CN106115697B - A kind of preparation method of active carbon of the surface rich in petal-shaped graphene - Google Patents
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene Download PDFInfo
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Abstract
A kind of preparation method of active carbon the invention discloses surface rich in petal-shaped graphene, mesocarbon microspheres green-ball and KOH are mixed in proportion, water and a small amount of ethyl alcohol is added sufficiently to dissolve, it is dry, high-temperature activation sintering is then carried out, is cleaned, is filtered, obtain surfaces rich in graphene petal, specific surface 1855m2/ g, pore volume 1.13cm3The absorbent charcoal material of/g.Raw material sources of the present invention are abundant, and synthesis technology is simple, low in cost.The absorbent charcoal material of preparation is conducive to load nano active particle, helps to develop multi-functional Carbon Materials, that is, is used for the fields such as absorption, catalyst carrier, hydrogen storage, supercapacitor, lithium-sulfur cell.
Description
Technical field
The present invention relates to porous activated carbon technologies of preparing, and in particular to there are the active carbons of petal-shaped graphene for a kind of surface
The preparation method of material.
Background technique
Mesocarbon microspheres (mesocarbon microbeads, abbreviation MCMB) is in coal tar pitch, coal tar, petroleum drip
It is green, how etc. the liquid crystal shape anisotropy Carbonaceous mesophase sphere that is formed in the carbonisation of condensed-nuclei aromatics compound.Intermediate-phase carbon
Easily graphitization and electric conductivity be good when having orientation multi-layer sheet structure inside microballoon, while having an excellent self sintering, high temperature, carbon
There are the edges of many orientation aromatic hydrocarbons for charcoal residual value height, excellent chemical stability, thermal stability, thermal conductivity and its surface after change
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..
Based on MCMB special structure and performance characteristics, more and more researchers and manufacturing enterprise are begun to focus on
MCMB, and using it as carbon precursor to prepare active carbon with high specific surface area material.Researcher's discovery, MCMB structure and work
Change condition is to influence the principal element of active carbon pore structure.MCMB structure mainly have class dimension shape structure, class longitude shape structure and
Class onion-like structure." Fuel Processing Technol., 2010,91,17-24 " report a kind of KOH activation to document
The method of MCMB, specifically using the MCMB of three kinds of different structures as presoma, using KOH as activator at 900 DEG C, as a result, it has been found that
Irregularly, the multi-layer sheet structure of shape distortion, which is more advantageous to, obtains active carbon with high specific surface area material, and maximum specific surface area is reachable
To 2542.8m2/g.This method activation temperature is higher, obtained spherical activated carbon coarse surface structure, and with a large amount of oriented layers
It splits." Appl.Surf.Sci., 2007,254,506-512 " report the high ratio that KOH activation is prepared using microwave heating method to document
There is a large amount of irregular shape distribution in the active carbon of surface area and pore volume, the absorbent charcoal material surface that this method obtains
Pit, and a few granules are burst apart.
The two dimensional crystal for only one layer of atomic thickness that graphene is made of carbon atom, is presently found most thin, strong
Degree maximum, a kind of strongest novel nano-material of electrical and thermal conductivity performance.Relative to graphene single layer, graphene synusia (several layers of original
Sub- thickness) it is easier to obtain and carried out extensively in the fields such as absorption, catalysis and mobile device, aerospace, new energy battery
General basis and application study.Preparation method in relation to graphene synusia mainly has mechanical stripping method, oxidation-reduction method, chemical gas
Phase sedimentation etc..These preparation methods are relatively complicated, higher cost.
The composite construction that active carbon and graphene are obtained by special chemical synthesis process is beneficial to play active carbon
With the double dominant of graphene performance, the multifunction of material is realized.Such as graphene is activated into available have excellent performance
Supercapacitor, and active carbon/graphene composite structure is expected to be applied to lithium-sulfur cell, carry medicine, 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
A kind of preparation method of active carbon the object of the present invention is to provide surface rich in petal-shaped graphene, raw material come
Source is abundant, simple process, low in cost；Prepared active carbon/graphene composite structure has a characteristic that Surface Creation is big
Measure petal-like graphene, large specific surface area.The absorbent charcoal material is conducive to load nano active particle, helps to develop multi-functional
Carbon Materials are used for the fields such as absorption, catalyst carrier, hydrogen storage, supercapacitor, lithium-sulfur cell.
To achieve the above objectives, the present invention is to adopt the following technical scheme that:
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder and sheet KOH 1:(3-10 in mass ratio) it weighs, by load weighted raw material
It is placed in nickel crucible, deionized water, which is added, dissolves KOH sufficiently, forms solution；
(2) add ethanol solution again in the solution that step (1) obtains, stirred with glass bar；
(3) solution that step (2) sufficiently dissolves is placed in thermostatic drying chamber sufficiently dry；Obtain mesocarbon microspheres and
KOH mixed-powder；
(4) mesocarbon microspheres and KOH mixed-powder that step (3) drying obtains are subjected to high-temperature activation processing: will put
There is the nickel crucible of mixed-powder to be placed in tube furnace, is warming up under argon atmosphere from room temperature with the heating rate of 5 DEG C/min
900-1200 DEG C, heat preservation 1-2h；Then with furnace natural cooling；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, is then obtained in freeze-day with constant temperature
Surface is rich in the active carbon of petal-shaped graphene.
Further, the carbonaceous mesophase spherules are the green-ball without high-temperature process, and granularity is 1-40 μm.
Further, the argon atmosphere, throughput 50-100sccm.
Further, the surface is rich in the active carbon of petal-shaped graphene, specific surface 409-1855m2/ g, average hole
Diameter is 2nm-4nm.
Further, drying temperature is 70-120 DEG C in step (3), soaking time 24-72h.
Further, freeze-day with constant temperature is dried for 24 hours in rapid (5) for 60 DEG C.
Further, comprising the following steps:
(1) mesocarbon microspheres powder and sheet KOH are analyzed pure 1:5 in mass ratio to weigh, by load weighted original
Material is placed in nickel crucible, and deionized water, which is added, dissolves KOH sufficiently；The mesocarbon microspheres powder is without high-temperature process
Green-ball, granularity be 1-40 μm；
(2) it is obtained in solution in step (1) and ethanol solution is added, stirred with glass bar, make mesocarbon microspheres powder
Last sufficiently dissolution；
(3) step (2) acquisition solution is placed in thermostatic drying chamber, 80 DEG C of drying temperature, soaking time 48h is filled
Divide drying；
(4) mesocarbon microspheres and KOH mixed-powder that drying obtains are subjected to high-temperature activation processing: mixed powder will be placed with
The nickel crucible at end is placed in tube furnace, is warming up to 1000 DEG C, heat preservation from room temperature with the heating rate of 5 DEG C/min under argon atmosphere
1h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case；The surface is rich in the activity of petal-shaped graphene
Charcoal, the outer average pore size 2.55nm, specific surface area 1855m of ball2/g。
Compared with prior art, the invention has the advantages that
1, the present invention uses mesocarbon microspheres to prepare active carbon with high specific surface area for carbon source, it is advantageous that intermediate-phase carbon
There is orientation layer of charcoal inside microballoon, a large amount of functional group is contained on surface, and the reactivity of carbon atom is high around surface, for various
It is modified that there is high activity.
2, the activated carbon surface of forefathers' activation preparation is coarse, only crackle, cavity, little particle.Obtained work of the invention
Property carbon structure it is novel, a large amount of graphene petal is contained on surface.
3, the specific surface for the active carbon that the present invention obtains is big, can reach 1855m2A large amount of nano-pore is contained on/g, surface
Hole, aperture 2-4nm are conducive to the load of tiny active particle.
4, preparation method of the present invention is simple, at low cost, easy to industrialized production.
Detailed description of the invention
Fig. 1 is the SEM low power and high power photo for the active carbon that the embodiment of the present invention 2 (a and b) and example 3 (c and d) obtain.
Fig. 2 is the active carbon section SEM low power (a) and high power (b) photo that the embodiment of the present invention 2 obtains.
Fig. 3 is active carbon TEM (a), HRTEM (b) and the diffraction spot (c) that the embodiment of the present invention 2 obtains.
Specific embodiment
Embodiment 1
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder (for without the green-ball of high-temperature process, granularity is 1-40 μm) and sheet KOH points
It analyses pure 1:8 in mass ratio to be weighed, load weighted raw material is placed in nickel crucible, appropriate amount of deionized water, which is added, keeps KOH abundant
Dissolution；
(2) a small amount of ethanol solution is added in the above solution, is stirred with glass bar, keeps mesocarbon microspheres complete
Dissolution；The purpose that a small amount of dehydrated alcohol is added is to be completely dissolved mesocarbon microspheres in the solution.
(3) the above-mentioned solution sufficiently dissolved is placed in thermostatic drying chamber, 100 DEG C of drying temperature, soaking time 36h；Into
Row is sufficiently dry；
(4) mesocarbon microspheres and KOH mixed-powder obtained drying carries out high-temperature activation processing, i.e., will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warming up to 900 DEG C from room temperature with the heating rate of 5 DEG C/min under argon atmosphere, is protected
Warm 1h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case.
The active carbon that the present embodiment obtains, average pore size 2.15nm, specific surface area 801m2/g。
Embodiment 2
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder (for without the green-ball of high-temperature process, granularity is 1-40 μm) and sheet KOH points
It analyses pure 1:5 in mass ratio to be weighed, load weighted raw material is placed in nickel crucible, appropriate amount of deionized water, which is added, keeps KOH abundant
Dissolution；
(2) a small amount of ethanol solution is added in the above solution, is stirred with glass bar, keeps mesocarbon microspheres complete
Dissolution；
(3) the above-mentioned solution sufficiently dissolved is placed in thermostatic drying chamber, 80 DEG C of drying temperature, soaking time 48h；It carries out
It is sufficiently dry；
(4) mesocarbon microspheres and KOH mixed-powder obtained drying carries out high-temperature activation processing, i.e., will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warming up to 1000 DEG C, heat preservation from room temperature with the heating rate of 5 DEG C/m under argon atmosphere
1h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case.
The powder that the present embodiment obtains, the outer average pore size 2.55nm, specific surface area 1855m of ball2/g。
It will be seen from figure 1 that spherical mesocarbon microspheres is after high temperature KOH activation, there is graphene petal in surface.
The section Fig. 2 can be seen that the active carbon inside solid rich in graphene petal, and graphene petal is primarily present in surface.Fig. 3 into
One step illustrates the presence and structure feature of graphene, i.e. graphene is polycrystalline form, and 7-8 layers general, structure is intact.
Embodiment 3
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder (for without the green-ball of high-temperature process, granularity is 1-40 μm) and sheet KOH points
It analyses pure 1:5 in mass ratio to be weighed, load weighted raw material is placed in nickel crucible, appropriate amount of deionized water, which is added, keeps KOH abundant
Dissolution；
(2) a small amount of ethanol solution is added in the above solution, is stirred with glass bar, keeps mesocarbon microspheres complete
Dissolution；
(3) the above-mentioned solution sufficiently dissolved is placed in thermostatic drying chamber, 70 DEG C of drying temperature, soaking time 72h；It carries out
It is sufficiently dry；
(4) mesocarbon microspheres and KOH mixed-powder obtained drying carries out high-temperature activation processing, i.e., will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warming up to 1100 DEG C, heat preservation from room temperature with the heating rate of 5 DEG C/m under argon atmosphere
1h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case.
The powder that the present embodiment obtains, the outer average pore size 3.01nm, specific surface area 409m of ball2/g。
Embodiment 4
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder (for without the green-ball of high-temperature process, granularity is 1-40 μm) and sheet KOH points
It analyses pure 1:3 in mass ratio to be weighed, load weighted raw material is placed in nickel crucible, appropriate amount of deionized water, which is added, keeps KOH abundant
Dissolution；
(2) a small amount of ethanol solution is added in the above solution, is stirred with glass bar, keeps mesocarbon microspheres complete
Dissolution；
(3) the above-mentioned solution sufficiently dissolved is placed in thermostatic drying chamber, 120 DEG C of drying temperature, soaking time is for 24 hours；Into
Row is sufficiently dry；
(4) mesocarbon microspheres and KOH mixed-powder obtained drying carries out high-temperature activation processing, i.e., will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warming up to 1200 DEG C, heat preservation from room temperature with the heating rate of 5 DEG C/m under argon atmosphere
2h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case.
Embodiment 5
A kind of preparation method of active carbon of the surface rich in petal-shaped graphene, comprising the following steps:
(1) by mesocarbon microspheres powder (for without the green-ball of high-temperature process, granularity is 1-40 μm) and sheet KOH points
It analyses pure 1:10 in mass ratio to be weighed, load weighted raw material is placed in nickel crucible, appropriate amount of deionized water, which is added, keeps KOH abundant
Dissolution；
(2) a small amount of ethanol solution is added in the above solution, is stirred with glass bar, keeps mesocarbon microspheres complete
Dissolution；
(3) the above-mentioned solution sufficiently dissolved is placed in thermostatic drying chamber, 90 DEG C of drying temperature, soaking time 72h；It carries out
It is sufficiently dry；
(4) mesocarbon microspheres and KOH mixed-powder obtained drying carries out high-temperature activation processing, i.e., will be placed with mixing
The nickel crucible of powder is placed in tube furnace, is warming up to 900 DEG C, heat preservation from room temperature with the heating rate of 5 DEG C/m under argon atmosphere
2h；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then the constant temperature at 60 DEG C is dry
The dry active carbon for obtaining surface for 24 hours and being rich in petal-shaped graphene in dry case.
Claims (5)
1. a kind of preparation method of active carbon of surface rich in petal-shaped graphene, which comprises the following steps:
(1) by mesocarbon microspheres powder and sheet KOH 1:(3-10 in mass ratio) it weighs, load weighted raw material is placed in
In nickel crucible, deionized water, which is added, dissolves KOH sufficiently, forms solution；
(2) add ethanol solution again in the solution that step (1) obtains, stirred with glass bar；
(3) solution that step (2) sufficiently dissolves is placed in thermostatic drying chamber sufficiently dry；Obtain mesocarbon microspheres and KOH
Mixed-powder；
(4) mesocarbon microspheres and KOH mixed-powder that step (3) drying obtains are subjected to high-temperature activation processing: mixed by being placed with
The nickel crucible for closing powder is placed in tube furnace, is warming up to 1000- from room temperature with the heating rate of 5 DEG C/min under argon atmosphere
1200 DEG C, heat preservation 1-2h；Then with furnace natural cooling；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then freeze-day with constant temperature obtains surface again
Active carbon rich in petal-shaped graphene；
The carbonaceous mesophase spherules are the green-ball without high-temperature process, and granularity is 1-40 μm；
The surface is rich in the active carbon of petal-shaped graphene, specific surface 409-1855m2/ g, average pore size 2nm-4nm.
2. a kind of preparation method of active carbon of the surface rich in petal-shaped graphene as described in claim 1, which is characterized in that
The argon atmosphere, throughput 50-100sccm.
3. a kind of preparation method of the active carbon of surfaces rich in graphene petal as described in claim 1, which is characterized in that step
Suddenly drying temperature is 70-120 DEG C in (3), soaking time 24-72h.
4. a kind of preparation method of the active carbon of surfaces rich in graphene petal as described in claim 1, which is characterized in that step
Suddenly freeze-day with constant temperature is dried for 24 hours in (5) for 60 DEG C.
5. a kind of preparation method of the active carbon of surfaces rich in graphene petal as described in claim 1, which is characterized in that packet
Include following steps:
(1) mesocarbon microspheres powder and sheet KOH are analyzed pure 1:5 in mass ratio to weigh, load weighted raw material is set
In nickel crucible, deionized water, which is added, dissolves KOH sufficiently；The mesocarbon microspheres powder is the life without high-temperature process
Ball, granularity are 1-40 μm；
(2) it is obtained in solution in step (1) and ethanol solution is added, stirred with glass bar, fill mesocarbon microspheres powder
Divide dissolution；
(3) step (2) acquisition solution is placed in thermostatic drying chamber, 80 DEG C of drying temperature, soaking time 48h, is carried out sufficiently dry
It is dry；
(4) mesocarbon microspheres and KOH mixed-powder that drying obtains are subjected to high-temperature activation processing: mixed-powder will be placed with
Nickel crucible is placed in tube furnace, is warming up to 1000 DEG C, heat preservation 1h from room temperature with the heating rate of 5 DEG C/min under argon atmosphere；
(5) powder obtained after activation processing is sufficiently cleaned with dilute hydrochloric acid, is filtered by vacuum, then in 60 DEG C of thermostatic drying chamber
Middle drying obtains the active carbon that surface is rich in petal-shaped graphene for 24 hours；The surface is rich in the active carbon of petal-shaped graphene, ball
Outer average pore size 2.55nm, specific surface area 1855m2/g。
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| CN109179376A (en) * | 2018-08-28 | 2019-01-11 | 扬州大学 | The method that latex foam prepares porous carbon nanomaterial |
| 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 |
| CN110669314B (en) * | 2019-09-30 | 2020-11-10 | 西安交通大学 | High-dispersion graphene resin-based composite material and preparation method and application thereof |
| CN112038635B (en) * | 2020-08-04 | 2021-12-28 | 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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