CN106219539A - A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon - Google Patents
A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon Download PDFInfo
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- CN106219539A CN106219539A CN201610592426.XA CN201610592426A CN106219539A CN 106219539 A CN106219539 A CN 106219539A CN 201610592426 A CN201610592426 A CN 201610592426A CN 106219539 A CN106219539 A CN 106219539A
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- activated carbon
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- 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
- C01P2006/12—Surface area
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- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The present invention relates to the preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon; the present invention is with sucrose as raw material; sucrose is mixed according to mass ratio is soluble in water with ammonium hydrogen carbonate; compound is carried out lyophilization; again the material after lyophilization is placed in high temperature furnace, under the protection of inert atmosphere, is brought rapidly up to preset temperature; carry out high temperature cabonization, prepare the activated carbon of high-specific surface area hierarchical porous structure.The activated carbon that the present invention prepares has higher specific surface area, and specific surface area reaches 1950 2360m2/g；And the activated carbon for preparing of the present invention has an abundant pore structure, micropore, mesoporous, macropore coexist, wherein microporosity be 53 63%, mesoporous rate be 27 32%, big porosity is 5 18%.
Description
Technical field
The invention belongs to activated carbon preparing technical field, be specifically related to a kind of high-specific surface area hierarchical porous structure activated carbon
Preparation method.
Background technology
Activated carbon is to have the carbonaceous adsorbing material that pore structure is flourishing, specific surface area is big, selective adsorption capacity is strong.?
Under conditions of Yi Ding, a certain or Cucumber of liquid or gas is carried out adsorbing and removing, purifies, refines or reclaim, thus real
Refined and the purification of environment of existing product.Even to this day, activated carbon be widely used in industry, agricultural, national defence, traffic,
The every field such as food, medicine, environmental conservation.The raw material preparing activated carbon at present mainly has Linesless charcoal, wood flour, various shell, coal
Charcoal and the contour carbonaceous material of petroleum coke.The method preparing activated carbon at present conventional has physical activation method, chemical activation method or physics
The method that activation is combined with chemical activation.In physical activation method conventional activated gas be steam, carbon dioxide and they
Mixed gas, will the technique that carries out being reacted to form hole with activated gas of the material with carbon element after carbonization.Chemical activation method be by
After various carbon raw materials uniformly mix with chemical drugs or impregnate, at a suitable temperature, through carbonization, activate and reclaim chemistry
The processes such as medicine produce a kind of method of activated carbon.Chemical activating agent used is usually zinc chloride, phosphoric acid or alkali.Physically activated
After referring to first carbon raw material is carried out carbonization, chemical activation with chemical activation combined techniques, then carry out the further reaming of gas activation.
It is generally acknowledged that the hole of activated carbon is made up of macropore, mesopore and micropore, macropore diameter is 50～2000nm, and mesopore is 2～50nm, micro-
Aperture, hole is less than 2nm.
Although the activated carbon that the method for preparation obtains at present has bigger specific surface area, but main based on micropore, hole
Structure is single.Meanwhile, prior art is prepared activated carbon and typically wants first carbonization, then carry out high-temperature activation with chemical activating agent, place
The reason time is long, complex process, and chemical activation reagent contamination environment.
Summary of the invention
It is an object of the invention to provide a kind of high-specific surface area hierarchical porous structure to overcome the deficiencies in the prior art
The preparation method of activated carbon.Sucrose, with sucrose as raw material, is mixed according to mass ratio is soluble in water by the present invention with ammonium hydrogen carbonate, will
Compound carries out lyophilization, then is placed in high temperature furnace by the material after lyophilization, under the protection of inert atmosphere, rises rapidly
Temperature, to preset temperature, carries out high temperature cabonization, prepares the activated carbon of high-specific surface area hierarchical porous structure.The present invention prepares
Activated carbon there is higher specific surface area, specific surface area reaches 1950-2360m2/g；And the activated carbon that the present invention prepares
Having an abundant pore structure, micropore, mesoporous, macropore coexist, wherein microporosity be 53-63%, mesoporous rate be 27-32%, macropore
Rate is 5-18%.
For realizing above-mentioned technical purpose, the technical solution used in the present invention is:
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon, comprises the following steps:
Step (1): sucrose is soluble in water according to mass ratio 5:1-3 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；
By compound lyophilization, obtain lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, under an inert atmosphere；
The thermal treatment zone of high temperature furnace is heated to 700-900 DEG C, then the lyophilization material being placed on room temperature district pushes to adding of high temperature furnace
Hot-zone, and high temperature cabonization 0.5-3h at 700-900 DEG C；It is cooled to room temperature after end and obtains high-specific surface area hierarchical porous structure
Activated carbon.
The further preferred scheme of the preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon that the present invention provides
For:
Wherein, in step (1), sucrose and ammonium hydrogen carbonate are preferably 5:2-3 according to mass ratio；More preferably 5:3.
Wherein, the thermal treatment zone of high temperature furnace is heated to 700-900 DEG C described in (2) by step, and wherein heating rate is 100-
150℃/min；Wherein, the temperature of high temperature cabonization is preferably 800-900 DEG C, and the time of high temperature cabonization is preferably 1.5-2.5h.
Wherein, the inert atmosphere in the present invention is the mixed atmosphere of nitrogen, argon or nitrogen and argon.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon that the present invention proposes, compared with prior art,
Have the beneficial effect that
(1) activated carbon that the present invention prepares has higher specific surface area, and specific surface area reaches 1950-2360m2/
g。
(2) active carbon pore structure that the present invention prepares enriches, and micropore, mesoporous, macropore coexist, and wherein microporosity is
53-63%, mesoporous rate are 27-32%, and big porosity is 5-18%.
(3) present invention process is simple, it is not necessary to through carbonization, the complicated technology of reactivation, directly carries out carbonization；And
The present invention need not product is carried out post processing, and the material after carbonization can directly use.
Detailed description of the invention
Embodiment 1
Step (1): sucrose is soluble in water according to mass ratio 5:1 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；Will
Compound lyophilization, obtains lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, in a nitrogen atmosphere；
The thermal treatment zone of high temperature furnace is heated to 700 DEG C, and wherein heating rate is 100 DEG C/min, then is placed on the lyophilization in room temperature district
Material pushes to the thermal treatment zone of high temperature furnace, and high temperature cabonization 3h at 700 DEG C；It is cooled to room temperature after end and obtains high-specific surface area
The activated carbon of hierarchical porous structure.
Embodiment 2
Step (1): sucrose is soluble in water according to mass ratio 5:2 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；Will
Compound lyophilization, obtains lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, under an argon atmosphere；
The thermal treatment zone of high temperature furnace is heated to 800 DEG C, and wherein heating rate is 100 DEG C/min；It is placed on the lyophilization in room temperature district again
Material pushes to the thermal treatment zone of high temperature furnace, and high temperature cabonization 1.5h at 800 DEG C；It is cooled to room temperature after end and obtains high-ratio surface
The activated carbon of long-pending hierarchical porous structure.
Embodiment 3
Step (1): sucrose is soluble in water according to mass ratio 5:2 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；Will
Compound lyophilization, obtains lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, under an argon atmosphere；
The thermal treatment zone of high temperature furnace is heated to 850 DEG C, and wherein heating rate is 120 DEG C/min；It is placed on the lyophilization in room temperature district again
Material pushes to the thermal treatment zone of high temperature furnace, and high temperature cabonization 2.5h at 850 DEG C；It is cooled to room temperature after end and obtains high-ratio surface
The activated carbon of long-pending hierarchical porous structure.
Embodiment 4
Step (1): sucrose is soluble in water according to mass ratio 5:3 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；Will
Compound lyophilization, obtains lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, in a nitrogen atmosphere；
The thermal treatment zone of high temperature furnace is heated to 900 DEG C, and wherein heating rate is 150 DEG C/min, then is placed on the lyophilization in room temperature district
Material pushes to the thermal treatment zone of high temperature furnace, and high temperature cabonization 0.5h at 900 DEG C；It is cooled to room temperature after end and obtains high-ratio surface
The activated carbon of long-pending hierarchical porous structure.
Performance detects:
The performance measurement result of the activated carbon now embodiment 1-embodiment 4 obtained presents in Table 1, as seen from Table 1
The activated carbon that the present invention prepares has higher specific surface area, and specific surface area reaches 1950-2360m2/g；And system of the present invention
The standby activated carbon obtained has an abundant pore structure, and micropore, mesoporous, macropore coexist, wherein microporosity be 53-63%, mesoporous rate
For 27-32%, big porosity is 5-18%.
The character of the activated carbon that table 1 present invention prepares
| Sample | Specific surface area (m2/g) | Mesoporous rate (%) | Microporosity (%) | Big porosity (%) |
| Embodiment 1 | 1950 | 30 | 53 | 17 |
| Embodiment 2 | 2286 | 32 | 59 | 9 |
| Embodiment 3 | 2360 | 32 | 63 | 5 |
| Embodiment 4 | 2154 | 27 | 55 | 18 |
The explanation being not directed in the detailed description of the invention of the present invention belongs to techniques well known, refers to known technology and adds
To implement.
The present invention, through validation trial, achieves satisfied trial effect.
Embodiments of the present invention are not limited to above-described embodiment, and that makes on the premise of without departing from present inventive concept is various
Within change belongs to protection scope of the present invention.
Claims (6)
1. the preparation method of a high-specific surface area hierarchical porous structure activated carbon, it is characterised in that comprise the following steps:
Step (1): sucrose is soluble in water according to mass ratio 5:1-3 with ammonium hydrogen carbonate, and mix homogeneously obtains compound；Will be mixed
Close material lyophilization, obtain lyophilization material；
Step (2): the room temperature district that the lyophilization material that step (1) obtains is placed in high temperature furnace, under an inert atmosphere；By height
The thermal treatment zone of temperature stove is heated to 700-900 DEG C, then the lyophilization material being placed on room temperature district pushes to the thermal treatment zone of high temperature furnace,
And at 700-900 DEG C high temperature cabonization 0.5-3h；It is cooled to room temperature after end and obtains the activity of high-specific surface area hierarchical porous structure
Charcoal.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon the most according to claim 1, it is characterised in that
In step (1), sucrose is 5:2-3 with the mass ratio of ammonium hydrogen carbonate.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon the most according to claim 1 and 2, its feature exists
In, in step (1), sucrose is 5:3 with the mass ratio of ammonium hydrogen carbonate.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon the most according to claim 1, it is characterised in that
The thermal treatment zone of high temperature furnace is heated to 700-900 DEG C described in (2) by step, and wherein heating rate is 100-150 DEG C/min.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon the most according to claim 1, it is characterised in that
In step (2), the temperature of high temperature cabonization is 800-900 DEG C, and the time of high temperature cabonization is 1.5-2.5h.
The preparation method of a kind of high-specific surface area hierarchical porous structure activated carbon the most according to claim 1, it is characterised in that
Described inert atmosphere is the mixed atmosphere of nitrogen, argon or nitrogen and argon.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108394882A (en) * | 2018-03-08 | 2018-08-14 | 中国检验检疫科学研究院 | A kind of ultralight porous carbon materials and preparation method thereof |
| CN110028051A (en) * | 2019-04-24 | 2019-07-19 | 陕西科技大学 | A method of sodium-ion battery is prepared with porous carbon negative pole material based on sucrose |
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| CN105129797A (en) * | 2015-07-20 | 2015-12-09 | 山东大学 | Preparation method of ammoniation-activation plant activated carbon |
| CN105236405A (en) * | 2015-09-11 | 2016-01-13 | 中国石油大学(华东) | Convenient biomass-based nitrogen-doped active carbon preparation method |
| CN105439143A (en) * | 2014-08-21 | 2016-03-30 | 中国科学院大连化学物理研究所 | Hierarchical porous activated carbon used for a super capacitor and preparation method thereof |
| CN105460918A (en) * | 2015-12-23 | 2016-04-06 | 海安常州大学高新技术研发中心 | Preparation method of hollow carbon sphere |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
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2016
- 2016-07-25 CN CN201610592426.XA patent/CN106219539A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439143A (en) * | 2014-08-21 | 2016-03-30 | 中国科学院大连化学物理研究所 | Hierarchical porous activated carbon used for a super capacitor and preparation method thereof |
| CN105129797A (en) * | 2015-07-20 | 2015-12-09 | 山东大学 | Preparation method of ammoniation-activation plant activated carbon |
| CN105236405A (en) * | 2015-09-11 | 2016-01-13 | 中国石油大学(华东) | Convenient biomass-based nitrogen-doped active carbon preparation method |
| CN105460918A (en) * | 2015-12-23 | 2016-04-06 | 海安常州大学高新技术研发中心 | Preparation method of hollow carbon sphere |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394882A (en) * | 2018-03-08 | 2018-08-14 | 中国检验检疫科学研究院 | A kind of ultralight porous carbon materials and preparation method thereof |
| CN108394882B (en) * | 2018-03-08 | 2021-04-06 | 中国检验检疫科学研究院 | Ultra-light porous carbon material and preparation method thereof |
| CN110028051A (en) * | 2019-04-24 | 2019-07-19 | 陕西科技大学 | A method of sodium-ion battery is prepared with porous carbon negative pole material based on sucrose |
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Application publication date: 20161214 |