CN105502371B - A kind of liquid phase strip preparation method of graphene - Google Patents
A kind of liquid phase strip preparation method of graphene Download PDFInfo
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- CN105502371B CN105502371B CN201610004175.9A CN201610004175A CN105502371B CN 105502371 B CN105502371 B CN 105502371B CN 201610004175 A CN201610004175 A CN 201610004175A CN 105502371 B CN105502371 B CN 105502371B
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- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
Abstract
The invention provides a kind of liquid phase strip preparation method of graphene, methods described is：The first step：Using aromatic compound as remover, stripper solution is configured, graphite powder is added, after being sufficiently stirred, obtains graphite prestripping dispersion liquid；Second step：The graphite prestripping dispersion liquid that the first step obtains by ultrasound and/or mechanical shearing peel off and disperseed, obtains graphene mixed dispersion：3rd step：Graphene mixed dispersion obtained by second step is centrifuged, then takes upper solution to dialyse, impurity is removed, obtains pure graphene product.The present invention can efficiently separate graphite flake layer, obtain substantial amounts of graphene in a short time, and obtained graphene is individual layer or few layer, conduction/good in thermal property, high comprehensive performance.The present invention have it is simple to operate, efficiency high, it is green the advantages that, be expected to realize prepared by the industrialization of graphene.
Description
Technical field
The invention belongs to technical field of graphene preparation, is a kind of liquid phase strip preparation method of graphene specifically.
Background technology
Graphene is a kind of " cellular " thin slice for the similar regular hexagon being made up of single layer of carbon atom, has preferable two
Tie up crystal structure.Graphene has great specific surface area (2630m2/ g) and super large carrier mobility (15000cm2/
(Vs)), its thermal conductivity is up to 5000W/ (mK).It is most tough in test material simultaneously, and intensity reaches 130GPa, than
Taller more than 100 times of steel.A kind of new material excellent as the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, stone
Black alkene is referred to as " king of new material ", there is great application prospect in fields such as energy storage, catalysis, electronics and biologic medicals.Herein
Under background, prepared by the scale of high-quality graphene turn into the key factor for meeting its application demand.
2004, the physicist An Delie lids nurses and Constantine Nuo Woxiao loves of Man Chesidun universities of Britain, lead to
Graphene is prepared from directional thermal decomposition graphite in the method for crossing adhesive tape mechanical stripping graphite, and this is to be prepared for the first time in the world
Grapheme two-dimension material.Hereafter the preparation of graphene turns into the study hotspot of scientific research personnel always, but at present there has been no quality and
The all gratifying preparation method of efficiency.
The graphene quality that the main flow preparation method such as epitaxial growth method and chemical vapor deposition CVD of graphene obtain
Height, there is certain advantage, but process conditions are complicated, and condition is difficult to control, and graphite oxide prepared by the dilute method of redox graphite
Alkene is readily incorporated the crystal structure defects of graphene, although can prepare on a large scale, performance has certain gap with graphene, and
Chemical reagent used is mostly poisonous.In contrast to this, liquid phase stripping method because with technique is simple, gained graphene performance is good,
The advantages that green non-poisonous reagent can be selected, is favored by more and more scientific research personnel.In liquid phase peels off graphite technology of preparing,
Preparation of the separation to graphene between graphite flake layer has a major impact.
The A of Publication No. CN 104495826 Chinese invention patent, there is provided a kind of single-layer graphene dispersion liquid and its system
Preparation Method, the dispersant such as dodecyl sodium sulfate is added in graphene solution, graphite in the solution scattered is promoted, to institute
Dispersion soln must be mixed and carry out mechanical shearing stripping, the dispersion soln of single-layer graphene can be obtained.The method uses organic
Solvent is mostly poisonous, thus limits the industrially prepared of graphene.
Therefore, high performance graphite is realized with the process meanses of a kind of environmental protection, low cost, good, the easy large-scale production of controllability
Preparing for alkene is significant.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to the liquid phase for proposing a kind of graphene peels off preparation side
Method, promote graphite flake layer separation using remover, the method for preparing high-quality graphene, solve prior art production efficiency
Low, the problems such as properties of product difference, the method is simple to operate, cost industry metaplasia that is low, green, being expected to realize graphene
Production.
The present invention is achieved by the following technical solutions：
To achieve the above object, the liquid phase strip preparation method of a kind of graphene of the present invention, comprises the following steps：
The first step：Using aromatic compound as remover, stripper solution is configured, adds graphite powder, after being sufficiently stirred,
Obtain graphite prestripping dispersion liquid；
Second step：The graphite prestripping dispersion liquid that the first step obtains by ultrasound and/or mechanical shearing peel off and divided
Dissipate, obtain graphene mixed dispersion；
3rd step：Graphene mixed dispersion obtained by second step is centrifuged, then takes upper solution to dialyse,
Impurity is removed, obtains pure graphene product.
Further, in the first step：Constantly it is stripped in view of graphite, the graphene or graphite flake layer of formation compare table
Area is big, it is difficult to and it is fully dispersed in the solution, thus the graphite solution of low concentration is more beneficial for the implementation of the present invention, stone of the present invention
Graphite concentration is preferably 0.1-20wt% in black prestripping dispersion liquid, and accordingly, the concentration of stripper solution is preferably 0.5-
10wt%.
Further, in the first step：The implementation of the present invention can use various different types of graphite, preferably scale
One or more in graphite, expansible graphite, graphite oxide powder, directional thermal decomposition graphite.
Further, in the first step：The aromatic compound remover, aromatic hydrocarbon and its derivative can be used
Thing, phenol (o-phenol, to biphenol and its esters), aromatic alcohol and its esters, aromatic acid and its esters, aromatic ester, fragrance
One or more in ether, aromatic nitro compound.In order to dissolve these removers, currently used solvent such as chloroform,
Acetone, toluene, dimethylbenzene etc. are toxic, and the preferably water/alcohol-soluble such as hydroquinones, catechol, sodium phenate is preferable in the present invention
Compound as remover so that implementation of the invention need to only use the environmentally friendly solvent such as water or alcohol.
Further, in the first step：Take into full account it is green in the case of, solvent of the invention is preferably
One kind in water, ethanol, glycerine or its is a variety of.
Further, in the first step：In order that graphite is uniformly dispersed in the solution, described stirring, preferably magnetic
Power stirs, and rotating speed is preferably 500-2000rpm, and mixing time is preferably 0.5-5 hours.
Further, in the second step：To make graphite be sufficiently separated under remover effect, described ultrasound, the time
Preferably 0.5-5 hours.
Further, in the second step：Described mechanical shearing, the equipment of use is preferably magnetic stirrer, shearing
One or more in mulser, homogenizer, ball mill, grinder, dispersion machine, fluid collider.
Further, in the 3rd step：Because graphene is difficult to settle in centrifuge, high speed centrifugation be more beneficial for from
The heart separates, and centrifugal rotational speed is preferably 5000-20000rpm, and centrifugation time is preferably 2-30 minutes.
Further, in the 3rd step：In order to obtain the higher graphene of purity, dialysis time is preferred in the present invention
For 1-5 days.
The present invention liquid phase stripping on the basis of add high activity remover (aromatic compound), these removers due to
Similar hexa-atomic carbon structure be present to graphite, effectively parent can be attached to graphite flake layer surface, insert between lamella, in assisting ultrasonic
Or during the stripping means such as emulsification pretreatment, graphite is layers-separated, realizes that short route produces high-quality graphene.It is used in the present invention
Remover is that prior art did not used, it is active high the advantages of.This remover of this fit on.The optional water of the present invention,
Alcohol or its mixed solution as green and environment-friendly solvent, have it is green, the advantages that being expected to realize graphene industrialization production.
Compared with prior art, beneficial effects of the present invention：
(1) the creative remover that high activity is added in ultrasound/physical shear stripping process, remover can be inserted effectively
Between entering graphite flake layer, the process of high velocity impact occurs in ultrasound/shear history with high-velocity fluid, wall or dispersed substance for graphite
Middle quick separating, the obtained graphene number of plies is few, and individual layer ratio is high.
(2) remover of the invention is preferably hydroquinones, catechol or sodium phenate, and water/alcohol-soluble is excellent, therefore is made
It is solvent that water or ethanol, which can be selected, in standby process, and production process is green.
(3) method of creative selection dialysis, carries out graphene purification, obtains the graphene of high-purity.
(4) preparation process of the present invention is simple, and cost is not high, and preparation time is short, is expected to realize the industrialized production of graphene.
Brief description of the drawings
Fig. 1 is that the liquid phase of the graphene of preferred embodiment of the present invention peels off preparation technology flow chart.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
As shown in figure 1, be a kind of process chart of the liquid phase strip preparation method of graphene of the present invention, the inventive method
Using aromatic compound as remover, stripper solution is configured, graphite powder is added, after being sufficiently stirred, obtains graphite prestripping
Dispersion liquid；Obtained graphite prestripping dispersion liquid by ultrasound and/or mechanical shearing peel off and disperseed, graphene is obtained and mixes
Close dispersion；Resulting graphene mixed dispersion is centrifuged, then takes upper solution to dialyse, removes impurity,
Obtain pure graphene product.Following examples are provided below in conjunction with the technology of the present invention, to be further understood to the present invention.
Embodiment 1
The present embodiment provides a kind of liquid phase stripping method and prepares graphene, and basic operational steps are as follows：
The first step, configuration concentration are the 10wt% hydroquinones aqueous solution, and 1g expanded graphites are scattered in into the 999g solution
In, obtain the mixed liquor of 0.1wt% graphite.
Second step, the mixed liquor 5 hours of the first step is handled with magnetic agitation, makes its dispersed, mixing speed is
500rpm, obtain graphite prestripping dispersion liquid.
3rd step, graphite prestripping dispersion liquid is subjected to ultrasound and peeled off 0.5 hour, selected supersonic frequency is 10KHz, tentatively
Obtain graphene mixed dispersion.
4th step, with centrifuge, graphene mixed dispersion is centrifuged, selected centrifuge speed is 5000
Rev/min, centrifugation time is 30 minutes, takes upper strata centrifugate.
5th step, upper strata centrifugate is subjected to dialysis treatment, dialysis time is 2 days, removes foreign ion, obtains high-purity
Graphene.
Resulting graphene is 1-5 layers, and stability is good, and diameter is in 0.2-20 microns, good conductivity, in light, electric material
Had a good application prospect Deng field.
Embodiment 2
With being in place of the main difference of embodiment 1：The present embodiment 2 has changed remover, increases graphite dispersing solution concentration,
And mechanical stripping is carried out using the method for ball milling, while change other related process parameters.
The basic operational steps that the liquid phase stripping method of the present embodiment 2 prepares graphene are as follows：
The first step, configuration concentration is 0.5wt% aqueous sodium phenolate solution, by 1g directional thermal decompositions graphite dispersion in the 4g solution
In, obtain 20wt% graphite solution.
Second step, handle the mixed liquor 0.5 hour with magnetic agitation, make its dispersed, mixing speed is
2000rpm, obtain graphite prestripping dispersion liquid；
3rd step, resulting graphite prestripping dispersion liquid pours into ball grinder, using zirconium oxide as ball-milling medium, according to 50:1
Ratio of grinding media to material ball milling 10 hours, tentatively obtain graphene mixed dispersion.
4th step, with centrifuge, graphene mixed dispersion is centrifuged, selected centrifuge speed is 20000
Rev/min, centrifugation time is 2 minutes, takes upper strata centrifugate.
5th step, the upper strata centrifugate is subjected to dialysis treatment, dialysis time is 1 day, removes foreign ion, obtains high-purity
Spend graphene.
Resulting graphene is 1-10 layers, and diameter can be used as the altered contents of composite in 0.2-10 microns.
Embodiment 3
With being in place of the main difference of embodiment 1：The present embodiment 3 has changed stripper solution, is sheared using combination of ultrasound
The method of emulsification carries out graphite stripping, while changes other related process parameters.
The basic operational steps that the liquid phase stripping method of the present embodiment 3 prepares graphene are as follows：
The first step, configuration concentration are the glycerite of 1wt% catechol, and 1g graphite oxide powder is scattered in into 9g solution
In, obtain the mixed solution of 10wt% graphite.
Second step, handle the mixed liquor 3 hours with magnetic agitation, make its dispersed, mixing speed 1000rpm,
Obtain graphite prestripping dispersion liquid.
3rd step, gained graphite prestripping dispersion liquid is subjected to ultrasound and peeled off 5 hours, selected supersonic frequency is 20kHz.
4th step, the mixed solution that ultrasound stripping obtains is transferred in emulsification pretreatment machine, shear rate is set to
5000rpm, time are 1 hour, obtained graphene mixed dispersion.
5th step, with centrifuge, graphene mixed dispersion is centrifuged, selected centrifuge speed is 12000
Rev/min, centrifugation time is 10 minutes, takes upper strata centrifugate.
6th step, the upper strata centrifugate is subjected to dialysis treatment, dialysis time is 2 days, removes foreign ion, obtains high-purity
Spend graphene.
Most of resulting graphene is individual layer, and thickness is about 0.5-0.65nm, and diameter compares surface at 0.2-10 μm
Product is about in 500-5000m2/ g, can be as the timbering material in the carrier or bioengineered tissue of composite.
Embodiment 4
With being in place of the main difference of embodiment 1：The present embodiment 3 changes stripper solution, is sheared using combination of ultrasound
The method of emulsification carries out graphite stripping, while changes other related process parameters.
The basic operational steps that the liquid phase stripping method of the present embodiment 4 prepares graphene are as follows：
The first step, configuration concentration are water/ethanol (1 of 5wt% catechol：1 volume ratio) mixed solution, by 1g scales
Graphite dispersion obtains the mixed liquor of 1wt% graphite in 99g solution.
Second step, handle the mixed liquor 2 hours with magnetic agitation, make its dispersed, obtain graphite prestripping and disperse
Liquid.
3rd step, gained graphite prestripping dispersion liquid is subjected to ultrasound and peeled off 3 hours, selected supersonic frequency is 20kHz.
4th step, the mixed solution that ultrasound stripping obtains is transferred in emulsification pretreatment machine, shear rate is set to
5000rpm, time are 1 hour, obtained graphene mixed dispersion.
5th step, with centrifuge, graphene mixed dispersion is centrifuged, selected centrifuge speed is 18000
Rev/min, centrifugation time is 5 minutes, takes upper strata centrifugate.
6th step, the upper strata centrifugate is subjected to dialysis treatment, dialysis time is 5 days, removes foreign ion, obtains high-purity
Spend graphene.
Most of resulting graphene is individual layer, and thickness is about 0.34-0.41nm, and diameter is expected at 0.2-10 μm
Applied in photo-electric sensing equipment, electrode etc..
Embodiment 5
With being in place of the main difference of embodiment 1：The present embodiment 3 changes stripper solution, using combination of ultrasound fluid
The method of head-on collision carries out graphite stripping, while changes other related process parameters.
The basic operational steps that the liquid phase stripping method of the present embodiment 3 prepares graphene are as follows：
The first step, configuration concentration are water/ethanol/glycerine (volume ratio 1 of 5wt% catechol：1：1) mixing is molten
Liquid, 1g expanded graphites are scattered in 9g solution, obtain 10wt% graphite solution.
Second step, handle the mixed liquor 2 hours with magnetic agitation, make its dispersed, obtain graphite prestripping and disperse
Liquid.
3rd step, gained graphite prestripping dispersion liquid is subjected to ultrasound and peeled off 0.5 hour, selected supersonic frequency is 20kHz.
4th step, the mixed solution that ultrasound stripping obtains is transferred in fluid collider, acts on 2 hours, obtains graphite
Alkene mixed dispersion.
5th step, with centrifuge, graphene mixed dispersion is centrifuged, and selected centrifuge speed is
15000rpm, centrifugation time are 7 minutes, take upper strata centrifugate.
6th step, the upper strata centrifugate is subjected to dialysis treatment, dialysis time is 5 days, removes foreign ion, obtains high-purity
Spend graphene.
Most of resulting graphene is individual layer, and thickness is about 0.34-0.41nm, and diameter compares table at 0.2-10 μm
Area is about in 100-2000m2/ g, good conductivity, there is great application in fields such as energy storage, catalysis, electronics and biologic medicals
Prospect.
It should be appreciated that the parameter being related in above example can be adjusted within the scope of the present invention, such as high work
Property remover can use other materials of the prior art, it is not limited to the record in above-described embodiment.This is for ability
For field technique personnel, it is easily achieved on the basis of description of the invention record, therefore repeat no more.
For the present invention using graphite as raw material, aromatic compound is remover, adds solvent and is thoroughly mixed, is mixed
Dispersion.Means are peeled off with reference to ultrasonic disperse, mechanical shearing etc., remover enters graphite layers, destroys the model of graphite layers
The power effect of moral China, efficiently separates graphite flake layer, obtains substantial amounts of graphene in a short time.Obtained graphene be individual layer or
Few layer, conduction/good in thermal property, high comprehensive performance.The present invention have it is simple to operate, efficiency high, it is green the advantages that, be expected to
Realize prepared by the industrialization of graphene.
The section Example of the present invention is the foregoing is only, any restrictions not are done to the technical scope of the present invention,
Any modification made within the spirit and principles of the invention, equivalent substitution and improvement etc., it should be included in the guarantor of the present invention
Within the scope of shield.
Claims (7)
1. the liquid phase strip preparation method of a kind of graphene, it is characterised in that step is as follows：
The first step：Using aromatic compound as remover, stripper solution is configured, graphite powder is added, after being sufficiently stirred, obtains
Graphite prestripping dispersion liquid；
The remover is the one or more in hydroquinones, catechol, sodium phenate；
The graphite prestripping dispersion liquid, wherein：Graphite concentration is 0.1-20wt%, and stripping agent concentration is 0.5-10wt%；
Second step：The graphite prestripping dispersion liquid that the first step obtains by ultrasound and/or mechanical shearing peel off and disperseed, is obtained
To graphene mixed dispersion：
3rd step：Graphene mixed dispersion obtained by second step is centrifuged, then takes upper solution to dialyse, is removed
Impurity, obtain pure graphene product.
A kind of 2. liquid phase strip preparation method of graphene according to claim 1, it is characterised in that：In the first step：Institute
The graphite stated is the one or more in crystalline flake graphite, expansible graphite, graphite oxide powder, directional thermal decomposition graphite.
A kind of 3. liquid phase strip preparation method of graphene according to claim any one of 1-2, it is characterised in that：First
The configuration stripper solution is walked, wherein one or more of the solvent used for water, ethanol or glycerine.
A kind of 4. liquid phase strip preparation method of graphene according to claim any one of 1-2, it is characterised in that：First
In step：Described stirring is magnetic agitation, and rotating speed 500-2000rpm, mixing time is 0.5-5 hours.
A kind of 5. liquid phase strip preparation method of graphene according to claim any one of 1-2, it is characterised in that：Second
In step：Described ultrasonic time is 0.5-5 hours.
A kind of 6. liquid phase strip preparation method of graphene according to claim any one of 1-2, it is characterised in that：Second
In step：Described mechanical shearing, the equipment used for magnetic stirrer, emulsification pretreatment machine, homogenizer, ball mill, grinder, point
Dissipate the one or more in machine, fluid collider.
A kind of 7. liquid phase strip preparation method of graphene according to claim any one of 1-2, it is characterised in that：3rd
In step：Described centrifugation, wherein：Rotating speed is 5000-20000rpm, and centrifugation time is 2-30 minutes；Described dialysis, time is
1-5 days.
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| CN106517166B (en) * | 2016-10-19 | 2018-05-18 | 成都新柯力化工科技有限公司 | A kind of compound remover that graphene is prepared for slurry stirring stripping |
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| CN109956499A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院深圳先进技术研究院 | The stripping means of two-dimensional material |
| CN108298531A (en) | 2018-03-28 | 2018-07-20 | 苏州大学 | A kind of preparation method of graphene |
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| CN109036868A (en) * | 2018-09-07 | 2018-12-18 | 南京师范大学 | Graphene oxide assists liquid phase removing preparing graphite alkene/graphene oxide composite material method and its composite material and application |
| CN110564100B (en) * | 2018-11-23 | 2020-07-28 | 华中科技大学 | Polymer/graphite nanosheet composite material, and preparation and application thereof |
| CN109761227A (en) * | 2019-02-24 | 2019-05-17 | 黎剑辉 | A method of being prepared on a large scale high-quality graphene |
| CN110182792A (en) * | 2019-05-27 | 2019-08-30 | 华侨大学 | A kind of self-stabilization dispersed graphite alkene nano material and preparation method |
| CN110204962A (en) * | 2019-05-27 | 2019-09-06 | 华侨大学 | A kind of Graphene conductive ink and preparation method thereof |
| CN111170864B (en) * | 2020-01-19 | 2023-06-30 | 合肥艾克思维新材料科技有限公司 | Graphene dispersing agent and preparation method thereof, and preparation method of graphene |
| CN115057434B (en) * | 2022-01-25 | 2023-01-17 | 昆明理工大学 | Process and device for preparing graphene |
| CN114709506A (en) * | 2022-05-20 | 2022-07-05 | 中南大学 | Modification method of retired lithium ion battery negative electrode material |
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| CN103172053B (en) * | 2011-12-20 | 2015-02-04 | 中国科学院微电子研究所 | Method for preparing graphene through phase peeling of graphite by using mixed solvent |
| CN103253659B (en) * | 2013-05-23 | 2015-09-23 | 渤海大学 | A kind of ultrasonic wave peels off the method for preparing graphite alkene |
| CN105197916A (en) * | 2014-06-09 | 2015-12-30 | 余泉茂 | Novel method for preparing graphene/oxidized graphene |
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