CN109455716A - A kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group - Google Patents
A kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group Download PDFInfo
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- CN109455716A CN109455716A CN201811235417.0A CN201811235417A CN109455716A CN 109455716 A CN109455716 A CN 109455716A CN 201811235417 A CN201811235417 A CN 201811235417A CN 109455716 A CN109455716 A CN 109455716A
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- super capacitor
- active carbon
- capacitor active
- functional group
- surface oxygen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
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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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- 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
A kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group is that super capacitor active carbon is placed in the pallet in micro-wave oven, then microwave cavity is purged with inert atmosphere, the oxygen content value of microwave cavity is set to be down to 2-10ppm, open micro-wave oven, microwave heating time is 0.5-1min, and natural cooling has the super capacitor active carbon of ultra low surface oxygen-containing functional group to obtain the final product.The present invention has the advantages of simple process, low energy consumption, time-consuming short, and the oxygen-containing functional group of super capacitor active carbon can be greatly reduced.
Description
Technical field
The invention belongs to a kind of fields for reducing charcoal material surface functional group, relate in particular to a kind of reduction super capacitor
The method of activated carbon surface oxygen-containing functional group.
Background technique
Super capacitor active carbon is with high specific surface area, Gao Kongrong, high conductivity, low ash point, low metal ion, granule
The unique advantages such as diameter can be widely applied in the new energy energy storage devices such as supercapacitor, lead carbon battery, lithium-sulfur cell.Wherein,
The oxygen-containing functional group on super capacitor active carbon surface has stronger activity, carries out being easy to happen when charge and discharge in energy storage device
Decomposition reaction, and then the performance of electrolyte is influenced, cause the cycle performance of energy storage device unstable.To keep energy storage device higher
Cyclical stability, reduce super capacitor active carbon surface oxygen-containing functional group it is imperative.Currently, reducing super capacitor activity
The method of carbon surface oxygen-containing functional group is primarily introduced into reducing agent or carries out high-temperature hydrogen heat treatment, such as Li Kaixi (patent disclosure
Number: CN101597056A) etc. hydrazine hydrate, NaOH and diglycol are introduced in active carbon, then heat 190-220 DEG C,
To which oxygen-containing functional group be restored.But the above method can largely introduce miscellany substance, subsequent there is still a need for being further purified, technique mistake
Journey is excessively complicated.Such as shut out Huan (research of the hydrogen reducing to activated carbon electrodes Electrochemical Performances, Chinese solid-state ionics and state
Border electric powered motor technical seminar, 2006) etc. using commercial activated charcoal as raw material, 1h is pyrolyzed under 873K hydrogen atmosphere and is gone
It is high although can reduce the oxygen-containing functional group on super capacitor active carbon surface by above-mentioned technological means except oxygen-containing functional group
Warming treatment process, energy consumption is high, time-consuming, the loss of product is high, and the cost of super capacitor active carbon is caused to sharply increase.
Microwave is a kind of high-frequency electromagnetic wave, material can be made to be heated evenly, and accelerates super capacitor active carbon surface official
The fracture that can be rolled into a ball, to reduce the oxygen-containing functional group of material itself.In addition, being different from above-mentioned process route, microwave is to super electricity
The specific surface area and average pore size for holding active carbon do not influence.However, having not yet to see related patents or document report.
Summary of the invention
The purpose of the present invention is to provide a kind of simple process, low energy consumption, time-consuming short has the oxygen-containing function of ultra low surface
The preparation method of the super capacitor active carbon of group.
The present invention be regulated and controled by way of microwave heating using super capacitor active carbon as raw material microwave power and when
Between realize reduce super capacitor active carbon surface oxygen functional group purpose.Its principle is the magnetron by micro-wave oven, will be electric
Microwave can be converted to.Fast vibration is broken after the surface oxygen functional group of super capacitor active carbon absorbs microwave, it is final realize from
The purpose that Carbon Materials itself remove.
The present invention is achieved by the following technical scheme:
(1) super capacitor active carbon is placed in the pallet in micro-wave oven, it is then (every for 1-12ml/ming with flow velocity
Inert atmosphere required for every gram of super capacitor active carbon of minute) inert atmosphere purging microwave cavity 0.1-0.5min, make micro-
The oxygen content value of wave furnace chamber is down to 2-10ppm；
(2) open micro-wave oven, microwave power 0.1-0.5kWg, microwave heating time 0.5-1min, in microwave plus
Inert atmosphere flow velocity is reduced to 0.5-1ml/ming in thermal process；
(3) after microwave heating, natural cooling has the super capacitor active carbon of ultra low surface oxygen-containing functional group to obtain the final product.
Inert atmosphere as described above is argon gas, helium or nitrogen.
The specific surface area of the super capacitor active carbon of step (1) as described above is in 1500-2800m2Between/g, relatively optimization
Specific surface area is in 1600-2200m2Between/g, more optimal specific surface area is in 1600-2000m2Between/g.It is tested through many experiments
Card, the large specific surface area of super capacitor active carbon, hole is flourishing, in the surface oxygen functional group heated time of pore interior, heat
There is bigger difference in the field of force, microwave field, therefore the uniformity of oxygen-containing functional group fracture and stability are also inconsistent.When specific surface area is low
In 1500m2When/g, super capacitor active carbon exists largely without through hole, it is difficult to be conducted by thermal field；Work as specific surface area
Higher than 2800m2When/g, there are a large amount of through holes for super capacitor active carbon, it is difficult to be conducted by microwave field, two kinds of situations are equal
Cause surface oxygen functional group fracture insufficient.
Between 2.0-3.2nm, relatively optimization is averaged the average pore size of the super capacitor active carbon of step (1) as described above
Aperture is between 2-3nm, and more optimal average pore size is between 2.5-2.8nm.The average pore size pair of super capacitor active carbon
Its Electrochemical Performances is larger.Through lot of experiment validation, the solvated ion diameter of organic electrolyte is usually the left side 0.8nm
The right side, and the aperture that electrolyte ion is capable of free shuttling necessarily is greater than 2.5-4 times of solvated ion diameter.Hole lower than 2nm
Diameter reduces shuttle rate of the electrolyte ion in super capacitor active carbon hole, and then reduces the power characteristic of energy storage；It is high
It is unfavorable for charge storage of the electrolyte ion in super capacitor active carbon hole in the aperture of 3.2nm, and then reduces energy storage
Energy response.
The mass percent that the surface oxygen functional group of step (1) as described above accounts for super capacitor active carbon is 1-
10%.Compared with optimization surface oxygen functional group account for super capacitor active carbon mass percent be 1-5%, more optimal surface
The mass percent that oxygen-containing functional group accounts for super capacitor active carbon is 1-3%.Through the titration of Boehm functional group and elemental analysis inspection
It surveys, there are the oxygen-containing functional groups such as a large amount of carboxyl, hydroxyl, carbonyl, lactone group for super capacitor active carbon, due to super capacitor activity
Charcoal is by high-temperature heat treatment, and surface oxygen functional group mainly exists in the form of the stronger carbonyl of deactivation, quinonyl etc..This
A little functional group contents are higher, more difficult by microwave treatment.
Surface oxygen functional group in the super capacitor active carbon of the ultra low surface oxygen-containing functional group of step (3) as described above
The mass percent for accounting for super capacitor active carbon is 0.02-0.2%.
The present invention has the advantage that
This method process route is simple, and low energy consumption, time-consuming short, is conducive to industrialization promotion.
This method prepares the oxygen-containing functional group that super capacitor active carbon can be greatly reduced.
This method is except reduction oxygen-containing functional group, moreover it is possible to capacitance carbon be made to keep original specific surface area and average pore size.
Specific embodiment
Embodiment 1:
By 10g super capacitor active carbon (specific surface area: 1500m2/ g, average pore size: 3.2nm, surface oxygen functional group account for
The mass percent 1% of super capacitor active carbon) it is placed in the pallet in micro-wave oven, it is then the argon of 10ml/min with flow velocity
Microwave cavity 5min is swept in air-blowing, and the oxygen content value of microwave cavity is made to be down to 10ppm.Micro-wave oven is opened, microwave power is
1kW, microwave heating time 10min, argon gas flow velocity is reduced to 5ml/min in microwave heating process.After microwave heating, from
It is so cooling that up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor activity
The mass percent of charcoal is 0.02%, specific surface area: 1500m2/ g, average pore size: 3.2nm).
In contrast, it is placed in the pallet in box high-temperature hydrogen reduction furnace using above-mentioned 10g super capacitor active carbon, so
Hydrogen reducing furnace chamber 5min is purged for the argon gas of 10ml/min with flow velocity afterwards, is down to the oxygen content value of microwave cavity
10ppm.Hydrogen reducing furnace is opened, is warming up to 750 DEG C with 5 DEG C/min heating rate.It is passed through 3% (volume ratio) at this temperature
Hydrogen simultaneously keeps 40min.Stop logical hydrogen and natural cooling has the super capacitor of ultra low surface oxygen-containing functional group active to obtain the final product
Charcoal, surface oxygen functional group account for the variation of the mass percent and specific surface area and average pore size of super capacitor active carbon such as
Shown in table 1.The similar embodiment 1 of embodiments described below, is shown in Table 1.
Embodiment 2:
By 10g super capacitor active carbon (specific surface area: 1600m2/ g, average pore size: 3.0nm, surface oxygen functional group account for
The mass percent of super capacitor active carbon: 2%) being placed in the pallet in micro-wave oven, is then the argon of 30ml/min with flow velocity
Microwave cavity 5min is swept in air-blowing, and the oxygen content value of microwave cavity is made to be down to 6ppm.Unlatching micro-wave oven, microwave power 2kW,
Microwave heating time is 9min, and argon gas flow velocity is reduced to 6ml/min in microwave heating process.It is naturally cold after microwave heating
But up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor active carbon
Mass percent is 0.05%, specific surface area: 1600m2/ g, average pore size: 3.0nm).
Embodiment 3:
By 10g super capacitor active carbon (specific surface area: 2000m2/ g, average pore size: 2.8nm, surface oxygen functional group account for
The mass percent of super capacitor active carbon: 4%) being placed in the pallet in micro-wave oven, is then the nitrogen of 50ml/min with flow velocity
Microwave cavity 4min is swept in air-blowing, and the oxygen content value of microwave cavity is made to be down to 4ppm.Unlatching micro-wave oven, microwave power 3kW,
Microwave heating time is 8min, and argon gas flow velocity is reduced to 7ml/min in microwave heating process.It is naturally cold after microwave heating
But up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor active carbon
Mass percent is 0.08%, specific surface area: 2000m2/ g, average pore size: 2.8nm).
Embodiment 4:
By 10g super capacitor active carbon (specific surface area: 2200m2/ g, average pore size: 2.5nm, surface oxygen functional group account for
The mass percent of super capacitor active carbon: 6%) being placed in the pallet in micro-wave oven, is then the nitrogen of 80ml/min with flow velocity
Microwave cavity 3min is swept in air-blowing, and the oxygen content value of microwave cavity is made to be down to 2ppm.Unlatching micro-wave oven, microwave power 4kW,
Microwave heating time is 7min, and argon gas flow velocity is reduced to 8ml/min in microwave heating process.It is naturally cold after microwave heating
But up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor active carbon
Mass percent is 0.13%, specific surface area: 2200m2/ g, average pore size: 2.5nm).
Embodiment 5:
By 10g super capacitor active carbon (specific surface area: 2600m2/ g, average pore size: 2.2nm, surface oxygen functional group account for
The mass percent of super capacitor active carbon: 8%) being placed in the pallet in micro-wave oven, is then the helium of 100ml/min with flow velocity
Microwave cavity 2min is swept in air-blowing, and the oxygen content value of microwave cavity is made to be down to 4ppm.Unlatching micro-wave oven, microwave power 5kW,
Microwave heating time is 6min, and argon gas flow velocity is reduced to 9ml/min in microwave heating process.It is naturally cold after microwave heating
But up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor active carbon
Mass percent is 0.2%, specific surface area: 2600m2/ g, average pore size: 2.2nm).
Embodiment 6:
By 10g super capacitor active carbon (specific surface area: 2800m2/ g, average pore size: 2.0nm, surface oxygen functional group account for
The mass percent of super capacitor active carbon: 10%) being placed in the pallet in micro-wave oven, is then 120ml/min's with flow velocity
Helium purge microwave cavity 1min makes the oxygen content value of microwave cavity be down to 8ppm.Micro-wave oven is opened, microwave power is
5kW, microwave heating time 5min, argon gas flow velocity is reduced to 10ml/min in microwave heating process.After microwave heating, from
It is so cooling that up to the super capacitor active carbon with ultra low surface oxygen-containing functional group, (surface oxygen functional group accounts for super capacitor activity
The mass percent of charcoal is 0.06%, specific surface area: 2800m2/ g, average pore size: 2.0nm).
The comparison of two methods of 1 microwave of table and high-temperature hydrogen reduction removal surface oxygen functional group
Claims (12)
1. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group, it is characterised in that including as follows
Step:
(1) super capacitor active carbon is placed in the pallet in micro-wave oven, is then that 1-12ml/ming(is per minute with flow velocity
Inert atmosphere required for every gram of super capacitor active carbon) inert atmosphere purging microwave cavity 0.1-0.5min, make micro-wave oven
The oxygen content value of inner cavity is down to 2-10ppm；
(2) micro-wave oven, microwave power 0.1-0.5kWg, microwave heating time 0.5-1min, in microwave heating are opened
Inert atmosphere flow velocity is reduced to 0.5-1ml/ming in journey；
(3) after microwave heating, natural cooling has the super capacitor active carbon of ultra low surface oxygen-containing functional group to obtain the final product.
2. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as described in claim 1,
It is characterized in that the inert atmosphere is argon gas, helium or nitrogen.
3. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as described in claim 1,
It is characterized in that the specific surface area of the super capacitor active carbon is in 1500-2800m2Between/g.
4. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 3,
It is characterized in that the specific surface area of the super capacitor active carbon is in 1600-2200 m2Between/g.
5. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 4,
It is characterized in that the specific surface area of the super capacitor active carbon is in 1600-2000 m2Between/g.
6. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as described in claim 1,
It is characterized in that the average pore size of the super capacitor active carbon is between 2.0-3.2nm.
7. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 6,
It is characterized in that the average pore size of the super capacitor active carbon is between 2-3nm.
8. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 7,
It is characterized in that the average pore size of the super capacitor active carbon is between 2.5-2.8nm.
9. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as described in claim 1,
It is characterized in that the surface oxygen functional group in the super capacitor active carbon of the step (1) accounts for the matter of super capacitor active carbon
Amount percentage is 1-10%.
10. a kind of preparation method of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 9,
It is characterized in that the surface oxygen functional group in the super capacitor active carbon of the step (1) accounts for the matter of super capacitor active carbon
Amount percentage is 1-5%.
11. a kind of preparation side of the super capacitor active carbon with ultra low surface oxygen-containing functional group as claimed in claim 10
Method, it is characterised in that the surface oxygen functional group in the super capacitor active carbon of the step (1) accounts for super capacitor active carbon
Mass percent be 1-3%.
12. the super capacitor active carbon of the ultra low surface oxygen-containing functional group such as any one of claim 1-11 the method preparation,
It is characterized in that the surface oxygen functional group in the super capacitor active carbon of ultra low surface oxygen-containing functional group accounts for super capacitor activity
The mass percent of charcoal is 0.02-0.2%.
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Cited By (3)
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| CN112479209A (en) * | 2020-11-25 | 2021-03-12 | 河南省大潮炭能科技有限公司 | Low-temperature functional group removal by chemical method |
| CN114377653A (en) * | 2021-12-17 | 2022-04-22 | 农业部沼气科学研究所 | Directional rapid modification method of oxygen-containing functional groups on surface of activated carbon |
| CN115083788A (en) * | 2022-06-16 | 2022-09-20 | 广西科技大学 | Biomass-based high voltage-resistant porous carbon material and preparation method and application thereof |
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Cited By (3)
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| CN115083788A (en) * | 2022-06-16 | 2022-09-20 | 广西科技大学 | Biomass-based high voltage-resistant porous carbon material and preparation method and application thereof |
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