CN106315568A - Preparation method of graphene and graphene - Google Patents
Preparation method of graphene and graphene Download PDFInfo
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- CN106315568A CN106315568A CN201610706925.7A CN201610706925A CN106315568A CN 106315568 A CN106315568 A CN 106315568A CN 201610706925 A CN201610706925 A CN 201610706925A CN 106315568 A CN106315568 A CN 106315568A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention relates to a preparation method of graphene. The method comprises the following steps: (1) pretreating a biomass material to obtain a pretreated biomass material, wherein the biomass material comprises one or more of straws, rice hulls, peanut shells and bark; (2) mixing a metal catalyst with the pretreated biomass in the step (1), and carrying to obtain a catalyst-carried biomass material; (3) mixing a foaming agent with the catalyst-carried biomass material obtained in the step (2), and coating on a deposition component in a chemical vapor deposition reactor; and (4) introducing protective gas into the chemical vapor deposition reactor in the step (3), and keeping the temperature at 600-1000 DEG C for 5-20 hours to obtain the graphene. Compared with the prior art, the preparation method provided by the invention has the advantages of no environment pollution and low cost due to the use of the biomass material as the carbon source, and can easily implement industrial production of graphene.
Description
Technical field
The invention belongs to material with carbon element technical field, particularly relate to preparation method and the Graphene of a kind of Graphene.
Background technology
2004, the method that two scientists of Univ Manchester UK use micromechanics to peel off was found that Graphene,
And obtained Nobel Prize in physics in 2010.Graphene is a kind of single atomic thickness and the carbon atom with sp2 bond
Slab construction, in theory, there is perfect galvanized hexagonal wire mesh columnar structure, present excellence electronic stability, heat conductivity, optical property, power
Learn performance etc..After Graphene is found, owing to performance and the huge market application foreground of its excellence have caused physics
Research boom with fields such as material science.Graphene be at present the thinnest be also the hardest nano material, be provided simultaneously with printing opacity
The performance that numerous common materials do not possess such as property is good, heat conductivity is high, electron mobility is high, resistivity is low, mechanical strength is high, not
It is expected at numerous necks such as electrode, battery, transistor, touch screen, solar energy, sensor, super light material, medical treatment, desalinizations
Territory is extensively applied, and is one of the most promising advanced material.But, there is presently no effective method can volume production high-quality graphite
Alkene.
In order to allow outstanding grapheme material realize industrialized production and application, being necessary for developing one can give birth on a large scale
Produce and the number of plies and the controlled preparation method of size.The preparation method of Graphene has mechanical stripping method, epitaxial growth method, oxidation at present
Reducing process, ultrasonic stripping method, organic synthesis method, solvent-thermal method etc..In these methods, mechanical stripping method and epitaxial growth legal system
Standby efficiency is the lowest, it is difficult to meet large-scale needs.Oxidation-reduction method prepares the with low cost and easy of grapheme material powder body
Realize, but substantial amounts of waste liquid can be produced, environment is caused severe contamination, limits the extensive industrialized development of Graphene.
These methods are all using graphite ore as former material, and this mineral resources are not recyclable regeneratives, are unfavorable for the big rule of Graphene
Mould produces.
Biological material is a kind of natural reproducible resource, and environmentally safe has high in modern chemical industry
Potential using value, its yield is huge, but application market is the most wide, and chemically component analysis can be seen that, in biological material
Phosphorus content be about 60%, in terms of preparing material with carbon element, have huge prospect.
China Patent Publication No. 103466613A discloses a kind of method preparing Graphene for raw material with lignin.The party
First method will be equipped with the porcelain example boat of lignin and catalyst and puts in hinge tube furnace, is at the uniform velocity passed through inert protective gas,
In stove, with constant heating rate, sample is heated to target temperature from room temperature simultaneously, and keeps under target temperature, treat sample
When product temperature is down to room temperature, sample is taken out, after deionized water wash, vacuum filtration, oven drying at low temperature, obtains Graphene.This
The preparation technology of invention is easy, and gained quality of graphene is excellent, and productivity is considerable.But, the method uses anaerobic sintering, sintering
Temperature reaches 1500 DEG C, high to equipment requirements, and equipment preparation cost improves, it is impossible to be applied to large-scale production.
China Patent Publication No. 103935986A discloses a kind of side preparing Graphene with biological carbon source material high yield
Method, comprises the steps: that biological carbon source material joins in acid solution after microwaved, then through washing, dried, obtains pre-
The biological carbon source material processed；The biological carbon source material of pretreatment is mixed with catalyst, 600-1600 DEG C, protective gas deposits
At lower calcining 1-12h, after cooling, obtain described Graphene.The method significantly reduces production cost, it is achieved that Graphene
Large-scale industrial production.But, the method uses and has arrived some noble metal catalysts, not only cost improves, preparation
Graphene area is little, and it is poor to crystallize, and is unfavorable for the industrialized development of Graphene.
According to above-mentioned, obtain Graphene although grinding the most repeatedly, but owing to being answered by grinding pressure
The effect of power, grinds to clash into and graphite lattice is caused certain destruction, owing to grinding, graphite is applied pressure, to the graphite peeled off
Producing huge impulsive force, this impulsive force can make graphene layer produce fault of construction, easily causes graphene layer structural lattice
Defect, reduces the size of Graphene after peeling off so that prepared graphene product crystalline size is little, it is difficult to obtain large-size high-quality
Amount Graphene, either mechanical type ball milling or mechanical type Gas grinding, be all to sacrifice Graphene size and lattice is complete
Whole property；It addition, the crunch of abrasive media can cause graphite linings structure to become more closely and peeling effect can be caused on the contrary to drop
Low, cause milling time length, cost the highest；Furthermore, grind production Graphene at present and belong to batch (-type), graphite is being carried out
While stripping, the Graphene peeled off cannot be filtered out in time, thus be difficult to the volume production of continuous-stable, and easily
Pollute environment, it is difficult to realize Graphene industrialized production.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of Graphene, and the present invention is with biological material
Raw material, its wide material sources, renewable, environmentally safe, low cost, can be easily achieved the industrialized production of Graphene.
The technical scheme is that
The preparation method of a kind of Graphene, comprises the following steps:
(1) biological material being carried out pretreatment, obtain the biological material of pretreatment, described biological material includes straw
One or more in stalk, rice husk, Pericarppium arachidis hypogaeae, bark；
(2) preprocessing biomass in metallic catalyst and described step (1) is mixed, load, be loaded with
The biological material of catalyst；
(3) biological material being loaded with catalyst that foaming agent obtains with described step (2) is mixed, and being coated on
Learn in the means of deposition in gas-phase deposition reactor；
(4) CVD reactor in described step (3) is passed through protective gas, at 600-1000 DEG C
Insulation 5-20h, obtains Graphene.
Compared with prior art, the invention has the beneficial effects as follows:
The preparation method that the present invention provides does not uses strong acid, environmentally safe, and the present invention is with biological material
For carbon source, the cost of raw material of carbon source is low and is readily available, and solves the problem that cost is high, it is achieved that Graphene industrialized production,
The present invention carries out pretreatment to biomass, on the one hand can remove in biological material the impurity such as cell wall, retain in biomass
Pectin, hemicellulose, cellulose；On the other hand reduce the polyphosphazene polymer in biological material right, make biomass in catalysis
Under agent effect, it is more easy to catalysis, biomass generation catalytic pyrolysis the most in the reactor, make biological material be easier to obtain thickness
For 0.3-5nm；Radial dimension is the Graphene of 10-20 μm.
On the basis of technique scheme, the present invention can also do following improvement.
Preferably, described step (1) specifically includes following steps:
After biomass cleaning, screening, it is crushed to 50-300 mesh, then through aqueous slkali soaking 5-10min, filters, be dried
Obtain the biological material of pretreatment.
Preferably, one or more during described aqueous slkali is sodium hydroxide, potassium hydroxide, calcium hydroxide.
Preferably, during described metallic catalyst includes cesium salt, aluminum isopropylate., manganese dioxide, antimony oxide, Cu-lyt.
One or more.
Preferably, the metallic catalyst in described step (2) with the mass ratio of the biological material in described step (1) is
(0.01-30): 1.
Preferably, described foaming agent include azodicarbonamide, 4,4 '-OBSH, unifor, 4,
One or more in 4 '-disulfonyl hydrazide, dinitrosopentamethylene tetramine.
Preferably, described foaming agent is (1-10) with the mass ratio of the biological material in described step (1): 1.
Preferably, described step (4) specifically includes following steps:
In CVD reactor, the rate of pressurization with 0.1-0.6Mpa/s is pressurized to 20-40Mpa, with 5-20
DEG C/heating rate of min is warming up to 600-1000 DEG C.
The present invention provides a kind of Graphene, prepares according to the preparation method described in technique scheme；
The thickness of described Graphene is 0.3-5nm；
The radial dimension of described Graphene is 10-20 μm.
The present invention provides the preparation method of a kind of Graphene, comprises the following steps: biological material is carried out pre-place by (1)
Reason, obtains the biological material of pretreatment, and described biological material includes the one in straw, rice husk, Pericarppium arachidis hypogaeae, bark or several
Kind；(2) preprocessing biomass in metallic catalyst and described step (1) is mixed, load, obtain being loaded with catalyst
Biological material；(3) biological material being loaded with catalyst that foaming agent obtains with described step (2) is mixed, and be coated with
It is overlying in the means of deposition in CVD reactor.(4) in the CVD reactor in described step (3)
It is passed through protective gas, at 600-1000 DEG C, is incubated 5-20h, obtains Graphene.
The present invention prepares Graphene and prepares Graphene synopsis with prior art
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
(1) in parts by weight, after 1 part of straw cleaning, screening, it is crushed to 50 mesh, then through soaking with sodium hydroxide 5min,
Filter, be dried to obtain the stalk material of pretreatment；
(2) in parts by weight, the pretreated straw in 0.01 part of cesium salt and described step (1) is mixed, loads,
To the stalk material being loaded with cesium salt；
(3) the straw material being loaded with cesium salt in parts by weight, 1 part of azodicarbonamide and described step (2) obtained
Material mixing, and be coated in the means of deposition in CVD reactor；
(4) CVD reactor in described step (3) is passed through protective gas, deposits in chemical gaseous phase
In reactor, the rate of pressurization with 0.1Mpa/s is pressurized to 20Mpa, is warming up to 600 DEG C with the heating rate of 5 DEG C/min, insulation
5h, obtains Graphene.
Graphite stripping formation thickness is at 0.3-5nm, and radial dimension is the large scale area graphite alkene of 10-20 μm.
Embodiment 2
(1) in parts by weight, after 10 parts of Pericarppium arachidis hypogaeaes cleanings, screenings, it is crushed to 200 mesh, then soaks through calcium hydroxide
10min, filters, is dried to obtain the Pericarppium arachidis hypogaeae material of pretreatment；
(2) in parts by weight, the pretreatment Pericarppium arachidis hypogaeae in 1 part of manganese dioxide and described step (1) is mixed, bears
Carry, obtain being loaded with the Pericarppium arachidis hypogaeae material of manganese dioxide；
(3) flower being loaded with manganese dioxide in parts by weight, 5 parts of unifor and described step (2) obtained
Raw shell material mixing, and be coated in the means of deposition in CVD reactor；
(4) CVD reactor in described step (3) is passed through protective gas, deposits in chemical gaseous phase
In reactor, the rate of pressurization with 0.3Mpa/s is pressurized to 30Mpa, is warming up to 800 DEG C with the heating rate of 10 DEG C/min, insulation
10h, obtains Graphene.
Graphite stripping formation thickness is at 0.3-5nm, and radial dimension is the large scale area graphite alkene of 10-20 μm.
Embodiment 3
(1) in parts by weight, after 100 parts of barks cleanings, screenings, it is crushed to 300 mesh, then soaks through calcium hydroxide
10min, filters, is dried to obtain the tree bark materials of pretreatment；
(2) in parts by weight, the pretreatment bark in 10 parts of Cu-lyt .s and described step (1) is mixed, loads,
Obtain being loaded with the tree bark materials of Cu-lyt.；
(3) in parts by weight, it is loaded with chlorine by what 100 parts of dinitrosopentamethylene tetramines and described step (2) obtained
Change cuprous tree bark materials mixing, and be coated in the means of deposition in CVD reactor；
(4) CVD reactor in described step (3) is passed through protective gas, deposits in chemical gaseous phase
In reactor, the rate of pressurization with 0.6Mpa/s is pressurized to 40Mpa, is warming up to 1000 DEG C with the heating rate of 20 DEG C/min, insulation
20h, obtains Graphene.
Graphite stripping formation thickness is at 0.3-5nm, and radial dimension is the large scale area graphite alkene of 10-20 μm.
Comparative example 1
(1) in parts by weight, after 50 parts of rice husks cleanings, screenings, it is crushed to 10 mesh, then soaks through calcium hydroxide
1min, filters, is dried to obtain the rice hull material of pretreatment；
(2) in parts by weight, the pretreatment rice husk in 5 parts of antimony oxides and described step (1) is mixed, bears
Carry, obtain being loaded with the rice hull material of antimony oxide；
(3) in parts by weight, by 100 part 4, what 4 '-OBSH and described step (2) obtained is loaded with three oxygen
Change the rice hull material mixing of two antimony, and be coated in the means of deposition in CVD reactor；
(4) CVD reactor in described step (3) is passed through protective gas, deposits in chemical gaseous phase
In reactor, the rate of pressurization with 0.01Mpa/s is pressurized to 10Mpa, is warming up to 300 DEG C with the heating rate of 2 DEG C/min, insulation
1h, obtains Graphene.
Graphite stripping formation thickness is at 20-50nm, and radial dimension is the large scale area graphite alkene of 1-5 μm.
Comparative example 2
(1) in parts by weight, after 30 parts of straws cleanings, screenings, it is crushed to 400 mesh, then soaks through potassium hydroxide
20min, filters, is dried to obtain the stalk material of pretreatment；
(2) in parts by weight, the pretreated straw in 3 parts of aluminum isopropylate. and described step (1) is mixed, loads,
Obtain being loaded with the stalk material of aluminum isopropylate.；
(3) straw being loaded with aluminum isopropylate. in parts by weight, 60 parts of unifor and described step (2) obtained
Stalk material mixing, and be coated in the means of deposition in CVD reactor；
(4) CVD reactor in described step (3) is passed through protective gas, deposits in chemical gaseous phase
In reactor, the rate of pressurization with 2Mpa/s is pressurized to 60Mpa, is warming up to 2000 DEG C with the heating rate of 50 DEG C/min, insulation
30h, obtains Graphene.
Graphite stripping formation thickness is at 20-50nm, and radial dimension is the large scale area graphite alkene of 1-5 μm.
By above example with comparative example it can be seen that the preparation method of present invention offer is with biological material as carbon
Source, prepares Graphene, and not only biomass source is extensive, and low cost, renewable, environmentally safe, beneficially graphite
Alkene industrialized production, and the Graphene thickness obtained is low, the biggest so as to get the application of Graphene wider.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (9)
1. the preparation method of a Graphene, it is characterised in that comprise the following steps:
(1) biological material is carried out pretreatment, obtains the biological material of pretreatment, described biological material include straw,
One or more in rice husk, Pericarppium arachidis hypogaeae, bark；
(2) preprocessing biomass in metallic catalyst and described step (1) is mixed, load, obtain being loaded with catalysis
The biological material of agent；
(3) biological material being loaded with catalyst that foaming agent obtains with described step (2) is mixed, and be coated on chemistry gas
In means of deposition in phase deposition reactor；
(4) CVD reactor in described step (3) is passed through protective gas, is incubated at 600-1000 DEG C
5-20h, obtains Graphene.
Preparation method the most according to claim 1, it is characterised in that described step (1) specifically includes following steps:
After biomass cleaning, screening, it is crushed to 50-300 mesh, then through aqueous slkali soaking 5-10min, filters, be dried to obtain
The biological material of pretreatment.
Preparation method the most according to claim 2, it is characterised in that described aqueous slkali is sodium hydroxide, potassium hydroxide, hydrogen
One or more in calcium oxide.
Preparation method the most according to claim 1, it is characterised in that described metallic catalyst include cesium salt, aluminum isopropylate.,
One or more in manganese dioxide, antimony oxide, Cu-lyt..
Preparation method the most according to claim 1, it is characterised in that the metallic catalyst in described step (2) is with described
The mass ratio of the biological material in step (1) is (0.01-30): 1.
Preparation method the most according to claim 1, it is characterised in that described foaming agent include azodicarbonamide, 4,4 '-
One or more in OBSH, unifor, 4,4 '-disulfonyl hydrazide, dinitrosopentamethylene tetramine.
Preparation method the most according to claim 1, it is characterised in that described foaming agent and the biology in described step (1)
The mass ratio of material is (1-10): 1.
Preparation method the most according to claim 1, it is characterised in that described step (4) specifically includes following steps:
In CVD reactor, the rate of pressurization with 0.1-0.6Mpa/s is pressurized to 20-40Mpa, with 5-20 DEG C/min
Heating rate be warming up to 600-1000 DEG C.
9. a Graphene, it is characterised in that prepare according to the preparation method described in claim 1-8 any one；
The thickness of described Graphene is 0.3-5nm；
The radial dimension of described Graphene is 10-20 μm.
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| CN109809749A (en) * | 2019-04-02 | 2019-05-28 | 四川聚创石墨烯科技有限公司 | A kind of construction method of graphite alkenes cement-base composite material |
| CN110357077A (en) * | 2019-07-23 | 2019-10-22 | 路英军 | A kind of biomass graphene preparation method |
| CN110395720A (en) * | 2019-09-03 | 2019-11-01 | 王志朋 | The method for preparing vertical graphene film as raw material using biomass |
| CN112299768A (en) * | 2020-11-13 | 2021-02-02 | 西安建筑科技大学 | Graphene functionalized cement-based material and preparation method thereof |
| CN116060002A (en) * | 2023-02-24 | 2023-05-05 | 中国科学院生态环境研究中心 | Graphene-loaded metal monoatomic composite material, preparation method and application |
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| GB2612290A (en) * | 2021-09-01 | 2023-05-03 | Grown Graphene Ltd | Graphene-like material |
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| CN109809749A (en) * | 2019-04-02 | 2019-05-28 | 四川聚创石墨烯科技有限公司 | A kind of construction method of graphite alkenes cement-base composite material |
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| CN112299768A (en) * | 2020-11-13 | 2021-02-02 | 西安建筑科技大学 | Graphene functionalized cement-based material and preparation method thereof |
| CN112299768B (en) * | 2020-11-13 | 2022-05-03 | 西安建筑科技大学 | Graphene functionalized cement-based material and preparation method thereof |
| CN116060002A (en) * | 2023-02-24 | 2023-05-05 | 中国科学院生态环境研究中心 | Graphene-loaded metal monoatomic composite material, preparation method and application |
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