CN110482548A - A method of removing super capacitor active carbon oxygen-containing functional group - Google Patents
A method of removing super capacitor active carbon oxygen-containing functional group Download PDFInfo
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- CN110482548A CN110482548A CN201910834110.0A CN201910834110A CN110482548A CN 110482548 A CN110482548 A CN 110482548A CN 201910834110 A CN201910834110 A CN 201910834110A CN 110482548 A CN110482548 A CN 110482548A
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- active carbon
- super capacitor
- capacitor active
- oxygen
- functional group
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- 239000003990 capacitor Substances 0.000 title claims abstract description 81
- 125000000524 functional group Chemical group 0.000 title claims abstract description 31
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 59
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 56
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000001301 oxygen Substances 0.000 claims abstract description 44
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 44
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 24
- 238000010792 warming Methods 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012530 fluid Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 16
- 239000003610 charcoal Substances 0.000 description 14
- 238000007789 sealing Methods 0.000 description 7
- 230000009467 reduction Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001146 hypoxic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to a kind of methods for removing super capacitor active carbon oxygen-containing functional group, belong to super capacitor active carbon preparation technical field, super capacitor active carbon is solved because oxygen-containing height leads to the technical problem of cyclical stability difference, solution are as follows: be warming up to super capacitor active carbon investment in 180 DEG C -320 DEG C of fluid unit in advance, by being passed through a certain proportion of nitrogen hydrogen mixeding gas.180 DEG C -320 DEG C at a temperature of, active carbon and hydrogen full and uniform haptoreaction carry out rewinding after 10min-30min.The process can effectively remove active carbon oxygen-containing functional group, have good economy and adaptability, be suitable for industrialized production.
Description
Technical field
The invention belongs to super capacitor active carbon preparation technical fields, and in particular to be a kind of removing super capacitor activity
The method of charcoal oxygen-containing functional group.
Background technique
Supercapacitor is the interfacial bilayer by being formed between electrode and electrolyte come the new component of storage energy.
Its electrode material is mainly porous carbon materials, including active powdered carbon, activated carbon fibre, carbon nanotube and carbon gels etc., wherein surpassing
Grade capacitor active carbon is exactly outstanding person therein, but the oxygen-containing functional group on super capacitor active carbon surface has stronger electrification
Activity is learned, reaction of easily decomposing in charge and discharge follows the decline of bad stability so as to cause supercapacitor, so removing is super
Grade capacitor activated carbon surface oxygen-containing functional group has great science and application value.
Currently, the technique of deoxidation passivation is primarily introduced into reducing agent or carries out high temperature thermal reduction.As Zhang Zhong (publication number:
106082210 A of CN) etc. put the raw materials into reduction furnace, be warming up to 650-1200 DEG C by reduction furnace, high temperature is passed through protection gas
Body, static state are fired, and 1-6h is restored.This method has the disadvantage that be heat-treated by high temperature, and energy consumption increases, and cost is increase accordingly；Also
The former time is long, low efficiency；Static state is fired, and heat leak is uneven, and reduction is uneven；Temperature is too high to be easy to cause collapsing for hole,
Specific surface area is reduced.Such as Du Piyi (109592681 A of publication number CN) by activated carbon sample under reducing atmosphere, at 300 DEG C
When roast 1~2h, remove surface texture in oxygen-containing functional group, obtain electrode material for super capacitor highly pure active charcoal.Have
Following disadvantage: static state roasting, reducing gas need to permeate into, and the recovery time is long, and loss reducing gas amount is big.
Summary of the invention
In order to overcome the deficiencies in the prior art, super capacitor active carbon is solved because oxygen-containing height leads to cyclical stability
The technical problem of difference, the present invention provide a kind of simple process, low energy consumption, it is high-efficient, be easy to industrialized removing super capacitor work
The method of property charcoal oxygen-containing functional group.The super-active capacitance carbon oxygen content of acquisition is low, and technical process has, consumption lower using temperature
Can be small, reaction is abundant, time-consuming is short, the product proportion of goods damageds are low, increase specific surface area the advantages that.
The present invention is achieved by the following technical programs.
A method of removing super capacitor active carbon oxygen-containing functional group, comprising the following steps:
S1, fluidized bed is warming up to 180 DEG C -320 DEG C, super capacitor active carbon then is added on the bed of fluidized bed；
S2, the temperature-resistant of fluidized bed is kept, is passed through nitrogen and hydrogen mixture into fluidized bed from the feed inlet of fluidized bed, reacts 10-
30min removes the oxygen-containing functional group of super capacitor active carbon；
S3, to step S2 after reaction, fluidized bed is naturally cooling to room temperature, nitrogen or argon gas is then led into furnace, by step
Super capacitor active carbon made from S2 is blown out and is collected by the discharge port of fluidized bed.
Further, in the step S1, the oxygen content of the super capacitor active carbon is 3-12wt%.
Further, in the step S2, the mass ratio of super capacitor active carbon and hydrogen are as follows: 9:1-18:1.
Further, in the step S2, the volume ratio of hydrogen is 5%-30% in the nitrogen and hydrogen mixture.
Further, in the step S3, the oxygen content of super capacitor active carbon obtained is 0.01-0.2wt%.
The invention has the following beneficial effects:
1, this technique can quickly, simplicity be prepared into hypoxic super-active capacitance carbon, temperature is relatively low, less energy-consuming,
Reaction is abundant, time-consuming short, and the product proportion of goods damageds are low, increase specific surface area, significantly reduce rate of oxygen, has good economy
And adaptability, it is suitable for industrialized production.Super capacitor active carbon oxygen content after deoxidation is 0.01-0.2wt%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of fluidized bed used in present invention removing super capacitor active carbon oxygen-containing functional group.
In figure: 1 is feed inlet, and 2 be air inlet, and 3 be discharge port, and 4 be sealing shell, and 5 be gas outlet, and 6 be bed.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1
By the raw material (specific surface area: 1800m of 10g active carbon2 / g, oxygen content 3wt%) the preparatory stream for being warming up to 300 DEG C of investment
On the bed for changing bed (as shown in Figure 1)；The fluidized bed includes sealing shell 4 and bed 6, and bed 6 is set to sealing shell 4
The intracorporal lower part of chamber, the top of sealing shell 4 are set as gas outlet 5, and the bottom of sealing shell 4 is set as air inlet 2, and sealing is outer
The top of 4 side wall of shell is provided with feed inlet 1, the lower part of 4 side wall of the sealing shell and top for being located at bed 6 is provided with discharge port
3；
The nitrogen and hydrogen mixture of hydrogen content 5% is passed through into fluidized bed from the air inlet 2 of fluidized bed, and in 300 DEG C of at a temperature of constant temperature
18min is reacted, the oxygen-containing functional group of super capacitor active carbon is removed；
Naturally then near room temperature after reaction leads to nitrogen into reaction bed or super capacitor active carbon is blown out and received by argon gas
Collection.(super capacitor active carbon oxygen content is 0.12wt%, specific surface area: 1876m to obtained super capacitor active carbon2 /g)。
Introduce reducing agent: by the raw material (specific surface area: 1800m of 10g active carbon2 / g, oxygen content 3wt%) leading in hydrogen
Under atmosphere, 2h is roasted at 300 DEG C, is removed the oxygen-containing functional group in surface texture, is obtained super capacitor active carbon (super capacitor
Active carbon oxygen content is 2.72wt%, specific surface area: 1783m 2 /g)。
High temperature reduction: the raw material (specific surface area: 1800m2/g, oxygen content 3wt%) of 10g active carbon is placed in tube furnace
In high pure nitrogen protection under 850 DEG C of constant temperature 5h.Room temperature is naturally cooled under inert atmosphere protection, obtains super capacitor activity
Charcoal (super capacitor active carbon oxygen content is 1.76wt%, specific surface area: 2/g of 1207m).
It can be seen that as introducing super capacitor active carbon product made from two methods of reducing agent and high temperature reduction,
Oxygen content is than the high oxygen content of the product obtained according to scheme provided by the present application, and specific surface area according to the application than providing
The obtained specific surface area of product of scheme it is low.So super capacitor active carbon made from technical solution provided by the invention, increases
Big specific surface area, simultaneously effective reduces rate of oxygen.
Embodiment 2
By the raw material (specific surface area: 1700m of 10g active carbon2/ g, oxygen content 5wt%) the preparatory stream for being warming up to 300 DEG C of investment
On the bed 6 for changing bed apparatus (as shown in Figure 1)；The nitrogen hydrogen mixing of hydrogen content 5% is passed through into fluidized bed from fluidized bed feed inlet 2
Gas, and in 300 DEG C of at a temperature of isothermal reaction 18min, remove the oxygen-containing functional group of super capacitor active carbon；After reaction certainly
Then right near room temperature leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.Obtained super capacitor is living
Property charcoal (super capacitor active carbon oxygen content be 0.40wt%, specific surface area: 1733m2/g)。
Embodiment 3
By the raw material (specific surface area: 1700m of 10g active carbon2 / g, oxygen content 5wt%) the preparatory stream for being warming up to 270 DEG C of investment
On the bed 6 for changing bed apparatus (as shown in Figure 1)；The nitrogen hydrogen mixing of hydrogen content 5% is passed through into fluidized bed from fluidized bed feed inlet 2
Gas, and in 270 DEG C of at a temperature of isothermal reaction 15min, remove the oxygen-containing functional group of super capacitor active carbon；After reaction certainly
Then right near room temperature leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.Obtained super capacitor is living
Property charcoal (super capacitor active carbon oxygen content be 0.25wt%, specific surface area: 1756m2/g)。
Embodiment 4
By the raw material (specific surface area: 1700m of 10g active carbon2 / g, oxygen content 5wt%) the preparatory stream for being warming up to 320 DEG C of investment
On the bed 6 for changing bed apparatus (as shown in Figure 1)；The nitrogen hydrogen mixing of hydrogen content 5% is passed through into fluidized bed from fluidized bed feed inlet 2
Gas, and in 320 DEG C of at a temperature of isothermal reaction 10min, remove the oxygen-containing functional group of super capacitor active carbon；After reaction certainly
Then right near room temperature leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.Obtained super capacitor is living
Property charcoal (super capacitor active carbon oxygen content be 0.15wt%, specific surface area: 1812m2/g)。
Embodiment 5
By the raw material (specific surface area: 2300m of 20g active carbon2 / g, oxygen content 10wt%) investment is warming up to 260 DEG C in advance
On the bed 6 of fluid unit (as shown in Figure 1)；The nitrogen hydrogen that hydrogen content 5% is passed through into fluidized bed from fluidized bed feed inlet 2 is mixed
Close gas, and 260 DEG C at a temperature of keep 30min reacted, remove the oxygen-containing functional group of super capacitor active carbon；Reaction knot
Naturally then near room temperature after beam leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.What is obtained is super
(super capacitor active carbon oxygen content is 0.50wt%, specific surface area: 2380m to capacitor active carbon2/g)。
Embodiment 6
By the raw material (specific surface area: 2300m of 20g active carbon2/ g, oxygen content 10wt%) the preparatory stream for being warming up to 260 DEG C of investment
On the bed 6 for changing bed apparatus (as shown in Figure 1)；The nitrogen hydrogen mixing of hydrogen content 17% is passed through into fluidized bed from fluidized bed feed inlet 2
Gas, and in 260 DEG C of at a temperature of isothermal reaction 27min, remove the oxygen-containing functional group of super capacitor active carbon；After reaction certainly
Then right near room temperature leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.Obtained super capacitor is living
Property charcoal (super capacitor active carbon oxygen content be 0.29wt%, specific surface area: 2383m2/g)。
Embodiment 7
By the raw material (specific surface area: 2300m of 20g active carbon2 / g, oxygen content 10wt%) investment is warming up to 260 DEG C in advance
On the bed 6 of fluid unit (as shown in Figure 1)；The nitrogen hydrogen that hydrogen content 30% is passed through into fluidized bed from fluidized bed feed inlet 2 is mixed
Gas is closed, and in 260 DEG C of at a temperature of isothermal reaction 21min, removes the oxygen-containing functional group of super capacitor active carbon；After reaction
Naturally then near room temperature leads to nitrogen into furnace or super capacitor active carbon is blown out and collected by argon gas.Obtained super capacitor
(super capacitor active carbon oxygen content is 0.25wt%, specific surface area: 2382m to active carbon2/g)。
Embodiment 8
By the raw material (specific surface area: 2300m of 10g active carbon2/ g, oxygen content 10wt%) the preparatory stream for being warming up to 260 DEG C of investment
On the bed 6 for changing bed apparatus (as shown in Figure 1)；From the feed inlet 2 of fluidized bed into fluidized bed by be passed through activated carbon raw material with
The nitrogen and hydrogen mixture of the mass ratio 15:1 of hydrogen, and in 260 DEG C of at a temperature of isothermal reaction 30min, it is living to remove super capacitor
The oxygen-containing functional group of property charcoal；Naturally then near room temperature after reaction leads to nitrogen or argon gas for super capacitor activity into furnace
Charcoal blows out and collects.Obtain super capacitor active carbon (super capacitor active carbon oxygen amount be 0.25wt%, specific surface area:
2382m2/g)。
Embodiment 9
By the raw material (specific surface area: 2300m of 10g active carbon2 / g, oxygen content 10wt%) investment is warming up to 260 DEG C in advance
On the bed 6 of fluid unit (as shown in Figure 1)；From the feed inlet 2 of fluidized bed into fluidized bed by being passed through activated carbon raw material
It is living to remove super capacitor and in 260 DEG C of at a temperature of isothermal reaction 30min with the nitrogen and hydrogen mixture of the mass ratio 9:1 of hydrogen
The oxygen-containing functional group of property charcoal；Naturally then near room temperature after reaction leads to nitrogen or argon gas for super capacitor activity into furnace
Charcoal blows out and collects.Obtain super capacitor active carbon (super capacitor active carbon oxygen content be 0.40wt%, specific surface area:
2380m2/g)。
Embodiment 10
By the raw material (specific surface area: 2300m of 10g active carbon2 / g, oxygen content 10wt%) investment is warming up to 260 DEG C in advance
On the bed 6 of fluid unit (as shown in Figure 1)；From the feed inlet 2 of fluidized bed into fluidized bed by being passed through activated carbon raw material
Super capacitor is removed and in 260 DEG C of at a temperature of isothermal reaction 30min with the nitrogen and hydrogen mixture of the mass ratio 18:1 of hydrogen
The oxygen-containing functional group of active carbon；Naturally then near room temperature after reaction leads to nitrogen or argon gas super capacitor is living into furnace
Property charcoal blows out and collects.Obtain super capacitor active carbon (super capacitor active carbon oxygen content be 0.23wt%, specific surface area:
2381m2/g)。
The present invention provides a kind of removing oxygen-containing functional groups of super-active capacitance carbon for efficiently preparing low oxygen content
Method, the material after removing oxygen-containing functional group are characterized in that high-specific surface area and low oxygen content.This super-active capacitor
Charcoal provides high specific capacitance, and then high stored energy capacitance and long-time stability are provided in later use.
The above description is only a preferred embodiment of the present invention and is not intended to restrict the invention, in embodiment technical solution
Same replacement is carried out to single or multiple technical parameters and forms new technical solution, equally all in claimed model
In enclosing；For those skilled in the art, the present invention can carry out various modifications and variations.It is all in spirit of the invention and
Any modification, equivalent replacement, improvement and so within principle, should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method for removing super capacitor active carbon oxygen-containing functional group, it is characterised in that the following steps are included:
S1, fluidized bed is warming up to 180 DEG C -320 DEG C, super capacitor active carbon then is added on the bed of fluidized bed；
S2, the temperature-resistant of fluidized bed is kept, is passed through nitrogen and hydrogen mixture into fluidized bed from the feed inlet of fluidized bed, reacts 10-
30min removes the oxygen-containing functional group of super capacitor active carbon；
S3, to step S2 after reaction, fluidized bed is naturally cooling to room temperature, nitrogen or argon gas is then led into furnace, by step
Super capacitor active carbon made from S2 is blown out and is collected by the discharge port of fluidized bed.
2. a kind of method for removing super capacitor active carbon oxygen-containing functional group according to claim 1, it is characterised in that: In
In the step S1, the oxygen content of the super capacitor active carbon is 3-12wt%.
3. a kind of method for removing super capacitor active carbon oxygen-containing functional group according to claim 1, it is characterised in that: In
In the step S2, the mass ratio of super capacitor active carbon and hydrogen are as follows: 9:1-18:1.
4. a kind of method for removing super capacitor active carbon oxygen-containing functional group according to claim 1, it is characterised in that: In
In the step S2, the volume ratio of hydrogen is 5%-30% in the nitrogen and hydrogen mixture.
5. a kind of method for removing super capacitor active carbon oxygen-containing functional group according to claim 1, it is characterised in that: In
In the step S3, the oxygen content of super capacitor active carbon obtained is 0.01-0.2wt%.
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| CN114275783A (en) * | 2022-01-29 | 2022-04-05 | 哈尔滨工业大学 | Mechanical ball milling based chemical activation porous carbon pore depth regulation and control method and compact energy storage application |
| CN114275763A (en) * | 2021-12-27 | 2022-04-05 | 天津大学 | Method for removing trace oxygen in porous carbon at low temperature |
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| CN111574642B (en) * | 2020-06-23 | 2021-03-19 | 湖南如虹制药有限公司 | Purification method of sugammadex sodium |
| CN114275763A (en) * | 2021-12-27 | 2022-04-05 | 天津大学 | Method for removing trace oxygen in porous carbon at low temperature |
| CN114275783A (en) * | 2022-01-29 | 2022-04-05 | 哈尔滨工业大学 | Mechanical ball milling based chemical activation porous carbon pore depth regulation and control method and compact energy storage application |
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