CN105502371A - Liquid-phase stripping preparation method of graphene - Google Patents
Liquid-phase stripping preparation method of graphene Download PDFInfo
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- CN105502371A CN105502371A CN201610004175.9A CN201610004175A CN105502371A CN 105502371 A CN105502371 A CN 105502371A CN 201610004175 A CN201610004175 A CN 201610004175A CN 105502371 A CN105502371 A CN 105502371A
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention provides a liquid-phase stripping preparation method of graphene. The liquid-phase stripping preparation method comprises the steps that first, an aromatic compound is used as a stripping agent to prepare a stripping agent solution, graphite powder is added, and graphite pre-stripping dispersion liquid is obtained after sufficient stirring; second, the graphite pre-stripping dispersion liquid obtained in the first step is subjected to stripping dispersion through ultrasonic and/or mechanical shear to obtain a graphene mixed dispersion system; third, the graphene mixed dispersion system obtained in the second step is centrifuged, the upper-layer solution can be taken for dialysis, and impurities are remove to obtain a pure graphene product. The liquid-phase stripping preparation method can effectively separate graphite flake layers, a large amount of graphene is obtained within a short period of time, and the prepared graphene is single-layer or double-layer graphene and is good in conductive/thermal performance and excellent in comprehensive performances. The liquid-phase stripping preparation method has the advantages of being simple in operation, high in efficiency and green, being environmentally-friendly and the like, and achievement of industrialized graphene preparation is hopeful.
Description
Technical field
The invention belongs to technical field of graphene preparation, specifically, is a kind of liquid phase strip preparation method of Graphene.
Background technology
Graphene is a kind of " cellular " thin slice by the similar regular hexagon of monolayer carbon atomic building, has desirable two dimensional crystal structure.Graphene has great specific surface area (2630m
2/ g) and the carrier mobility (15000cm of super large
2/ (Vs)), its thermal conductivity can reach 5000W/ (mK).Simultaneously it is the most tough in test material, and intensity reaches 130GPa, more taller than steel more than 100 times.As the thinnest, intensity is maximum, electrical and thermal conductivity performance the is excellent a kind of type material that find at present, Graphene is called as " king of novel material ", has great application prospect in fields such as energy storage, catalysis, electronics and biologic medicals.In this context, the scale preparation of high-quality graphene becomes the key factor meeting its application demand.
2004, the physicist An Delie of Man Chesidun university of Britain. lid nurse and Constantine. Nuo Woxiaoluofu, prepare Graphene by the method for adhesive tape mechanically peel graphite from directional thermal decomposition graphite, this is that first time prepares grapheme two-dimension material in the world.After this preparation of Graphene becomes the study hotspot of scientific research personnel always, but not yet has all gratifying preparation method of quality and efficiency at present.
The Graphene quality that the main flow preparation method of Graphene obtains as epitaxial growth method and chemical vapour deposition CVD is high, there is certain advantage, but processing condition are complicated, condition is wayward, and the standby graphene oxide of the rare legal system of redox graphite easily introduces the crystal structure defects of Graphene, although can prepare on a large scale, performance and Graphene have certain gap, and chemical reagent used is mostly poisonous.In contrast to this, technique is simple, gained Graphene performance is good, can select the advantages such as green non-poisonous reagent because have for liquid phase stripping method, is subject to the favor of more and more scientific research personnel.Peel off in graphite technology of preparing in liquid phase, the preparation of the separation between graphite flake layer to Graphene has material impact.
Publication number is the Chinese invention patent of CN104495826A, provide a kind of single-layer graphene dispersion liquid and preparation method thereof, the dispersion agents such as sodium laurylsulfonate are added in graphene solution, facilitate graphite dispersion in the solution, mechanical shearing stripping is carried out to gained blending dispersion solution, the dispersion soln of single-layer graphene can be obtained.The organic solvent that this method uses is mostly poisonous, thus limits the industry preparation of Graphene.
Therefore, the preparation of High-performance graphene is realized with the process means of a kind of environmental protection, low cost, good, the easy large-scale production of controllability significant.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, propose a kind of liquid phase strip preparation method of Graphene, graphite flake layer is separated to utilize stripper to promote, prepare the method for high-quality graphene, solve prior art production efficiency low, the problems such as product performance difference, this method is simple to operate, and cost is low, environmental protection, the industrialization that is expected to realize Graphene are produced.
The present invention is achieved by the following technical solutions:
For achieving the above object, the liquid phase strip preparation method of a kind of Graphene of the present invention, comprises the steps:
The first step: take aromatics as stripper, configuration stripper solution, adds Graphite Powder 99, after fully stirring, obtains graphite prestripping dispersion liquid;
Second step: the graphite prestripping dispersion liquid the first step obtained carries out stripping dispersion by ultrasonic and/or mechanical shearing, obtains Graphene mixed dispersion;
3rd step: the Graphene mixed dispersion obtained by second step carries out centrifugal, then gets upper solution dialysis, and removing impurity, obtains pure graphene product.
Further, in the described the first step: consider that graphite is constantly stripped, Graphene or the graphite flake layer specific surface area of formation are large, be difficult to fully disperse in the solution, thus the graphite solution of lower concentration is more conducive to enforcement of the present invention, in graphite prestripping dispersion liquid of the present invention, graphite concentration is preferably 0.1-20wt%, and accordingly, the concentration of stripper solution is preferably 0.5-10wt%.
Further, in the described the first step: enforcement of the present invention can adopt various different types of graphite, be preferably one or more in crystalline flake graphite, expansible black lead, graphite oxide powder, directional thermal decomposition graphite.
Further, in the described the first step: described aromatics stripper, one or more in fragrant hydrocarbons and their derivates, phenol (o-phenol, to biphenol and its esters), aromatic alcohol and its esters, aromatic acid and its esters, aromatic ester, aromatic oxide, aromatic nitro compound can be adopted.In order to dissolve these strippers, solvent ratio conventional is at present as toxic in chloroform, acetone, toluene, dimethylbenzene etc., in the present invention, the water/good compound of alcohol dissolubility such as preferred Resorcinol, pyrocatechol, sodium phenylate is as stripper, makes enforcement of the present invention only need the environmentally friendly solvents such as use water or alcohol.
Further, in the described the first step: when taking into full account environmental protection, solvent of the present invention is preferably one in water, ethanol, glycerine or it is multiple.
Further, in the described the first step: in order to make graphite be uniformly dispersed in the solution, described stirring, be preferably magnetic agitation, rotating speed is preferably 500-2000rpm, and churning time is preferably 0.5-5 hour.
Further, in described second step: for making graphite fully be separated under stripper effect, described is ultrasonic, and the time is preferably 0.5-5 hour.
Further, in described second step: described mechanical shearing, the equipment of employing be preferably in magnetic stirrer, emulsification pretreatment machine, homogenizer, ball mill, shredder, dispersion machine, fluid collider one or more.
Further, in described 3rd step: because Graphene is difficult to sedimentation in centrifuges, high speed centrifugation is more conducive to centrifugation, and centrifugal rotational speed is preferably 5000-20000rpm, and centrifugation time is preferably 2-30 minute.
Further, in described 3rd step: in order to obtain the higher Graphene of purity, in the present invention, dialysis time is preferably 1-5 days.
The present invention adds high reactivity stripper (aromatics) on the basis that liquid phase is peeled off, owing to there is similar hexa-atomic carbon structure to graphite in these strippers, effectively parent can be attached to graphite flake layer surface, insert between lamella, when assisting ultrasonic or emulsification pretreatment etc. peel off means, graphite is separated layer by layer, realizes short route and produces high-quality graphene.Stripper used in the present invention is that prior art did not adopt, and has active high advantage.This stripper of this fit on.The present invention can select water, alcohol or its mixing solutions as green and environment-friendly solvent, has environmental protection, is expected to realize the advantages such as Graphene industrialization production.
Compared with prior art, beneficial effect of the present invention:
(1) creationaryly in ultrasonic/physical shear stripping process, highly active stripper is added, stripper can effectively insert between graphite flake layer, graphite in ultrasonic/shear history with sharp separation in the process of high-velocity fluid, wall or dispersed substance generation high velocity impact, the Graphene number of plies obtained is few, and individual layer ratio is high.
(2) stripper of the present invention is preferably Resorcinol, pyrocatechol or sodium phenylate, and water/alcohol dissolubility is excellent, and therefore preparation process can select water or ethanol to be solvent, production process environmental protection.
(3) the creationary method selecting dialysis, carries out Graphene purification, obtains highly purified Graphene.
(4) preparation process of the present invention is simple, and cost is not high, and preparation time is short, is expected to the suitability for industrialized production realizing Graphene.
Accompanying drawing explanation
Fig. 1 is that the liquid phase of the Graphene of preferred embodiment of the present invention peels off preparation technology's schema.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
As shown in Figure 1, be the process flow sheet of the liquid phase strip preparation method of a kind of Graphene of the present invention, the inventive method take aromatics as stripper, and configuration stripper solution, adds Graphite Powder 99, after fully stirring, obtains graphite prestripping dispersion liquid; The graphite prestripping dispersion liquid obtained is carried out stripping dispersion by ultrasonic and/or mechanical shearing, obtains Graphene mixed dispersion; Undertaken centrifugal by obtained Graphene mixed dispersion, then get upper solution dialysis, removing impurity, obtains pure graphene product.Following examples are provided, to do further understanding to the present invention below in conjunction with the technology of the present invention.
Embodiment 1
The present embodiment provides a kind of liquid phase stripping method to prepare Graphene, and basic operational steps is as follows:
The first step, configuration concentration is the Resorcinol aqueous solution of 10wt%, is scattered in by 1g expanded graphite in this solution of 999g, obtains the mixed solution of 0.1wt% graphite.
Second step, the mixed solution of the utilization magnetic agitation process the first step 5 hours, make it dispersed, stirring velocity is 500rpm, obtains graphite prestripping dispersion liquid.
3rd step, carries out ultrasonic stripping 0.5 hour by graphite prestripping dispersion liquid, and selected ultrasonic frequency is 10KHz, tentatively obtains Graphene mixed dispersion.
4th step, use whizzer, undertaken centrifugal by Graphene mixed dispersion, selected centrifuge speed is 5000 revs/min, and centrifugation time is 30 minutes, gets upper strata centrifugate.
5th step, carries out dialysis treatment by upper strata centrifugate, and dialysis time is 2 days, removes foreign ion, obtains high purity graphite alkene.
The Graphene obtained is 1-5 layer, good stability, and diameter is at 0.2-20 micron, and good conductivity, has a good application prospect in fields such as optical, electrical materials.
Embodiment 2
Be with embodiment 1 main difference part: the present embodiment 2 has changed stripper, increases graphite dispersing solution concentration, and adopt the method for ball milling to carry out mechanically peel, change other related process parameters simultaneously.
The basic operational steps that the present embodiment 2 liquid phase stripping method prepares Graphene is as follows:
The first step, configuration concentration is the aqueous sodium phenolate solution of 0.5wt%, by 1g directional thermal decomposition graphite dispersion in this solution of 4g, obtains 20wt% graphite solution.
Second step, use this mixed solution of magnetic agitation process 0.5 hour, make it dispersed, stirring velocity is 2000rpm, obtains graphite prestripping dispersion liquid;
3rd step, the graphite prestripping dispersion liquid obtained pours ball grinder into, take zirconium white as ball-milling medium, according to the ratio of grinding media to material ball milling 10 hours of 50:1, tentatively obtains Graphene mixed dispersion.
4th step, use whizzer, undertaken centrifugal by Graphene mixed dispersion, selected centrifuge speed is 20000 revs/min, and centrifugation time is 2 minutes, gets upper strata centrifugate.
5th step, carries out dialysis treatment by this upper strata centrifugate, and dialysis time is 1 day, removes foreign ion, obtains high purity graphite alkene.
The Graphene obtained is 1-10 layer, and diameter is at 0.2-10 micron, and the altered contents that can be used as matrix material uses.
Embodiment 3
Be with embodiment 1 main difference part: the present embodiment 3 has changed stripper solution, adopt the method for combination of ultrasound emulsification pretreatment to carry out graphite stripping, change other related process parameters simultaneously.
The basic operational steps that the present embodiment 3 liquid phase stripping method prepares Graphene is as follows:
The first step, configuration concentration is the glycerine solution of the pyrocatechol of 1wt%, is scattered in 9g solution by 1g graphite oxide powder, obtains the mixing solutions of 10wt% graphite.
Second step, use this mixed solution of magnetic agitation process 3 hours, make it dispersed, stirring velocity is 1000rpm, obtains graphite prestripping dispersion liquid.
3rd step, gained graphite prestripping dispersion liquid is carried out ultrasonic stripping 5 hours, and selected ultrasonic frequency is 20kHz.
4th step, transferred in emulsification pretreatment machine by the mixing solutions that ultrasonic stripping obtains, velocity of shear is set to 5000rpm, and the time is 1 hour, the Graphene mixed dispersion obtained.
5th step, use whizzer, undertaken centrifugal by Graphene mixed dispersion, selected centrifuge speed is 12000 revs/min, and centrifugation time is 10 minutes, gets upper strata centrifugate.
6th step, carries out dialysis treatment by this upper strata centrifugate, and dialysis time is 2 days, removes foreign ion, obtains high purity graphite alkene.
The Graphene great majority obtained are individual layer, and thickness is approximately 0.5-0.65nm, and diameter is at 0.2-10 μm, and specific surface area is greatly about 500-5000m
2/ g, can be used as the timbering material in the carrier of matrix material or bioengineered tissue.
Embodiment 4
Be with embodiment 1 main difference part: the present embodiment 3 changes stripper solution, adopt the method for combination of ultrasound emulsification pretreatment to carry out graphite stripping, change other related process parameters simultaneously.
The basic operational steps that the present embodiment 4 liquid phase stripping method prepares Graphene is as follows:
The first step, configuration concentration is water/ethanol (1:1 volume ratio) mixing solutions of the pyrocatechol of 5wt%, is scattered in 99g solution by 1g crystalline flake graphite, obtains the mixed solution of 1wt% graphite.
Second step, uses this mixed solution of magnetic agitation process 2 hours, makes it dispersed, obtain graphite prestripping dispersion liquid.
3rd step, gained graphite prestripping dispersion liquid is carried out ultrasonic stripping 3 hours, and selected ultrasonic frequency is 20kHz.
4th step, transferred in emulsification pretreatment machine by the mixing solutions that ultrasonic stripping obtains, velocity of shear is set to 5000rpm, and the time is 1 hour, the Graphene mixed dispersion obtained.
5th step, use whizzer, undertaken centrifugal by Graphene mixed dispersion, selected centrifuge speed is 18000 revs/min, and centrifugation time is 5 minutes, gets upper strata centrifugate.
6th step, carries out dialysis treatment by this upper strata centrifugate, and dialysis time is 5 days, removes foreign ion, obtains high purity graphite alkene.
The Graphene great majority obtained are individual layer, and thickness is approximately 0.34-0.41nm, and diameter, at 0.2-10 μm, is expected to apply in photo-electric sensing equipment, electrode etc.
Embodiment 5
Be with embodiment 1 main difference part: the present embodiment 3 changes stripper solution, adopt the method for combination of ultrasound fluid head-on collision to carry out graphite stripping, change other related process parameters simultaneously.
The basic operational steps that the present embodiment 3 liquid phase stripping method prepares Graphene is as follows:
The first step, configuration concentration is the mixing solutions of the water/ethanol/glycerine (volume ratio 1:1:1) of the pyrocatechol of 5wt%, is scattered in 9g solution by 1g expanded graphite, obtains 10wt% graphite solution.
Second step, uses this mixed solution of magnetic agitation process 2 hours, makes it dispersed, obtain graphite prestripping dispersion liquid.
3rd step, gained graphite prestripping dispersion liquid is carried out ultrasonic stripping 0.5 hour, and selected ultrasonic frequency is 20kHz.
4th step, transfers to the mixing solutions that ultrasonic stripping obtains in fluid collider, acts on 2 hours, obtains Graphene mixed dispersion.
5th step, use whizzer, undertaken centrifugal by Graphene mixed dispersion, selected centrifuge speed is 15000rpm, and centrifugation time is 7 minutes, gets upper strata centrifugate.
6th step, carries out dialysis treatment by this upper strata centrifugate, and dialysis time is 5 days, removes foreign ion, obtains high purity graphite alkene.
The Graphene great majority obtained are individual layer, and thickness is approximately 0.34-0.41nm, and diameter is at 0.2-10 μm, and specific surface area is greatly about 100-2000m
2/ g, good conductivity, has great application prospect in fields such as energy storage, catalysis, electronics and biologic medicals.
Should be understood that, the parameter related in above embodiment can adjust within the scope of the present invention, and such as high reactivity stripper can adopt other materials of the prior art, is not limited to the record in above-described embodiment.This is easy to realize, therefore repeats no more to those skilled in the art on the basis that specification sheets of the present invention is recorded.
The present invention take graphite as raw material, and aromatics is stripper, adds solvent and is fully uniformly mixed, obtain mixed dispersion.In conjunction with the stripping such as ultrasonic disperse, mechanical shearing means, stripper enters graphite layers, destroys the van der Waals interaction of graphite layers, is effectively separated graphite flake layer, obtains a large amount of Graphenes at short notice.Obtained Graphene is individual layer or few layer, conduction/good in thermal property, high comprehensive performance.The present invention has simple to operate, the advantages such as efficiency is high, environmental protection, is expected to the industrialization preparation realizing Graphene.
The foregoing is only section Example of the present invention, not do any restriction to technical scope of the present invention, all any amendments made within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a liquid phase strip preparation method for Graphene, is characterized in that step is as follows:
The first step: take aromatics as stripper, configuration stripper solution, adds Graphite Powder 99, after fully stirring, obtains graphite prestripping dispersion liquid;
Second step: the graphite prestripping dispersion liquid the first step obtained carries out stripping dispersion by ultrasonic and/or mechanical shearing, obtains Graphene mixed dispersion:
3rd step: the Graphene mixed dispersion obtained by second step carries out centrifugal, then gets upper solution dialysis, and removing impurity, obtains pure graphene product.
2. the liquid phase strip preparation method of a kind of Graphene according to claim 1, it is characterized in that: in the first step: described stripper is aromatics, is one or more in fragrant hydrocarbons and their derivates, phenol, aromatic alcohol and its esters, aromatic acid and its esters, aromatic ester, aromatic oxide, aromatic nitro compound.
3. the liquid phase strip preparation method of a kind of Graphene according to claim 2, is characterized in that: one or more in described stripper Resorcinol, pyrocatechol, sodium phenylate.
4. the liquid phase strip preparation method of a kind of Graphene according to claim 1, is characterized in that: in the first step: described graphite is one or more in crystalline flake graphite, expansible black lead, graphite oxide powder, directional thermal decomposition graphite.
5. the liquid phase strip preparation method of a kind of Graphene according to claim 1, is characterized in that: in the first step: described graphite prestripping dispersion liquid, and wherein: graphite concentration is 0.1-20wt%, stripper concentration is 0.5-10wt%.
6. the liquid phase strip preparation method of a kind of Graphene according to any one of claim 1-5, is characterized in that: the solvent described in the first step is one or more of water, ethanol or glycerine.
7. the liquid phase strip preparation method of a kind of Graphene according to any one of claim 1-5, is characterized in that: in the first step: described stirring is magnetic agitation, and rotating speed is 500-2000rpm, and churning time is 0.5-5 hour.
8. the liquid phase strip preparation method of a kind of Graphene according to any one of claim 1-5, is characterized in that: in second step: described ultrasonic time is 0.5-5 hour.
9. the liquid phase strip preparation method of a kind of Graphene according to any one of claim 1-5, it is characterized in that: in second step: described mechanical shearing, the equipment of employing is one or more in magnetic stirrer, emulsification pretreatment machine, homogenizer, ball mill, shredder, dispersion machine, fluid collider.
10. the liquid phase strip preparation method of a kind of Graphene according to any one of claim 1-5, is characterized in that: in the 3rd step: described is centrifugal, wherein: rotating speed is 5000-20000rpm, and centrifugation time is 2-30 minute; Described dialysis, the time is 1-5 days.
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| CN105948033A (en) * | 2016-07-11 | 2016-09-21 | 黑龙江碳时代石墨烯科技有限公司 | Method of preparing graphene by means of wet microwave stripping |
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| 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 |
| WO2020239143A1 (en) * | 2019-05-27 | 2020-12-03 | 华侨大学 | Graphene conductive ink and preparation method therefor |
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| CN111170864A (en) * | 2020-01-19 | 2020-05-19 | 安徽大学 | Graphene dispersing agent, preparation method thereof and preparation method of graphene |
| 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 |
| CN115057434A (en) * | 2022-01-25 | 2022-09-16 | 昆明理工大学 | Process and device for preparing graphene |
| CN114735686A (en) * | 2022-04-29 | 2022-07-12 | 湖州市吴兴区核源金属新材研究院 | Preparation method of graphene aqueous solution and graphene nanosheet |
| 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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