CN105948028A - Method for preparation of graphene precursor by internal mixer peeling and graphene precursor - Google Patents
Method for preparation of graphene precursor by internal mixer peeling and graphene precursor Download PDFInfo
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- CN105948028A CN105948028A CN201610296453.2A CN201610296453A CN105948028A CN 105948028 A CN105948028 A CN 105948028A CN 201610296453 A CN201610296453 A CN 201610296453A CN 105948028 A CN105948028 A CN 105948028A
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Abstract
The invention provides a method for preparation of a graphene precursor by internal mixer peeling and a graphene precursor. Graphite is subjected to long time infiltration treatment in an aqueous dispersion liquid of an excess intercalator, a carbohydrate substance is used as a bonding and peeling carrier, through shearing and stretching of the viscous carbohydrate substance by an internal mixer, the graphite is indirectly stretched, sheared and peeled by the viscous carbohydrate substance under the bonding effect of the carbohydrate substance so as to obtain the graphene precursor. The provided shear mode is mild, the technical defect that the layered structure of graphene is destroyed due to the direct action of machinery's huge shearing force on graphene in a mechanical peeling process in the prior is effectively overcome, at the same time, destruction of chemical reaction to the graphene structure in the prior art is also avoided, thus realizing the technical effects of high product quality and little environmental pollution, etc. The precursor prepared by the method provided by the invention has stable properties and is easy to be stripped into graphene.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to a kind of method that Graphene presoma is prepared in banbury stripping
And Graphene presoma.
Background technology
Graphene (graphene), is that a kind of to be formed hexagon by carbon atom with sp2 hybrid orbital be honeycomb lattice
Flat film, the only two-dimensional material of a carbon atom thickness.Univ Manchester UK Andre Geim in 2004 with
Konstantin Novoselov successfully utilizes adhesive tape to peel off the mode of graphite, it was demonstrated that available single-layer graphene, and obtains
The Nobel prize for physics of 2010.Graphene be at present the thinnest be also the hardest material, heat conductivity is higher than nanometer
Carbon pipe and diamond, its electron mobility also ratio CNT or silicon wafer height under room temperature, resistivity ratio copper or silver are lower, for mesh
The material that on former world, resistivity is minimum.Therefore, developing low-cost, high yield prepare the method for high-quality graphene becomes business
The premise of application, is also the place of research key.
The preparation method of Graphene mainly includes that chemical vapour deposition technique, oxidation intercalation restore method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain high-quality Graphene, but productivity is low, and substrate is required height, turns
Move and there is difficulty greatly；Oxidation intercalation restores method and can realize producing Graphene in batches, but due to stone in oxidizing process
The structure of ink alkene is destroyed, it is difficult to obtain high-quality graphene product；Liquid phase stripping method is in a suitable solvent, utilizes
Graphite flake layer is dissociated by ultrasonic energy, but, solvent stripping method is prepared Graphene existence and is difficult to remove asking of residual solvent
Topic, and solvent stripping productivity is the lowest.By contrast, mechanical stripping method is that one can prepare high-quality stone with low cost
The simple method of ink alkene.
Chinese invention patent application number 201280019582.7 discloses a kind of method preparing Graphene, is passed through by graphite
Grinding, ball milling, airflow milling etc. are ground 0.5-4 hour by ionic liquid and are obtained Graphene.Graphite is promoted by ionic liquid
Stripping, but use that to grind for a long time the Graphene crystalline size obtained little, and Graphene layer crystal can be made by ionic liquid
Lattice are affected.
Chinese invention patent application number 201410260297.5 discloses the preparation method of a kind of Graphene, by citric acid
And/or the carboxylating agent such as one or more the mixture in oxalic acid and carboxylic acid derivates thereof is carried out as graphite intercalation reagent
Ball milling, but although making ink can thinning peel off under the special adsorption of carboxylating agent, but owing to grinding, graphite is applied pressure,
The graphite peeled off is produced huge impulsive force, and this impulsive force can make graphene layer produce fault of construction, easily causes graphite
Alkene Rotating fields lattice defect, and the Graphene prepared is carboxylation, and product needs again to process.
Chinese invention patent application number 201410717660.1 discloses the shearing stripping of a kind of aqueous phase and prepares the side of Graphene
Method, uses the method for chemical oxidation intercalation or electrochemical intercalation to carry out intercalation processing by raw graphite, makes intercalator enter graphite
Interlayer, prepares graphite intercalation compound, and follow-up employing shearing stirrer stirs and then prepares Graphene.Due in the program
Have employed the strong oxidizers such as sulphuric acid, nitric acid, perchloric acid and obtain graphite intercalation compound as intercalator, after chemical reaction, this
The Graphene that method obtains is the most defective, affects the electric conductivity of Graphene, and can cause environmental pollution, limits this method extensive
Industrial applications.
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 quality of Graphene after peeling off, additionally, in order to improve mechanical stripping efficiency, entered graphite before mechanical treatment
Row intercalation process occurs chemical reaction, is easily destroyed graphene-structured, pollute environment, be not easy to prepare high-quality graphite
Alkene, it is difficult to realize large-scale industrial and produce.
Summary of the invention
For the problems referred to above faced in the current scheme to graphite mechanical stripping, the present invention proposes a kind of banbury stripping
From preparation method and the Graphene presoma of Graphene presoma, by by graphite in the aqueous dispersions of excess intercalator long time
Between after infiltration processes, be mixed feeding banbury by the intercalated graphite in moistening shape and appropriate glucide, cutting by banbury
Cut and stretch, make graphite be glued under the bonding effect of glucide, stretch, shear stripping obtain Graphene presoma with sugar
Mixture, the most cleaned, be dried to obtain Graphene presoma.Presoma prepared by the present invention is for preparing Graphene
Optimum feed stock, it is easy to peel off into Graphene.
For solve the problems referred to above, the present invention by the following technical solutions:
On the one hand providing a kind of method that Graphene presoma is prepared in banbury stripping, described method comprises the steps:
(1) using graphite powder as raw material, described raw material and excess intercalator are placed in the deionized water containing dispersant, described
Raw material is 1:(0.8-2 with described excess intercalator, the mass ratio of the described deionized water three containing dispersant): (5-20),
Stirring mixed solution is uniformly distributed to raw material, and described mixed solution is carried out supersound process, and arranging ultrasonic power is 10-200KW,
Supersound process 2-30 hour, obtains the graphite powder dispersion liquid of infiltration；
(2) the graphite powder dispersion liquid of infiltration is centrifuged process, be filtrated to get moistening graphite powder, by moistening graphite powder with
Glucide blended under agitation, described moistening graphite powder is 1:4-20 with the mass ratio of glucide, obtains graphite powder/sugar mixing
Thing；
(3) graphite powder/sugar mixture is added in banbury, banbury technique is set, by shearing and the stretching of banbury, makes
Graphite is glued in jelly, stretches, shears and peel off the mixture obtaining Graphene/sugar；
(4) mixture of Graphene/sugar step (3) obtained is before deionized water cleans 3-10 time, is dried to obtain Graphene
Drive body.
Preferably, described graphite powder is natural flake graphite, aquadag, expansible graphite, highly oriented graphite, thermal cracking
At least one in graphite composite powder；Intercalator is acrylamide, Methanamide, potassium acetate, dimethyl sulfoxide, carbamide, ethylenediamine, diformazan
At least one in base sulfoxide.
Preferably, at least one during described glucide is sucrose, glucose, fructose, maltose.
Preferably, in the described deionized water containing dispersant, the weight ratio of dispersant and deionized water is 1:100-
150, described dispersant be in sodium lauryl sulphate, dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, 1-pyridine acid extremely
Few one.
Preferably, described in step (1), the mixing speed of mixed solution is 10-300rpm, centrifugal place described in step (2)
The rotating speed of reason is 100-1500rpm, and disengaging time is 30-60 minute.
Preferably, the banburying process of described banbury is 80-180 DEG C, 10r/min, 95-200 DEG C, 20r/min, 115-
250 DEG C, each banburying 40-60min in the case of 30r/min.
Preferably, described it is dried as evaporation drying or spray drying.
On the other hand a kind of Graphene presoma is provided, above-mentioned preparation method utilizes banbury to shear stripping and prepare
Graphene presoma.This Graphene presoma disperses i.e. to can get Graphene by simple and mechanical stripping.
The Graphene presoma prepared by the present invention is utilized to utilize mechanical means to separate Graphene, performance test such as table 1
Shown in.
Table 1:
The method that Graphene presoma is prepared in the present invention a kind of banbury stripping, compared with prior art, its prominent feature and
Excellent effect is:
1, the method that Graphene presoma is prepared in a kind of banbury stripping that the present invention provides, with graphite as raw material, utilizes saccharide
Material is bonding stripping carrier, by shearing and the tensile viscosity glucide of banbury, makes bonding at glucide of graphite
Under effect, indirectly stretched by the glucide of viscosity, shearing stripping obtains Graphene presoma, it is provided that cut mode is gentle, has
Effect avoids the significant shear power of machinery during mechanical stripping and directly acts on Graphene and destroy the layer structure of Graphene.
2, this programme is prepared in the way of pure physics, it is to avoid the chemical reaction destruction to graphene-structured, it is thus achieved that
Product quality higher, few to environment.
3, scheme preparation technology disclosed by the invention is simple, and raw material sources are extensive, low cost, the presoma character prepared
Stable, easily store and transport, it is easy to accomplish large-scale industrial produces.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should be interpreted as the present invention
Scope be only limitted to Examples below.In the case of without departing from said method thought of the present invention, according to ordinary skill
Various replacements that knowledge and customary means are made or change, should be included in the scope of the present invention.
Embodiment 1
(1) using natural flake graphite powder body as raw material, natural flake graphite powder body and excessive propene amide are placed in containing ten
In the deionized water of sodium dialkyl sulfate, natural flake graphite powder body and acrylamide, described containing sodium lauryl sulphate
The mass ratio of deionized water three is 1:0.8:5, in the deionized water containing sodium lauryl sulphate sodium lauryl sulphate with
The weight ratio of deionized water is 1:100, is then stirred mixed solution, and arranging mixing speed is 10rpm, stirring mixing
After solution is uniformly distributed to raw material, mixed solution being carried out supersound process, arranging ultrasonic power is 10KW, and supersound process 30 is little
Time, obtain the natural flake graphite powder dispersion liquid of infiltration；
(2) being centrifuged the natural flake graphite powder dispersion liquid of infiltration processing, the rotating speed of centrifugal treating is 100rpm, during separation
Between be 60 minutes, be then filtrated to get moistening natural flake graphite powder, by moistening natural flake graphite powder and sucrose granules
Blended under agitation, moistening graphite powder is 1:4 with the mass ratio of sucrose granules, obtains natural flake graphite powder/sucrose mixture；
(3), during natural flake graphite powder/sucrose mixture adds banbury, the sweet sweetening process of banbury banbury is set for first to set
Put 180 DEG C, 10r/min banburying 40min, be then warming up to 200 DEG C, 20r/min banburying 40min, finally heat up 250 DEG C,
30r/min banburying 60min, makes sucrose melt and increases its mobility and viscosity, by shearing and the stretching of banbury, makes
Graphite, under the bonding effect of glucide, is indirectly obtained presoma obtain stone by the glucide stretching of viscosity, shearing stripping
The mixture of ink alkene/sucrose；
(4) mixture of Graphene/sucrose step (3) obtained obtains graphite through deionized water cleaning 10 times, evaporation drying
Alkene presoma.Through test, the 90% Graphene presoma radial dimension obtained in embodiment 5 is 150-260 μm, 90% Graphene
Presoma thickness is 30-40 μm.
Embodiment 2
(1) using aquadag body as raw material, aquadag powder body and excess Methanamide are placed in containing sodium lauryl sulphate
Deionized water in, aquadag powder body and Methanamide, the quality of the described deionized water three containing sodium lauryl sulphate
Ratio is 1:1:10, and in the deionized water containing sodium lauryl sulphate, sodium lauryl sulphate with the weight ratio of deionized water is
1:100, is then stirred mixed solution, and arranging mixing speed is 50rpm, and stirring mixed solution is uniformly distributed to raw material
After, mixed solution is carried out supersound process, arranging ultrasonic power is 100KW, supersound process 15 hours, obtains the colloid stone of infiltration
Powdered ink dispersion liquid；
(2) being centrifuged the aquadag powder dispersion liquid of infiltration processing, the rotating speed of centrifugal treating is 100rpm, and disengaging time is
60 minutes, then it is filtrated to get moistening aquadag powder, by moistening aquadag powder and sucrose granules blended under agitation, moistening
The mass ratio of graphite powder and sucrose granules be 1:4, obtain aquadag powder/sucrose mixture；
(3), during aquadag powder/sucrose mixture adds banbury, the sweet sweetening process of banbury banbury is set for first to arrange
180 DEG C, 10r/min banburying 40min, be then warming up to 200 DEG C, 20r/min banburying 50min, and finally heat up 250 DEG C, 30r/
Min banburying 60min, makes sucrose melt and increases its mobility and viscosity, by shearing and the stretching of banbury, makes graphite
Under melted sucrose bonding effect, indirectly obtained presoma obtain Graphene/sucrose by the sucrose stretching of viscosity, shearing stripping
Mixture；
(4) mixture of Graphene/sucrose step (3) obtained obtains graphite through deionized water cleaning 10 times, evaporation drying
Alkene presoma.Through test, the 90% Graphene presoma radial dimension obtained in embodiment 5 is 240-420 μm, 90% Graphene
Presoma thickness is 15-30 μm.
Embodiment 3
(1) using expansible graphite as raw material, expansible graphite powder body and excess Methanamide are placed in containing lauryl sulphate acid
In the deionized water of sodium, expansible graphite powder body and Methanamide, the described deionized water three containing sodium lauryl sulphate
Mass ratio is 1:1:10, in the deionized water containing sodium lauryl sulphate the weight of sodium lauryl sulphate and deionized water it
Ratio is 1:100, is then stirred mixed solution, and arranging mixing speed is 50rpm, and stirring mixed solution uniformly divides to raw material
After cloth, mixed solution being carried out supersound process, arranging ultrasonic power is 100KW, supersound process 15 hours, obtains the colloid of infiltration
Graphite powder dispersion liquid；
(2) being centrifuged the expansible graphite powder dispersion liquid of infiltration processing, the rotating speed of centrifugal treating is 100rpm, disengaging time
It is 60 minutes, is then filtrated to get moistening expansible graphite powder, moistening expansible graphite powder is stirred with maltose granule
Being blended, moistening graphite powder is 1:4 with the mass ratio of maltose granule, obtains aquadag powder/maltose mixture；
(3), during aquadag powder/maltose mixture adds banbury, the sweet sweetening process of banbury banbury is set for first to arrange
80 DEG C, 10r/min banburying 40min, be then warming up to 950 DEG C, 20r/min banburying 50min, and finally heat up 115 DEG C, 30r/
Min banburying 60min, makes sucrose melt and increases its mobility and viscosity, by shearing and the stretching of banbury, makes graphite
Under melted sucrose bonding effect, indirectly obtained presoma obtain Graphene/maltose by the sucrose stretching of viscosity, shearing stripping
Mixture；
(4) mixture of Graphene/sucrose step (3) obtained obtains graphite through deionized water cleaning 10 times, evaporation drying
Alkene presoma.Through test, the 90% Graphene presoma radial dimension obtained in embodiment 3 is 150-200 μm, 90% Graphene
Presoma thickness is 25-30 μm.
Embodiment 4
(1) using expansible graphite as raw material, expansible graphite powder body and excess dimethyl sulfoxide are placed in containing polyvinyl pyrrole
In the deionized water of alkanone, expansible graphite powder body and dimethyl sulfoxide, the described deionized water three containing polyvinylpyrrolidone
The mass ratio of person is 1:2:15, polyvinylpyrrolidone and the weight of deionized water in the deionized water containing polyvinylpyrrolidone
The ratio of amount is 1:150, is then stirred mixed solution, and arranging mixing speed is 300rpm, and stirring mixed solution is to raw material
After being uniformly distributed, mixed solution being carried out supersound process, arranging ultrasonic power is 200KW, and supersound process 2 hours is infiltrated
Aquadag powder dispersion liquid；
(2) being centrifuged the expansible graphite powder dispersion liquid of infiltration processing, the rotating speed of centrifugal treating is 500rpm, disengaging time
It is 40 minutes, is then filtrated to get moistening expansible graphite powder, moistening expansible graphite powder is stirred with maltose granule
Being blended, moistening graphite powder is 1:4 with the mass ratio of maltose granule, obtains aquadag powder/maltose mixture；
(3), during aquadag powder/maltose mixture adds banbury, the sweet sweetening process of banbury banbury is set for first to arrange
80 DEG C, 10r/min banburying 40min, be then warming up to 950 DEG C, 20r/min banburying 50min, and finally heat up 115 DEG C, 30r/
Min banburying 60min, makes sucrose melt and increases its mobility and viscosity, by shearing and the stretching of banbury, makes graphite
Under melted sucrose bonding effect, indirectly obtained presoma obtain Graphene/maltose by the sucrose stretching of viscosity, shearing stripping
Mixture；
(4) mixture of Graphene/sucrose step (3) obtained obtains Graphene through deionized water cleaning 3 times, spray drying
Presoma.Through test, the 90% Graphene presoma radial dimension obtained in embodiment 4 is 290-400 μm, before 90% Graphene
Driving body thickness is 25-35 μm.
Embodiment 5
(1) using expansible graphite as raw material, expansible graphite powder body and excess dimethyl sulfoxide are placed in containing polyvinyl pyrrole
In the deionized water of alkanone, expansible graphite powder body and dimethyl sulfoxide, the described deionized water three containing polyvinylpyrrolidone
The mass ratio of person is 1:2:20, polyvinylpyrrolidone and the weight of deionized water in the deionized water containing polyvinylpyrrolidone
The ratio of amount is 1:150, is then stirred mixed solution, and arranging mixing speed is 300rpm, and stirring mixed solution is to raw material
After being uniformly distributed, mixed solution being carried out supersound process, arranging ultrasonic power is 200KW, and supersound process 2 hours is infiltrated
Aquadag powder dispersion liquid；
(2) being centrifuged the expansible graphite powder dispersion liquid of infiltration processing, the rotating speed of centrifugal treating is 1500rpm, during separation
Between be 30 minutes, be then filtrated to get moistening expansible graphite powder, moistening expansible graphite powder stirred with maltose granule
Mixing blended, moistening graphite powder is 1:4 with the mass ratio of maltose granule, obtains aquadag powder/maltose mixture；
(3), during aquadag powder/maltose mixture adds banbury, the sweet sweetening process of banbury banbury is set for first to arrange
120 DEG C, 10r/min banburying 40min, be then warming up to 180 DEG C, 20r/min banburying 40min, be finally cooled to 115 DEG C,
30r/min banburying 40min, makes sucrose melt and increases its mobility and regulate its viscosity, by the shearing of banbury and
Stretching, makes graphite under melted sucrose bonding effect, is indirectly obtained presoma obtain stone by the sucrose stretching of viscosity, shearing stripping
The mixture of ink alkene/maltose；
(4) mixture of Graphene/sucrose step (3) obtained obtains Graphene through deionized water cleaning 8 times, spray drying
Presoma.Through test, the 90% Graphene presoma radial dimension obtained in embodiment 5 is 350-500 μm, before 90% Graphene
Driving body thickness is 20-30 μm.
Claims (9)
1. the method that Graphene presoma is prepared in a banbury stripping, it is characterised in that described method comprises the steps:
(1) using graphite powder as raw material, described raw material and excess intercalator are placed in the deionized water containing dispersant, described
Raw material is 1:(0.8-2 with described excess intercalator, the mass ratio of the described deionized water three containing dispersant): (5-20),
Stirring mixed solution is uniformly distributed to raw material, and described mixed solution is carried out supersound process, and arranging ultrasonic power is 10-200KW,
Supersound process 2-30 hour, obtains the graphite powder dispersion liquid of infiltration；
(2) the graphite powder dispersion liquid of infiltration is centrifuged process, be filtrated to get moistening graphite powder, by moistening graphite powder with
Glucide blended under agitation, described moistening graphite powder is 1:4-20 with the mass ratio of glucide, obtains graphite powder/sugar mixing
Thing；
(3) graphite powder/sugar mixture is added in banbury, banbury technique is set, by shearing and the stretching of banbury, makes
Graphite is glued in jelly, stretches, shears and peel off the mixture obtaining Graphene/sugar；
(4) mixture of Graphene/sugar step (3) obtained is before deionized water cleans 3-10 time, is dried to obtain Graphene
Drive body.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that described
Graphite powder is at least in natural flake graphite, aquadag, expansible graphite, highly oriented graphite, thermal cracking graphite composite powder
Kind.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that described
Intercalator is at least one in acrylamide, Methanamide, potassium acetate, dimethyl sulfoxide, carbamide, ethylenediamine, dimethyl sulfoxide.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that described
Glucide is at least one in sucrose, glucose, fructose, maltose.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that described
In deionized water containing dispersant, dispersant is 1:100-150 with the weight ratio of deionized water, and described dispersant is 12
At least one in alkyl sodium sulfate, dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, 1-pyridine acid.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that step
(1) mixing speed of mixed solution described in is 10-300rpm, and described in step (2), the rotating speed of centrifugal treating is 100-
1500rpm, disengaging time is 30-60 minute.
A kind of method utilizing banbury shearing stripping to prepare Graphene presoma the most according to claim 1, its feature
Being, the banburying process of described banbury is 80-180 DEG C, 10r/min, 95-200 DEG C, 20r/min, 115-250 DEG C, 30r/
Each banburying 40-60min in the case of min.
The method that Graphene presoma is prepared in a kind of banbury stripping the most according to claim 1, it is characterised in that described
Be dried as evaporation drying or spray drying.
9. a Graphene presoma, it is characterised in that described Graphene presoma is by described in claim arbitrary in claim 1-7
A kind of preparation method prepare Graphene presoma.
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| CN107418206A (en) * | 2017-05-25 | 2017-12-01 | 成都新柯力化工科技有限公司 | A kind of high dispersive graphene heat conduction masterbatch and preparation method |
| CN114763261A (en) * | 2021-01-14 | 2022-07-19 | 中国科学院大连化学物理研究所 | Method for preparing graphene material and graphene material obtained by method |
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