 | 2016-07-06 | 青岛大学 | Active carbon electrode material as well as preparation method and application thereof |
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| JP2013249234A (en) * | 2012-06-01 | 2013-12-12 | Nankai Kogyo Kk | Activated carbon and method for producing the same |
| CN102689875A (en) * | 2012-06-11 | 2012-09-26 | 合肥工业大学 | Method for preparing microbiologically treated carbon material for supercapacitor |
| CN105244178A (en) * | 2015-10-28 | 2016-01-13 | 王彦博 | Super capacitor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108022762A (en) * | 2016-11-11 | 2018-05-11 | 南京大学 | The method that nitrating porous carbon electrode material for super capacitor is prepared based on peanut shell |
| CN107424846A (en) * | 2017-06-14 | 2017-12-01 | 亿曼丰科技（深圳）有限公司 | Ultracapacitor based on inverse-excitation type switch power-supply low pass filter |
| CN107602126A (en) * | 2017-09-27 | 2018-01-19 | 张绍乙 | A kind of preparation method of porous carbon-silicon composite material |
| CN107602126B (en) * | 2017-09-27 | 2020-10-30 | 张绍乙 | Preparation method of porous carbon-silicon composite material |
| CN108109853A (en) * | 2017-12-25 | 2018-06-01 | 武汉大学 | The preparation method and application of superelevation specific surface porous carbon biomass electrode material |
| CN110112003A (en) * | 2019-04-01 | 2019-08-09 | 中国矿业大学 | A method of recycling industrial waste Oil Paint Slag prepares electrode material for super capacitor |
| CN110112003B (en) * | 2019-04-01 | 2020-12-25 | 中国矿业大学 | Method for preparing supercapacitor electrode material by recycling industrial waste paint residues |
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Application publication date: 20161109 |