CN106115697A - A kind of preparation method of the rich surface activated carbon containing petal-shaped Graphene - Google Patents
A kind of preparation method of the rich surface activated carbon containing petal-shaped Graphene Download PDFInfo
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- CN106115697A CN106115697A CN201610480464.6A CN201610480464A CN106115697A CN 106115697 A CN106115697 A CN 106115697A CN 201610480464 A CN201610480464 A CN 201610480464A CN 106115697 A CN106115697 A CN 106115697A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
Abstract
The invention discloses the preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, MCMB green-ball and KOH are mixed in proportion, add water and a small amount of ethanol fully dissolves, it is dried, carry out high-temperature activation sintering subsequently, clean, sucking filtration, obtain surfaces rich in graphene petal, specific surface 1855m2/ g, pore volume 1.13cm3The absorbent charcoal material of/g.Abundant raw material source of the present invention, synthesis technique is simple, with low cost.The absorbent charcoal material of preparation is beneficial to load nano active granule, contributes to developing multi-functional Carbon Materials, is i.e. used for the fields such as absorption, catalyst carrier, hydrogen storage, ultracapacitor, lithium-sulfur cell.
Description
Technical field
The present invention relates to porous activated carbon technology of preparing, be specifically related to a kind of surface and there is the activated carbon of petal-shaped Graphene
The preparation method of material.
Background technology
MCMB (mesocarbon microbeads is called for short MCMB) is in coal tar pitch, coal tar, oil drip
The liquid crystal shape anisotropy Carbonaceous mesophase spheroid formed in carbonisation blue or green, the condensed-nuclei aromatics compound such as how.Intermediate-phase carbon
There is oriented layer chip architecture, easy graphitization and electric conductivity is good, carbon when there is the self sintering of excellence, high temperature simultaneously inside microsphere
There is the edge of many orientation aromatic hydrocarbons in chemical stability, heat stability, heat conductivity and its surface that after change, charcoal residual value is high, excellent
Group, these features make MCMB be widely used in preparing high-performance liquid chromatography filler, THE ULTRA-HIGH SURFACE AREA ACTIVATED CARBON, lithium
Electrode for secondary battery, catalyst carrier etc..
The structure special based on MCMB and performance characteristics, increasing researcher and manufacturing enterprise begin to focus on
MCMB, and using it as carbon precursor in order to prepare active carbon with high specific surface area material.Researcher finds, MCMB structure and work
Change condition is the principal element affecting active carbon pore structure.MCMB structure mainly have class dimension shape structure, class longitude shape structure and
Class onion-like structure.Document " Fuel Processing Technol., 2010,91,17-24 " reports a kind of KOH activation
The method of MCMB, specifically with the MCMB of three kinds of different structures as presoma, with KOH as activator at 900 DEG C, found that
Irregularly, the multi-layer sheet structure of shape distortion be more beneficial for obtain active carbon with high specific surface area material, its high specific surface area up to
To 2542.8m2/g.The method activation temperature is higher, the spherical activation carbon surface rustic obtained, and with a large amount of oriented layers
Split.Document " Appl.Surf.Sci., 2007,254,506-512 " reports the height ratio using microwave heating method to prepare KOH activation
Surface area and the activated carbon of pore volume, the absorbent charcoal material surface that the method obtains occurs in that substantial amounts of irregularly shaped distribution
Pit, and a few granules bursts apart.
The two dimensional crystal of only one layer of atomic thickness that Graphene is made up of carbon atom, is have now been found that the thinnest, strong
A kind of novel nano-material that degree is maximum, electrical and thermal conductivity performance is the strongest.Relative to Graphene monolayer, (several layers former for Graphene synusia
Sub-thickness) it is more easy to obtain and carried out extensively in fields such as absorption, catalysis and mobile device, Aero-Space, new forms of energy batteries
General basis and applied research.About the preparation method predominantly organic tool stripping method of Graphene synusia, oxidation-reduction method, chemistry gas
Phase sedimentation etc..These preparation methoies are relatively complicated, relatively costly.
Obtained the composite construction of activated carbon and Graphene by special chemical synthesis process, be beneficial to play activated carbon
Double dominant with Graphene performance, it is achieved the multifunction of material.Such as Graphene activation can be obtained excellent performance
Ultracapacitor, and activated carbon/graphene composite structure is expected to be applied to lithium-sulfur cell, medicine carrying, catalyst carrier field etc.
(Small,2011,7,3163-3168；Adv.Mater.,2013,25,2909-2914；Adv.Funct.Mater.,2013,
23,5326-5333.)。
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, its raw material comes
Source is abundant, technique is simple, with low cost；Prepared activated carbon/graphene composite structure has a characteristic that Surface Creation is big
Measuring petal-like Graphene, specific surface area is big.This absorbent charcoal material is beneficial to load nano active granule, contributes to developing multi-functional
Carbon Materials, is i.e. used for the fields such as absorption, catalyst carrier, hydrogen storage, ultracapacitor, lithium-sulfur cell.
For reaching object above, the present invention is to adopt the following technical scheme that:
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) by MCMB powder and lamellar KOH 1:(3-10 in mass ratio) weigh, by load weighted raw material
It is placed in nickel crucible, adds deionized water and make KOH fully dissolve, form solution；
(2) in the solution that step (1) obtains, add ethanol solution again, stir with Glass rod；
(3) solution that step (2) is fully dissolved is placed in thermostatic drying chamber the driest；Obtain MCMB and
KOH mixed-powder；
(4) step (3) is dried the MCMB obtained and KOH mixed-powder carries out high-temperature activation process: will put
The nickel crucible having mixed-powder is placed in tube furnace, is warmed up to the heating rate of 5 DEG C/min from room temperature under argon gas atmosphere
900-1200 DEG C, insulation 1-2h；Then with stove natural cooling；
(5) the powder dilute hydrochloric acid obtained after activation processing is fully cleaned, vacuum filtration, then obtain at freeze-day with constant temperature
The rich surface activated carbon containing petal-shaped Graphene.
Further, described carbonaceous mesophase spherules is the green-ball without high-temperature process, and granularity is 1-40 μm.
Further, described argon gas atmosphere, throughput is 50-100sccm.
Further, the described rich surface activated carbon containing petal-shaped Graphene, specific surface is 409-1855m2/ g, average hole
Footpath is 2nm-4nm.
Further, in step (3), baking temperature is 70-120 DEG C, temperature retention time 24-72h.
Further, in rapid (5), freeze-day with constant temperature is 60 DEG C of dry 24h.
Further, comprise the following steps:
(1) MCMB powder and lamellar KOH analytical pure 1:5 in mass ratio are weighed, by load weighted former
Material is placed in nickel crucible, adds deionized water and makes KOH fully dissolve；Described MCMB powder is without high-temperature process
Green-ball, granularity is 1-40 μm；
(2) in step (1) obtains solution, add ethanol solution, stir with Glass rod, make MCMB powder
End is fully dissolved；
(3) step (2) acquisition solution is placed in thermostatic drying chamber, baking temperature 80 DEG C, temperature retention time 48h, fills
Divide and be dried；
(4) MCMB drying obtained and KOH mixed-powder carry out high-temperature activation process: will be placed with mixed powder
The nickel crucible at end is placed in tube furnace, is warmed up to 1000 DEG C, insulation from room temperature with the heating rate of 5 DEG C/min under argon gas atmosphere
1h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene；The described rich surface activity containing petal-shaped Graphene
Charcoal, outer average pore size 2.55nm of ball, specific surface area 1855m2/g。
Compared with prior art, the invention have the advantage that
1, the present invention uses MCMB to be that carbon source prepares active carbon with high specific surface area, it is advantageous that intermediate-phase carbon
Microsphere is internal exists orientation layer of charcoal, and substantial amounts of functional group is contained on surface, and around surface, the reactivity of carbon atom is high, for various
Modification has high activity.
2, forefathers to activate the activated carbon surface of preparation coarse, only crackle, cavity, little granule.The work obtained of the present invention
Property carbon structure novel, substantial amounts of Graphene petal is contained on its surface.
3, the specific surface of the activated carbon that the present invention obtains is big, can reach 1855m2/ g, substantial amounts of nano-pore is contained on its surface
Hole, aperture is 2-4nm, the load of the most tiny active particle.
4, preparation method of the present invention is simple, low cost, it is easy to industrialized production.
Accompanying drawing explanation
The SEM low power of the activated carbon that Fig. 1 is the embodiment of the present invention 2 (a and b) and example 3 (c and d) obtains and high power photo.
Fig. 2 is activated carbon cross section SEM low power (a) that obtains of the embodiment of the present invention 2 and high power (b) photo.
Fig. 3 is activated carbon TEM (a), HRTEM (b) and the diffraction spot (c) that the embodiment of the present invention 2 obtains.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) MCMB powder (being the green-ball without high-temperature process, granularity is 1-40 μm) and lamellar KOH are divided
Analyse pure 1:8 in mass ratio to weigh, load weighted raw material is placed in nickel crucible, add appropriate amount of deionized water and make KOH abundant
Dissolve；
(2) in above-mentioned solution, add a small amount of ethanol solution, stir with Glass rod, make MCMB complete
Dissolve；The purpose adding a small amount of dehydrated alcohol is to make MCMB be completely dissolved in the solution.
(3) solution of above-mentioned abundant dissolving is placed in thermostatic drying chamber, baking temperature 100 DEG C, temperature retention time 36h；Enter
Row is fully dried；
(4) MCMB and the KOH mixed-powder that drying are obtained carry out high-temperature activation process, will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warmed up to 900 DEG C from room temperature with the heating rate of 5 DEG C/min, protects under argon gas atmosphere
Temperature 1h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene.
The activated carbon that the present embodiment obtains, average pore size 2.15nm, specific surface area 801m2/g。
Embodiment 2
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) MCMB powder (being the green-ball without high-temperature process, granularity is 1-40 μm) and lamellar KOH are divided
Analyse pure 1:5 in mass ratio to weigh, load weighted raw material is placed in nickel crucible, add appropriate amount of deionized water and make KOH abundant
Dissolve；
(2) in above-mentioned solution, add a small amount of ethanol solution, stir with Glass rod, make MCMB complete
Dissolve；
(3) solution of above-mentioned abundant dissolving is placed in thermostatic drying chamber, baking temperature 80 DEG C, temperature retention time 48h；Carry out
Fully it is dried；
(4) MCMB and the KOH mixed-powder that drying are obtained carry out high-temperature activation process, will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warmed up to 1000 DEG C, insulation from room temperature with the heating rate of 5 DEG C/m under argon gas atmosphere
1h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene.
The powder that the present embodiment obtains, outer average pore size 2.55nm of ball, specific surface area 1855m2/g。
It will be seen from figure 1 that spherical MCMB is after high temperature KOH activates, surface occurs in that Graphene petal.
Fig. 2 cross section can be seen that the activated carbon interior solid rich in Graphene petal, and Graphene petal is primarily present in surface.Fig. 3 enters
One step illustrates that existence and the architectural feature of Graphene, i.e. Graphene are polycrystalline form, and general 7-8 layer, structure is intact.
Embodiment 3
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) MCMB powder (being the green-ball without high-temperature process, granularity is 1-40 μm) and lamellar KOH are divided
Analyse pure 1:5 in mass ratio to weigh, load weighted raw material is placed in nickel crucible, add appropriate amount of deionized water and make KOH abundant
Dissolve；
(2) in above-mentioned solution, add a small amount of ethanol solution, stir with Glass rod, make MCMB complete
Dissolve；
(3) solution of above-mentioned abundant dissolving is placed in thermostatic drying chamber, baking temperature 70 DEG C, temperature retention time 72h；Carry out
Fully it is dried；
(4) MCMB and the KOH mixed-powder that drying are obtained carry out high-temperature activation process, will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warmed up to 1100 DEG C, insulation from room temperature with the heating rate of 5 DEG C/m under argon gas atmosphere
1h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene.
The powder that the present embodiment obtains, outer average pore size 3.01nm of ball, specific surface area 409m2/g。
Embodiment 4
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) MCMB powder (being the green-ball without high-temperature process, granularity is 1-40 μm) and lamellar KOH are divided
Analyse pure 1:3 in mass ratio to weigh, load weighted raw material is placed in nickel crucible, add appropriate amount of deionized water and make KOH abundant
Dissolve；
(2) in above-mentioned solution, add a small amount of ethanol solution, stir with Glass rod, make MCMB complete
Dissolve；
(3) solution of above-mentioned abundant dissolving is placed in thermostatic drying chamber, baking temperature 120 DEG C, temperature retention time 24h；Enter
Row is fully dried；
(4) MCMB and the KOH mixed-powder that drying are obtained carry out high-temperature activation process, will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warmed up to 1200 DEG C, insulation from room temperature with the heating rate of 5 DEG C/m under argon gas atmosphere
2h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene.
Embodiment 5
The preparation method of a kind of rich surface activated carbon containing petal-shaped Graphene, comprises the following steps:
(1) MCMB powder (being the green-ball without high-temperature process, granularity is 1-40 μm) and lamellar KOH are divided
Analyse pure 1:10 in mass ratio to weigh, load weighted raw material is placed in nickel crucible, add appropriate amount of deionized water and make KOH abundant
Dissolve；
(2) in above-mentioned solution, add a small amount of ethanol solution, stir with Glass rod, make MCMB complete
Dissolve；
(3) solution of above-mentioned abundant dissolving is placed in thermostatic drying chamber, baking temperature 90 DEG C, temperature retention time 72h；Carry out
Fully it is dried；
(4) MCMB and the KOH mixed-powder that drying are obtained carry out high-temperature activation process, will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warmed up to 900 DEG C, insulation from room temperature with the heating rate of 5 DEG C/m under argon gas atmosphere
2h；
(5) fully being cleaned by the powder dilute hydrochloric acid obtained after activation processing, vacuum filtration, then the constant temperature at 60 DEG C is done
Dry case is dried 24h and obtains the rich surface activated carbon containing petal-shaped Graphene.
Claims (7)
1. the preparation method of the rich surface activated carbon containing petal-shaped Graphene, it is characterised in that comprise the following steps:
(1) by MCMB powder and lamellar KOH 1:(3-10 in mass ratio) weigh, load weighted raw material is placed in
In nickel crucible, add deionized water and make KOH fully dissolve, form solution；
(2) in the solution that step (1) obtains, add ethanol solution again, stir with Glass rod；
(3) solution that step (2) is fully dissolved is placed in thermostatic drying chamber the driest；Obtain MCMB and KOH
Mixed-powder；
(4) step (3) is dried the MCMB obtained and KOH mixed-powder carries out high-temperature activation process: will be placed with mixed
The nickel crucible closing powder is placed in tube furnace, is warmed up to 900-from room temperature with the heating rate of 5 DEG C/min under argon gas atmosphere
1200 DEG C, insulation 1-2h；Then with stove natural cooling；
(5) the powder dilute hydrochloric acid obtained after activation processing is fully cleaned, vacuum filtration, then obtain surface at freeze-day with constant temperature
Activated carbon rich in petal-shaped Graphene.
The preparation method of a kind of rich surface the most as claimed in claim 1 activated carbon containing petal-shaped Graphene, it is characterised in that
Described carbonaceous mesophase spherules is the green-ball without high-temperature process, and granularity is 1-40 μm.
The preparation method of a kind of rich surface the most as claimed in claim 1 activated carbon containing petal-shaped Graphene, it is characterised in that
Described argon gas atmosphere, throughput is 50-100sccm.
The preparation method of the activated carbon of a kind of surfaces rich in graphene petal the most as claimed in claim 1, it is characterised in that institute
Stating the rich surface activated carbon containing petal-shaped Graphene, specific surface is 409-1855m2/ g, average pore size is 2nm-4nm.
The preparation method of the activated carbon of a kind of surfaces rich in graphene petal the most as claimed in claim 1, it is characterised in that step
Suddenly in (3), baking temperature is 70-120 DEG C, temperature retention time 24-72h.
The preparation method of the activated carbon of a kind of surfaces rich in graphene petal the most as claimed in claim 1, it is characterised in that rapid
(5) in, freeze-day with constant temperature is 60 DEG C of dry 24h.
The preparation method of the activated carbon of a kind of surfaces rich in graphene petal the most as claimed in claim 1, it is characterised in that bag
Include following steps:
(1) MCMB powder and lamellar KOH analytical pure 1:5 in mass ratio are weighed, load weighted raw material is put
In nickel crucible, add deionized water and make KOH fully dissolve；Described MCMB powder is the life without high-temperature process
Ball, granularity is 1-40 μm；
(2) in step (1) obtains solution, add ethanol solution, stir with Glass rod, make MCMB powder fill
Divide and dissolve；
(3) step (2) acquisition solution is placed in thermostatic drying chamber, baking temperature 80 DEG C, temperature retention time 48h, fully does
Dry；
(4) MCMB drying obtained and KOH mixed-powder carry out high-temperature activation process: will be placed with mixed-powder
Nickel crucible is placed in tube furnace, is warmed up to 1000 DEG C, insulation 1h from room temperature with the heating rate of 5 DEG C/min under argon gas atmosphere；
(5) the powder dilute hydrochloric acid obtained after activation processing is fully cleaned, vacuum filtration, then at the thermostatic drying chamber of 60 DEG C
In be dried 24h and obtain rich surface containing the activated carbon of petal-shaped Graphene；The described rich surface activated carbon containing petal-shaped Graphene, ball
Outer average pore size 2.55nm, specific surface area 1855m2/g。
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| CN109809385A (en) * | 2019-01-25 | 2019-05-28 | 安徽益佳通电池有限公司 | A kind of lithium ion battery negative material of height ratio capacity and preparation method thereof |
| CN110669314A (en) * | 2019-09-30 | 2020-01-10 | 西安交通大学 | High-dispersion graphene resin-based composite material and preparation method and application thereof |
| CN112038635A (en) * | 2020-08-04 | 2020-12-04 | 湘潭大学 | Lithium-sulfur battery graphene-loaded cementite particle composite positive electrode material and preparation method thereof |
| CN112758916A (en) * | 2020-12-25 | 2021-05-07 | 西安交通大学 | Active graphene and method for preparing active graphene through mesophase pitch |
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