CN105776192B - A kind of method for continuous preparation graphene microchip of being delaminated using grinding - Google Patents
A kind of method for continuous preparation graphene microchip of being delaminated using grinding Download PDFInfo
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- CN105776192B CN105776192B CN201610106332.7A CN201610106332A CN105776192B CN 105776192 B CN105776192 B CN 105776192B CN 201610106332 A CN201610106332 A CN 201610106332A CN 105776192 B CN105776192 B CN 105776192B
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Abstract
The invention belongs to technical field of graphene, the method for more particularly to a kind of continuous preparation graphene microchip of being delaminated using grinding.Crystallization organic matter is dispersed in graphite presoma by the way that solvent is scattered, the deformation power produced using the repeated crystallization for crystallizing organic matter makes the distance increase of graphite layer frame, form intercalated graphite, by intercalated graphite feeding grinding machine for cutting charge into pieces, the stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, intercalated graphite is set to peel off to form graphene microchip, screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out to the graphene microchip for re-starting stripping, being evenly distributed.The graphene microchip number of plies prepared by the inventive method is 10 ~ 100 layers, and crystal structure is complete, efficient, low cost, continuous production high-quality graphene microplate, and preparation process environmental protection under high shear conditions. is realized, with significant market value.
Description
Technical field
The invention belongs to technical field of graphene, it is related to a kind of method that mechanical stripping prepares graphene, more particularly to one
Plant the method for utilizing grinding to delaminate continuous preparation graphene microchip.
Background technology
Graphene is a kind of single layer of carbon atom facestock material separated from graphite material, is with sp2 hydridization by carbon atom
The two-dimensional material of the cellular hexaplanar structure formed.Since two scientists of Univ Manchester UK in 2004 are used
Since " adhesive tape " mechanical stripping finds graphene, scientific circles and industrial quarters focus of attention are just turned into.Graphene is most thin at present
It is also most hard nano material, with good electricity-optics performance, mechanical property, heat-conductive characteristic and high electricity
Charge carrier mobilities, while the performance that also numerous common materials such as stronger mechanical strength and pliability do not possess, in energy
The numerous areas such as source, electronic material, biomedicine and environmental protection have potential application prospect.
However, limit very big the shortcomings of the expensive of grapheme material, low yield, poor ductility, cumbersome preparation process
Its application in actual industrial is made.Graphene microchip generally refers to carbon-coating number more than 10 layers, thickness in 5-100 nanometer ranges
Interior ultra-thin graphene stratiform accumulation body.Graphene microchip maintains the original planar carbon hexatomic ring conjugation crystal knot of graphite
Structure, the shape ratio (diameter/thickness ratio) with super large, and with nano thickness, therefore with excellent mechanical strength, conduction,
Heat conductivility and good lubrication, high temperature resistant and anticorrosion properties etc..This cause graphene microchip as additive with it is other
Material cladding formation composite, not only can put forward the performances such as intensity, hardness, corrosion-resistant, lubricity, the heat conduction of base material
Rise, and it can be made to possess excellent conduction, antistatic property, so as to obtain the composite of excellent performance.
The preparation method of current graphene microchip includes ball-milling method, ultrasonic method, high-temperature expansion stripping method, oxidation-reduction method
Deng.Such as China Patent Publication No. CN103601179A discloses the preparation method of the controllable graphene microchip of size, with big particle diameter
Expansible graphite is preparation highly expanded multiplying power expanded graphite under raw material, high temperature, using organic matter as intercalation thing, blending insertion expansion stone
In ink sheet layer, expanded graphite/organic matter composite is prepared, certain size size is ground into using pulverizer, high-temp combustion is swollen
It is swollen to peel off the graphene microchip for obtaining certain size.But graphene is prepared using high-temperature expansion stripping, condition is harsh, to equipment
It is required that high, it is impossible to continuous production, the large-scale production of graphene microchip is restricted.
China Patent Publication No. CN103803533A discloses a kind of preparation method of graphene, by expanded graphite and organic
Solvent mixing carries out ultrasound dissociation and obtains graphene microchip suspension, stands 0.2-5 hours, removes upper strata suspension, removes precipitation
Thing, drying obtains graphene microchip in 80 degree of baking ovens after filtering.The method peeled off using ultrasound prepares graphene microchip, is not required to
To pass through oxidation-reduction process, the lattice structure of prepared graphene is not destroyed, products obtained therefrom quality is high, but ultrasonic stripping method is needed
Substantial amounts of organic solvent is used, environment is polluted, and obtained graphene is difficult to purifies and separates, ultrasonic time is long, is unfavorable for rule
Modelling is produced.
China Patent Publication No. CN 104709900A disclose the preparation method of nano-graphene piece, by graphite material with
Intercalator and oxidant carry out intercalation oxidation and form graphite oxide, and it is nanometer to peel off graphite oxide by high-temperature heating
Graphite chip architecture, is suspended in liquid, imposes the mechanical shear stress more than 5000psi, reduction nano-graphite chip architecture
Lateral dimension and thickness, form nano-graphene piece suspension, dry and isolate nano-graphene piece, and heating reduction obtains graphite
Alkene piece.Graphene film is prepared using redox method, the structure of graphene can be destroyed, its performance, and production process is influenceed
In need to use substantial amounts of chemical reagent, energy consumption is big and pollution environment.
In summary, the preparation method of current graphene microchip be limited to each side such as production cost and properties of product because
Element, still without industrial applications.Therefore given birth in the urgent need to developing a kind of high efficiency, low cost, the graphene microchip of high product performance
Production method.
The content of the invention
The present invention proposes a kind of to delaminate continuous prepare using grinding for the demand of current burgeoning graphene microchip
The method of graphene microchip.The deformation power produced using the repeated crystallization for crystallizing organic matter makes the distance increase of graphite layer frame, is formed
Intercalated graphite, by intercalated graphite feeding grinding machine for cutting charge into pieces, the stripping of the shearing force formed using medium with the mutual friction of graphite material phase
Mill is acted on, and makes intercalated graphite peel off to form graphene microchip, and screening sorting is carried out to the graphite of stripping by vibrating screen classifier, will
Unstripped graphite, which is filtered out, re-starts stripping, the graphene microchip being evenly distributed.Graphite prepared by the inventive method
The alkene microplate number of plies is 10 ~ 100 layers, and crystal structure is complete, and product quality is high, realizes continuous production under high shear mechanical condition
High-quality graphene microplate, available for anticorrosive paint, improves pliability, wearability and the rustless property of coating.
To achieve the above object, the present invention is adopted the following technical scheme that:
A kind of utilize grinds the method that machine for cutting charge into pieces stripping prepares graphene, it is characterised in that the repetition for passing through organic matter is crystallized
Increase the interlamellar spacing of graphite, the shearing force the to be formed stripping graphite acquisition number of plies of delaminating is micro- for 10 ~ 100 layers of graphene using grinding
Piece, specific method is as follows:
(1)It is 2 ~ 3 in mass ratio by expanded graphite and organic polymer:1 mixing sends into Screw Extrusion as carbon material
Machine carries out extruding carbonization, is passed through reducibility gas, and it is 300 ~ 500 DEG C to set carburizing temperature, organic polymer is carbonized, with expansion
Graphite is mixed to form graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:1 ~ 10, at ambient temperature
15 ~ 30min mixing is stirred, surfactant is added and continues to stir 10 ~ 20min, graphite presoma is dispersed in ethanol water
In solution;
(3)It is 0.1 ~ 0.15 to add with graphite forerunner body mass ratio:1 crystallization organic matter, stirring mixing makes crystallization organic
Matter is dispersed in the layer structure of graphite presoma, is heated to 40 ~ 80 DEG C, solvent evaporative crystallization organic matter is with crystal form
Separate out, continuously add ethanol water, crystallization organic matter is dissolved again, reheat and separate out, so repeatedly 2 ~ 3 times, graphite linings
Between gradually increase with the solid-liquid transformation of organic matter, obtain intercalated graphite;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm,
The stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, peeling off intercalated graphite, to form graphene micro-
Piece;Screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out and re-starts stripping, is obtained
To the graphene microchip head product being evenly distributed;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively,
Dissolution is carried out, cleans, filter, being dried to obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Described organic polymer is any one in polyvinyl alcohol, polyethylene glycol, PLA, polyacrylic acid.
Described crystallization organic matter is any one in arginine, theanine, glutamine.
Described surfactant is tetramethyl ammonium hydrogen carbonate, dodecyl tetramethyl guanidine carbonate, cetyl trimethyl
Any one in ammonium bromide, cetyl benzenesulfonic acid sodium.
Described step(2)Described ethanol water is ethanol and water is 1 by volume:1 ~ 2 solution prepared.
The agitator of described grinding machine for cutting charge into pieces is to be carved with the equally distributed circulation port of at least four on multi-layer discs, disk,
Disk border is uniformly distributed 4 lead angles, when agitator drives graphite material to rotate, because of differential relation, medium and graphite material
Phase mutual friction forms the stripping mill effect based on shearing force, realizes effective dissociation of lamellar graphite, makes graphite peel off to form distribution
Uniform graphene microchip;Connection vibrating screen classifier immediately below described grinding machine for cutting charge into pieces, is carried out to the graphite not being completely exfoliated
Sorting, classification, are delaminated repeatedly to the graphene film not up to required.
A kind of method for continuous preparation graphene microchip of being delaminated using grinding of the present invention, graphite is passed through with organic polymer
Screw rod shearing is carbonized to form graphene presoma, and graphene presoma is dispersed in by the scattered organic matter that will crystallize of solvent
In, the organic matter for being interspersed in graphite layers is separated out with crystal form by heating crystalline, heating crystalline is dissolved repeatedly, by having
The force attenuation graphite layers power that the repeated deformation of machine matter is produced, makes graphite layers distance increase, beneficial to the stripping of graphite.Shape
Into intercalated graphite, by intercalated graphite feeding grinding machine for cutting charge into pieces, the shearing force formed using medium with the mutual friction of graphite material phase
Mill effect is shelled, makes intercalated graphite peel off to form graphene microchip, screening sorting is carried out to the graphite of stripping by vibrating screen classifier,
Unstripped graphite is filtered out to the graphene microchip for re-starting stripping, being evenly distributed.The present invention is delaminated using grinding
The graphene microchip continuously prepared, the number of plies is evenly distributed, and yield is high, and cost is low, is suitable for anticorrosive paint, makes the flexible of coating
Property, the lifting such as wearability, corrosion-resistant, rustless property, promote large-scale application of the graphene microchip in anticorrosive paint.The present invention
The main performance advantage of the graphene microchip of preparation such as table 1.
Index name | Radial dimension | Thickness | Yield | Cost |
Index performance | 5~10μm | 10 ~ 100 layers | 150~250kg/h | 0.2 ~ 0.6 yuan/g |
A kind of method for continuously preparing graphene microchip of being delaminated using grinding of the present invention, is protruded compared with prior art
The characteristics of and beneficial effect be:
1st, graphite layers are increased away from acquisition intercalated graphite utilizes the efficient of graphite by crystallizing the repeated crystallization of organic matter
Peel off.
2nd, shearing stripping is carried out to intercalated graphite by the delaminate shear action of generation of grinding, it is to avoid graphene layer structure
Damage;Unstripped graphite is subjected to screening separation using vibrosieve, peels off again, improves the charge stripping efficiency of graphite.
3rd, invention preparation method puts into low small, cost, non-environmental-pollution, can fast and efficiently prepare graphene microchip,
It is advantageously implemented the continuous large-scale production of high-quality graphene microplate.
Embodiment
The present invention is explained in detail below in conjunction with embodiment, the present invention is not restricted to.Do not departing from
In the case of above method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change
Enter, should be included in the scope of the protection.
Embodiment 1
(1)It is 3 in mass ratio by expanded graphite and polyvinyl alcohol:1 mixing is entered as carbon material, feeding screw extruder
Row extruding carbonization, is passed through reducibility gas, it is 500 DEG C to set carburizing temperature, polyvinyl alcohol is carbonized, shape is mixed with expanded graphite
Into graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:10, stir at ambient temperature
15 ~ 30min mixing is mixed, tetramethyl ammonium hydrogen carbonate is added and continues to stir 10 ~ 20min, graphite presoma is dispersed in ethanol
In the aqueous solution;
(3)It is 0.1 to add with graphite forerunner body mass ratio:1 arginine, stirring mixing makes crystallization organic matter dispersed
In the layer structure of graphite presoma, 40 ~ 80 DEG C are heated to, solvent evaporative crystallization organic matter is separated out with crystal form, continued
Ethanol water is added, crystallization organic matter is dissolved again, reheats and separates out, so repeatedly 2 ~ 3 times, graphite layers are with organic
The solid-liquid transformation of matter gradually increases, and obtains intercalated graphite;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm,
The stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, peeling off intercalated graphite, to form graphene micro-
Piece;Screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out and re-starts stripping, is obtained
To the graphene microchip head product being evenly distributed;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively,
Dissolution is carried out, cleans, filter, being dried to obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 2
(1)It is 2 in mass ratio by expanded graphite and polyethylene glycol:1 mixing is entered as carbon material, feeding screw extruder
Row extruding carbonization, is passed through reducibility gas, it is 300 DEG C to set carburizing temperature, organic polymer is carbonized, is mixed with expanded graphite
Form graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:8, stir at ambient temperature
15 ~ 30min mixing is mixed, dodecyl tetramethyl guanidine carbonate is added and continues to stir 10 ~ 20min, make graphite presoma dispersed
In ethanol water;
(3)It is 0.15 to add with graphite forerunner body mass ratio:1 theanine, stirring mixing makes crystallization organic matter uniformly divide
In the layer structure for being dispersed in graphite presoma, 40 ~ 80 DEG C are heated to, solvent evaporative crystallization organic matter is separated out with crystal form, after
It is continuous to add ethanol water, crystallization organic matter is dissolved again, reheat and separate out, so repeatedly 2 ~ 3 times, graphite layers are with having
The solid-liquid transformation of machine matter gradually increases, and obtains intercalated graphite;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm,
The stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, peeling off intercalated graphite, to form graphene micro-
Piece;Screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out and re-starts stripping, is obtained
To the graphene microchip head product being evenly distributed;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively,
Dissolution is carried out, cleans, filter, being dried to obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 3
(1)It is 2 in mass ratio by expanded graphite and PLA:1 mixing is carried out as carbon material, feeding screw extruder
Extruding carbonization, is passed through reducibility gas, and it is 500 DEG C to set carburizing temperature, organic polymer is carbonized, shape is mixed with expanded graphite
Into graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:5, stir at ambient temperature
15 ~ 30min mixing is mixed, cetyl trimethylammonium bromide is added and continues to stir 10 ~ 20min, make graphite presoma dispersed
In ethanol water;
(3)It is 0.12 to add with graphite forerunner body mass ratio:1 glutamine, stirring mixing makes crystallization organic matter uniform
In the layer structure for being dispersed in graphite presoma, 40 ~ 80 DEG C are heated to, solvent evaporative crystallization organic matter is separated out with crystal form,
Continuously add ethanol water, crystallization organic matter is dissolved again, reheat separate out, so repeatedly 2 ~ 3 times, graphite layers with
The solid-liquid transformation of organic matter gradually increases, and obtains intercalated graphite;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm,
The stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, peeling off intercalated graphite, to form graphene micro-
Piece;Screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out and re-starts stripping, is obtained
To the graphene microchip head product being evenly distributed;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively,
Dissolution is carried out, cleans, filter, being dried to obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 4
(1)It is 3 in mass ratio by expanded graphite and polyacrylic acid:1 mixing is entered as carbon material, feeding screw extruder
Row extruding carbonization, is passed through reducibility gas, it is 400 DEG C to set carburizing temperature, organic polymer is carbonized, is mixed with expanded graphite
Form graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:5, stir at ambient temperature
15 ~ 30min mixing is mixed, cetyl benzenesulfonic acid sodium is added and continues to stir 10 ~ 20min, graphite presoma is dispersed in second
In alcohol solution;
(3)It is 0.1 to add with graphite forerunner body mass ratio:1 glutamine, stirring mixing makes crystallization organic matter uniformly divide
In the layer structure for being dispersed in graphite presoma, 40 ~ 80 DEG C are heated to, solvent evaporative crystallization organic matter is separated out with crystal form, after
It is continuous to add ethanol water, crystallization organic matter is dissolved again, reheat and separate out, so repeatedly 2 ~ 3 times, graphite layers are with having
The solid-liquid transformation of machine matter gradually increases, and obtains intercalated graphite;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm,
The stripping mill effect of the shearing force formed using medium with the mutual friction of graphite material phase, peeling off intercalated graphite, to form graphene micro-
Piece;Screening sorting is carried out to the graphite of stripping by vibrating screen classifier, unstripped graphite is filtered out and re-starts stripping, is obtained
To the graphene microchip head product being evenly distributed;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively,
Dissolution is carried out, cleans, filter, being dried to obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Claims (6)
1. a kind of method for continuous preparation graphene microchip of being delaminated using grinding, it is characterised in that the repetition for passing through organic matter is crystallized
Increase the interlamellar spacing of graphite, the shearing force the to be formed stripping graphite acquisition number of plies of delaminating is micro- for 10 ~ 100 layers of graphene using grinding
Piece, specific method is as follows:
(1)It is 2 ~ 3 in mass ratio by expanded graphite and organic polymer:1 mixing is carried out as carbon material, feeding screw extruder
Extruding carbonization, is passed through reducibility gas, and it is 300 ~ 500 DEG C to set carburizing temperature, organic polymer is carbonized, mixed with expanded graphite
Conjunction forms graphene presoma;
(2)By step(1)In graphene presoma and ethanol water in mass ratio be 1:1 ~ 10, stir at ambient temperature
15 ~ 30min is mixed, and is added surfactant and is continued to stir 10 ~ 20min, graphene presoma is dispersed in ethanol water-soluble
In liquid;
(3)It is 0.1 ~ 0.15 to add with graphene forerunner body mass ratio:1 crystallization organic matter, stirring mixing makes crystallization organic matter
In the layer structure for being dispersed in graphene presoma, 40 ~ 80 DEG C are heated to, solvent evaporative crystallization organic matter is with crystal form
Separate out, continuously add ethanol water, crystallization organic matter is dissolved again, reheat and separate out, so repeatedly 2 ~ 3 times, graphite linings
Between gradually increase with the solid-liquid transformation of organic matter, obtain intercalated graphite;Described crystallization organic matter be arginine, theanine,
Any one in glutamine;
(4)By step(3)Obtained intercalated graphite is added in grinding machine for cutting charge into pieces, and setting mixing speed is 500 ~ 1000rpm, is utilized
The stripping mill effect for the shearing force that medium is formed with the mutual friction of graphite material phase, makes intercalated graphite peel off to form graphene microchip;It is logical
Cross vibrating screen classifier and screening sorting is carried out to the graphite of stripping, unstripped graphite is filtered out and re-starts stripping, is divided
The uniform graphene microchip head product of cloth;
(5)Collection step(4)In the graphene microchip head product that is collected into cleaned 2 ~ 3 times with water, ethanol, acetone respectively, carry out
Dissolution, to clean, filter, being dried to obtain the number of plies be 10 ~ 100 layers of graphene microchip;
The agitator of described grinding machine for cutting charge into pieces is to be carved with equally distributed circulation port on multi-layer discs, disk, and disk border is equal
4 lead angles of even distribution, when agitator drives graphite material to rotate, because of differential relation, medium and graphite material phase mutual friction shape
Into the stripping mill effect based on shearing force, effective dissociation of lamellar graphite is realized, graphite is peeled off the graphite to be formed and be evenly distributed
Alkene microplate;
Connection vibrating screen classifier, is sorted to the graphite not being completely exfoliated, is classified, to not immediately below described grinding machine for cutting charge into pieces
Reach that the graphene film of requirement is delaminated repeatedly.
2. a kind of method of continuous preparation graphene microchip of being delaminated using grinding according to claim 1, it is characterised in that
Described organic polymer is any one in polyvinyl alcohol, polyethylene glycol, PLA, polyacrylic acid.
3. a kind of method of continuous preparation graphene microchip of being delaminated using grinding according to claim 1, it is characterised in that
Step(2)Described ethanol water is ethanol and water is 1 by volume:1 ~ 2 solution prepared.
4. a kind of method of continuous preparation graphene microchip of being delaminated using grinding according to claim 1, it is characterised in that
Described surfactant is tetramethyl ammonium hydrogen carbonate, dodecyl tetramethyl guanidine carbonate, cetyl trimethylammonium bromide, ten
Any one in six sodium alkyl benzene sulfonates.
5. a kind of method of continuous preparation graphene microchip of being delaminated using grinding according to claim 1, it is characterised in that
The equally distributed circulation port of at least four is carved with the disk of described grinding machine for cutting charge into pieces.
6. a kind of method of continuous preparation graphene microchip of being delaminated using grinding according to claim 1, it is characterised in that
Described graphene microchip is used for anticorrosive paint.
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CN106744876A (en) * | 2016-12-21 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that utilization multi-level cone type kneading machine prepares grapheme material |
CN106908463B (en) * | 2017-03-09 | 2019-04-16 | 成都新柯力化工科技有限公司 | A method of it is distributed using scanning electron microscope detection graphene microchip layer |
CN107892294A (en) * | 2017-12-31 | 2018-04-10 | 周思齐 | The method and apparatus that high purity graphite rod produces graphene |
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