CN106744879A - A kind of application of the method and Graphene that Graphene is peeled off based on draft flowing deformation - Google Patents

A kind of application of the method and Graphene that Graphene is peeled off based on draft flowing deformation Download PDF

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CN106744879A
CN106744879A CN201611206711.XA CN201611206711A CN106744879A CN 106744879 A CN106744879 A CN 106744879A CN 201611206711 A CN201611206711 A CN 201611206711A CN 106744879 A CN106744879 A CN 106744879A
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graphene
graphite
stretching
paste
machine barrel
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CN106744879B (en
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陈庆
曾军堂
王镭迪
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Donggang Zhike Industrial Park Co ltd
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Chengdu New Keli Chemical Science Co Ltd
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    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/04Specific amount of layers or specific thickness
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
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Abstract

The present invention proposes a kind of application of the method and Graphene that Graphene is peeled off based on draft flowing deformation, by in the drawing mechanism that graphite and stickum are added designed, designed together, the chamber volume in machine barrel is set back and forth to reduce increase in the running using the cam follower in cavity, by graphite and stickum by cam and the reciprocating compression of reed in chamber, stretching, graphite mixture is under the bonding effect of viscosity additives, stretched by the additive of viscosity indirectly, shearing stripping obtains Graphene presoma, effectively prevent the crystal lattice damage that excessive shearing force is caused to Graphene.Scheme preparation process is simple disclosed by the invention, extensively, pollution-free, low cost, the quality of graphene prepared is high for raw material sources, and easily storage is transported, it is easy to accomplish scale industrial production.

Description

A kind of application of the method and Graphene that Graphene is peeled off based on draft flowing deformation
Technical field
The present invention relates to material processing field, and in particular to a kind of method and graphite that Graphene is peeled off based on draft flowing deformation The application of alkene.
Background technology
The plane carbon nanomaterial that Graphene is made up of one layer of carbon atom, is to be currently known most thin two-dimensional material, its Thickness is only 0.335nm, and it is made up of the lattice of six sides.It is bonded by σ between carbon atom in Graphene and is connect, imparts Graphene Extremely excellent mechanical property and structural rigidity.And, in Graphene, each carbon atom has a p electronics for non-bonding, These p electronics can be moved freely in crystal, and movement velocity is up to the 1/300 of the light velocity, impart that Graphene is good to lead Electrically.In optics aspect, Graphene is almost fully transparent, only absorbs 2.3% light.Graphene has peculiar mechanics, light Learn and electrical properties, Graphene possesses very vast potential for future development.
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, however low yield, it is high to substrate requirement, turn Move and there is greatly difficulty;Oxidation intercalation restores method and can realize producing Graphene in batches, but due to stone in oxidizing process The structure of black alkene is destroyed, it is difficult to obtain high-quality graphene product;Liquid phase stripping method is in a suitable solvent, to utilize Ultrasonic energy dissociates to graphite flake layer, however, solvent stripping method prepares Graphene presence to be difficult to remove asking for residual solvent Topic, and solvent stripping yield is general very low.By contrast, to be that one kind can be prepared with low cost high-quality for mechanical-physical stripping method Measure the method simple and easy to apply of Graphene.
Mechanical-physical stripping method prepares Graphene method simply, and preparation process is environment friendly and pollution-free, and production cost is more cheap, Favor is enjoyed in the industrial production.In order that graphite layers are peeling-off, the conventional stripping means of mechanical-physical stripping method have often Rule ball milling, stirring ball-milling, grinding etc..
Chinese invention patent application number 201410286173.4 discloses a kind of preparation method of Graphene, by graphite oxide Fractionlet is broken into the mode of mechanical shearing or ball milling, grinding stripping by airflow collision obtains Graphene.The invention is based on Fractionlet graphite oxide under low hydrogen concentration and low temperature reduction and stripping, there is provided it is prepared by a kind of safety, inexpensive hydrogen reduction The method of Graphene.But the collsion damage of this strength Rotating fields of Graphene, and the Graphene dimensioned area for obtaining is small.
Chinese invention patent application number 201280019582.7 discloses a kind of method for preparing Graphene, by grinding, Ball milling, airflow milling etc. grind 4 hours acquisition Graphenes by ionic liquid.The stripping of graphite is promoted by ionic liquid, but The Graphene crystalline size obtained using prolonged grinding is small, and by ionic liquid graphene layer lattice can be made to be subject to shadow Ring.
Due to grinding to graphite part applying pressure, to the graphite peeled off in the methods such as conventional ball mill, stirring ball-milling, grinding Producing huge impulsive force, this impulsive force can make graphene layer produce fault of construction, easily cause graphene layer structural lattice Defect, reduces the size of Graphene after peeling off so that obtained graphene product crystalline size is small, it is difficult to obtain large-size high-quality Amount Graphene;In addition, the crunch of abrasive media can cause the pinch shock to cause overlapping again for Graphene, can cause on the contrary Peeling effect reduction, causes that milling time is long, cost is very high, it is difficult to carry out large-scale industrialized production.
Stretching-machine is a kind of short with mixing time, and production efficiency is high, and operation is easy, reduces the loss of compounding ingredient, is improved The production equipment of the advantages of working condition, is widely used in the development & production of new material, different from conventional ball mill, stirring ball The methods such as mill, grinding, can also be used for preparing Graphene using stretching-machine.At present, China Patent Publication No. 105948028A is disclosed A kind of stretching-machine stripping prepares the method and Graphene presoma of Graphene presoma, by by graphite in excessive intercalator In aqueous dispersions after the treatment of infiltration for a long time, using glucide for bonding peels off carrier, by the shearing and stretching of stretching-machine Sticky glucide, makes graphite under the bonding effect of glucide, is peeled off by the glucide stretching of viscosity, shearing indirectly To Graphene presoma.But the stretcher structure in scheme does not have particularity, main stripping for bonding using glucide is carried Body, the Graphene dimensional homogeneity and charge stripping efficiency for peeling off acquisition is limited.
The content of the invention
For in the prior art with stretching-machine Graphene dimensional homogeneity and the limited technological deficiency of charge stripping efficiency, this hair It is bright propose it is a kind of based on draft flowing deformation peel off Graphene method and Graphene application, by by graphite and stickum together A kind of addition stretch release of designed, designed is prepared in the drawing mechanism of Graphene, is made in the running using the cam follower in cavity Chamber volume in machine barrel back and forth reduces increase, in chamber by graphite and stickum by the reciprocating compression of cam and reed, Stretching, graphite mixture obtains stone by the additive stretching of viscosity, shearing stripping indirectly under the bonding effect of viscosity additives Black alkene presoma, effectively prevent the crystal lattice damage that excessive shearing force is caused to Graphene.The stretching cam follower of special construction, Improve using stretching mechanism for Graphene quality and raising Graphene charge stripping efficiency.
To solve the above problems, the present invention uses following technical scheme:
On the one hand a kind of method that Graphene is peeled off based on draft flowing deformation is provided, it is characterised in that comprise the following steps:
(1)By graphite raw material, plasticity thing and solvent according to mass ratio be 1:5-10:2-5 mixing and stirrings, are configured to sticky cream Shape graphite mixture;
(2)The paste graphite mixture is put into drawing mechanism, power drive mechanism is connected, it is 50-80 to control operating temperature DEG C, setting rotating speed is 500-1000r/min, and during the central shaft is continued through, the cam described in rotation process turns The eccentric rotational motion of son, periodically compression and stretching cavity space, the paste graphite mixture are constantly compressed and are drawn Stretch, graphite is stripped into Graphene in drawing process, Graphene is collected by collecting mechanism.
Wherein, the graphite raw material is in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide At least one, the graphite raw material particle diameter be less than or equal to 1 millimeter;The plasticity thing is the EVA hot-melt adhesive with adhesivity, PA PUR, PES polyester hot-melt adhesives, PE polyethylene hot-melt adhesives, Water-Soluble Glucose, fructose, galactolipin, sorbose, Tagatose, flesh At least one in alcohol, mannose, the solvent is at least one in methyl alcohol, ethanol, isopropanol, normal propyl alcohol, deionized water.
Preferably, the graphite raw material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide In at least one, the graphite raw material particle diameter be less than or equal to 10 millimeters;
The plasticity thing is the EVA hot-melt adhesive with adhesivity, PA PURs, PE PURs, glucose, fructose, galactolipin, mountain At least one in pears sugar, Tagatose, inositol, mannose.
The solvent is at least one in methyl alcohol, ethanol, isopropanol, normal propyl alcohol, deionized water.
Preferably, the drawing mechanism includes:
Machine barrel, inside sets a temperature regulating device;
Charging mechanism, is arranged on the machine barrel, is made up of at least one spout;
Draft flowing deformation mechanism, is connected with the charging mechanism, including cross section is the cam follower not coaxial with machine barrel, can stretch The spring reed of compression deformation;
Power drive mechanism, including a motor, conducting central shaft is connected with the draft flowing deformation mechanism, described for driving Central shaft;
Collecting mechanism, is arranged on the machine barrel, is made up of at least one discharging opening, for collecting Graphene presoma;
Wherein, the paste graphite mixture for graphite raw material, plasticity thing and solvent being mixed adds the charging mechanism laggard Enter the drawing mechanism, during the central shaft is continued through, made the chamber in machine barrel in the running by the cam follower Building volume back and forth reduces increase, due to paste have viscosity, by chamber by the reciprocating compression of cam and reed, stretching, Make graphite that Graphene is stripped into drawing process, it is to avoid the damage that extrusion shearing is caused to Graphene, produce compression stress And tensile force, the paste graphite mixture is constantly compressed and is stretched, graphite is stripped into Graphene in drawing process.
Preferably, the barrel diameter of the drawing mechanism is 800-1100mm.
Preferably, under motor driving, wherein the cam follower direction pivots clockwise or counter-clockwise is eccentric Rotation, the chamber volume in machine barrel periodically reduces increase in the running, and the paste is in chamber by cam and reed Periodically compression, stretching, make the graphite Graphene is stripped into drawing process, it is to avoid extrusion shearing is made to Graphene Into damage, produce compression stress and tensile force, the paste graphite mixture is constantly compressed and is stretched, in drawing process Graphite is stripped into Graphene.
Preferably, the cam follower does the rotary motion of bias along central shaft.
Preferably, the cam follower surface covering wear-resistant ceramic layer or wear-resistant plastic layer.
Preferably, the collecting mechanism inside sets heating arrangements, continues directly to heat paste, moulding treatment.
On the other hand the present invention provides a kind of Graphene rubber, it is characterised in that include:Plastic rubber, above-mentioned side Graphene prepared by method, Graphene accounts for weight ratio for 0.005 ~ 0.02wt%, is uniformly distributed in the plastic rubber, solidify afterwards Obtain Graphene rubber.
Stretcher structure in existing scheme does not have particularity, and main is bonding stripping carrier, stripping using glucide It is limited from the Graphene dimensional homogeneity and charge stripping efficiency for obtaining.In consideration of it, the present invention proposes one kind based on draft flowing deformation stripping From the application of the method and Graphene of Graphene, by the drawing mechanism that graphite and stickum are added designed, designed together In, the chamber volume in machine barrel is back and forth reduced increase in the running using the cam follower in cavity, by graphite in chamber With stickum by the reciprocating compression of cam and reed, stretching, graphite mixture under the bonding effect of viscosity additives, indirectly Graphene presoma is obtained by the additive stretching of viscosity, shearing stripping, excessive shearing force is effectively prevent and Graphene is caused Crystal lattice damage.The stretching cam follower of special construction, improves using stretching mechanism for Graphene quality and raising graphite Alkene charge stripping efficiency.Scheme preparation process is simple disclosed by the invention, raw material sources are extensive, pollution-free, low cost, before preparing Volume property stabilization is driven, easily storage is transported, it is easy to accomplish scale industrial production.
By Graphene performance prepared by the present invention compared with common stretcher prepares Graphene, in Graphene quality, produce The aspects such as amount have the advantage that as shown in table 1.
Table 1:
Project Index
90% graphene film radial dimension 15-17μm
90% Graphene thickness 0.9-1.6nm
Charge stripping efficiency 74.8%
A kind of application of the method and Graphene that Graphene is peeled off based on draft flowing deformation, compared with prior art, its spy for protruding Point and excellent effect are:
1st, the application of a kind of method and Graphene that Graphene is peeled off based on draft flowing deformation that the present invention is provided, by designed, designed A kind of stretch release is prepared in the drawing mechanism of Graphene, makes the chamber in machine barrel in the running using the cam follower in cavity Volume back and forth reduces increase, by graphite and stickum by the reciprocating compression of cam and reed, stretching, graphite mixing in chamber Thing obtains Graphene presoma by the additive stretching of viscosity, shearing stripping indirectly under the bonding effect of viscosity additives, has Effect avoids the crystal lattice damage that excessive shearing force is caused to Graphene.
2nd, this programme is prepared in the way of pure physics, it is to avoid destruction of the chemical reaction to graphene-structured, obtain Product quality it is higher, environment is polluted few.
3rd, scheme preparation process is simple disclosed by the invention, raw material sources are extensive, low cost, the forerunner's volume property prepared Stabilization, easily storage are transported, it is easy to accomplish scale industrial production.
Brief description of the drawings
For further clearly a kind of stretch release prepares the stretching-machine of Graphene, illustrated by accompanying drawing.
Accompanying drawing 1:A kind of stretch release prepares the structural representation of the stretching-machine of Graphene in the embodiment of the present invention;
Accompanying drawing 2:The schematic diagram in the section of rotor in the embodiment of the present invention.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as into the present invention Scope be only limitted to following example.In the case where above method thought of the present invention is not departed from, according to ordinary skill Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1)It is 1 according to mass ratio by crystalline flake graphite, glucose and water that graphite raw material particle diameter is 0.5 millimeter:5:2 mix Uniformly, it is configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into stretching-machine spout, the stretching-machine is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 50 DEG C to control operating temperature, and setting rotating speed is 500r/min, is continuing through the center During axle, the eccentric rotational motion of the cam follower described in rotation process, periodically compression and stretching cavity space, institute State paste graphite mixture constantly to be compressed and stretched, graphite is stripped into Graphene in drawing process, by collecting mechanism Collect Graphene.
As shown in Figure 1 and shown in Fig. 2, the stretching-machine includes machine barrel 10, and the inside of machine barrel 10 sets a temperature regulating device 11, control Warm device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes the real-time measurement temperature of a thermocouple and feeds back, to control thing Material processing temperature maintains certain interval.A diameter of 800mm of machine barrel 10.Charging mechanism 20, is arranged on machine barrel 10, by least One spout 21 is constituted;Drawing mechanism 30, is connected with charging mechanism 20, including cross section is eccentric cam follower conduct Central shaft 31, cam follower covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, connect with drawing mechanism 30 Conducting is connect, for driving central shaft 31.Collecting mechanism 50, inside sets constant temperature heating device, and the temperature for controlling heater is 250 DEG C, for collecting Graphene.Under motor driving, the cam follower moves in a circle around central shaft, the rotor Rotate one week, cavity volume volume is in cyclically-varying, under the reciprocating motion of two panels reed 32,33, the paste graphite mixture Constantly compressed and stretched, graphite is stripped into Graphene in drawing process.
The Graphene that will can be collected is added in plastic rubber, accounts for weight ratio for 0.005wt%, and the solidify afterwards that stir are obtained To Graphene rubber.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 2
(1)It is 1 according to mass ratio by expanded graphite, EVA hot-melt adhesive and methyl alcohol that graphite raw material particle diameter is 0.3 millimeter:6:3 mixing Stir, be configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into stretching-machine spout, the stretching-machine is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 60 DEG C to control operating temperature, and setting rotating speed is 700r/min, is continuing through the center During axle, the eccentric rotational motion of the cam follower described in rotation process, periodically compression and stretching cavity space, institute State paste graphite mixture constantly to be compressed and stretched, graphite is stripped into Graphene in drawing process, by collecting mechanism Collect Graphene.
As shown in Figure 1 and shown in Fig. 2, the stretching-machine includes machine barrel 10, and the inside of machine barrel 10 sets a temperature regulating device 11, control Warm device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes the real-time measurement temperature of a thermocouple and feeds back, to control thing Material processing temperature maintains certain interval.A diameter of 900mm of machine barrel 10.Charging mechanism 20, is arranged on machine barrel 10, by least One spout 21 is constituted;Drawing mechanism 30, is connected with charging mechanism 20, including cross section is eccentric cam follower conduct Central shaft 31, cam follower covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, connect with drawing mechanism 30 Conducting is connect, for driving central shaft 31.Collecting mechanism 50, inside sets constant temperature heating device, and the temperature for controlling heater is 250 DEG C, for collecting Graphene.Under motor driving, the cam follower moves in a circle around central shaft, the rotor Rotate one week, cavity volume volume is in cyclically-varying, under the reciprocating motion of two panels reed 32,33, the paste graphite mixture Constantly compressed and stretched, graphite is stripped into Graphene in drawing process.
The Graphene that will can be collected is added in plastic rubber, accounts for weight ratio for 0.008wt.%, and the solidify afterwards that stir are obtained To Graphene rubber.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 3
(1)It is 1 according to mass ratio by highly oriented graphite, PA PURs and normal propyl alcohol that graphite raw material particle diameter is 0.2 millimeter:7:2 Mixing and stirring, is configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into stretching-machine spout, the stretching-machine is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 60 DEG C to control operating temperature, and setting rotating speed is 800r/min, and cam follower is turned in the same direction Dynamic, during the central shaft is continued through, two cam followers produce compression stress and tensile force described in rotation process, The paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting machine Structure collects Graphene.
As shown in Figure 1 and shown in Fig. 2, the stretching-machine includes machine barrel 10, and the inside of machine barrel 10 sets a temperature regulating device 11, control Warm device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes the real-time measurement temperature of a thermocouple and feeds back, to control thing Material processing temperature maintains certain interval.A diameter of 900mm of machine barrel 10.Charging mechanism 20, is arranged on machine barrel 10, by least One spout 21 is constituted;Drawing mechanism 30, is connected with charging mechanism 20, including cross section is eccentric cam follower conduct Central shaft 31, cam follower covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, connect with drawing mechanism 30 Conducting is connect, for driving central shaft 31.Collecting mechanism 50, inside sets constant temperature heating device, and the temperature for controlling heater is 250 DEG C, for collecting Graphene.Under motor driving, the cam follower moves in a circle around central shaft, the rotor Rotate one week, cavity volume volume is in cyclically-varying, under the reciprocating motion of two panels reed 32,33, the paste graphite mixture Constantly compressed and stretched, graphite is stripped into Graphene in drawing process.
The Graphene that will can be collected is added in plastic rubber, accounts for weight ratio for 0.01wt.%, and the solidify afterwards that stir are obtained To Graphene rubber.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 4
(1)It is 1 according to mass ratio by crystalline flake graphite, galactolipin and water that graphite raw material particle diameter is 0.3 millimeter:9:4 mix Uniformly, it is configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into stretching-machine spout, the stretching-machine is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 70 DEG C to control operating temperature, and setting rotating speed is 900r/min, and cam follower is turned in the same direction Dynamic, during the central shaft is continued through, two cam followers produce compression stress and tensile force described in rotation process, The paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting machine Structure collects Graphene.
As shown in Figure 1 and shown in Fig. 2, the stretching-machine includes machine barrel 10, and the inside of machine barrel 10 sets a temperature regulating device 11, control Warm device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes the real-time measurement temperature of a thermocouple and feeds back, to control thing Material processing temperature maintains certain interval.A diameter of 1000mm of machine barrel 10.Charging mechanism 20, is arranged on machine barrel 10, by extremely A few spout 21 is constituted;Drawing mechanism 30, is connected with charging mechanism 20, including cross section is that eccentric cam follower is made Centered on axle 31, cam follower covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with drawing mechanism 30 Connection conducting, for driving central shaft 31.Collecting mechanism 50, inside sets constant temperature heating device, controls the temperature of heater It it is 250 DEG C, for collecting Graphene.Under motor driving, the cam follower moves in a circle around central shaft, described turn Son is rotated one week, and cavity volume volume is in cyclically-varying, under the reciprocating motion of two panels reed 32,33, the paste graphite mixing Thing is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process.
The Graphene that will can be collected is added in plastic rubber, accounts for weight ratio for 0.015wt%, and the solidify afterwards that stir are obtained To Graphene rubber.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 5
(1)It is 1 according to mass ratio by thermal cracking graphite, mannose and water that graphite raw material particle diameter is 0.3 millimeter:10:5 mixing are stirred Mix uniform, be configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into stretching-machine spout, the stretching-machine is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 80 DEG C to control operating temperature, and setting rotating speed is 1000r/min, and cam follower is turned in the same direction Dynamic, during the central shaft is continued through, two cam followers produce compression stress and tensile force described in rotation process, The paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting machine Structure collects Graphene.
As shown in Figure 1 and shown in Fig. 2, the stretching-machine includes machine barrel 10, and the inside of machine barrel 10 sets a temperature regulating device 11, control Warm device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes the real-time measurement temperature of a thermocouple and feeds back, to control thing Material processing temperature maintains certain interval.A diameter of 1100mm of machine barrel 10.Charging mechanism 20, is arranged on machine barrel 10, by extremely A few spout 21 is constituted;Drawing mechanism 30, is connected with charging mechanism 20, including cross section is that eccentric cam follower is made Centered on axle 31, cam follower covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with drawing mechanism 30 Connection conducting, for driving central shaft 31.Collecting mechanism 50, inside sets constant temperature heating device, controls the temperature of heater It it is 250 DEG C, for collecting Graphene.Under motor driving, the cam follower moves in a circle around central shaft, described turn Son is rotated one week, and cavity volume volume is in cyclically-varying, under the reciprocating motion of two panels reed 32,33, the paste graphite mixing Thing is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process.
The Graphene that will can be collected is added in plastic rubber, accounts for weight ratio for 0.02wt%, and the solidify afterwards that stir are obtained Graphene rubber.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Table 2
Performance indications 90% graphene film radial dimension 90% Graphene thickness Charge stripping efficiency
Embodiment one 15-16μm 0.8-2nm 64.5%
Embodiment two 16-17μm 1.5-2nm 68.4%
Embodiment three 15-17μm 0.9-1.6nm 74.8%
Example IV 16-170μm 2.1-3.7nm 67.1%
Embodiment five 15-17μm 2.9-4.0nm 62.1%

Claims (9)

1. it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that comprise the following steps:
(1)By graphite raw material, plasticity thing and solvent according to mass ratio be 1:5-10:2-5 mixing and stirrings, are configured to sticky cream Shape graphite mixture;
(2)The paste graphite mixture is put into drawing mechanism, it is 50-80 DEG C to control operating temperature, and setting rotating speed is 50- 100r/min, material is continued through during central shaft in drawing mechanism, is transported in the eccentric rotary of rotation process cam rotor It is dynamic, periodically compression and stretching cavity space, the paste graphite mixture is constantly compressed and is stretched, in drawing process Graphite is stripped into Graphene, and Graphene is collected by collecting mechanism.
2. it is according to claim 1 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the graphite Raw material is at least one in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide, and the graphite is former Material particle diameter is less than or equal to 1 millimeter;The plasticity thing is the EVA hot-melt adhesive with adhesivity, PA PURs, PE PURs, grape At least one in sugar, fructose, galactolipin, sorbose, Tagatose, inositol, mannose;The solvent is methyl alcohol, ethanol, isopropyl At least one in alcohol, normal propyl alcohol, deionized water.
3. it is according to claim 1 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the stretching Mechanism includes:
Machine barrel, inside sets a temperature regulating device;
Charging mechanism, is arranged on the machine barrel, is made up of at least one spout;
Draft flowing deformation mechanism, is connected with the charging mechanism, including cross section is the cam follower not coaxial with machine barrel, can stretch The spring reed of compression deformation;
Power drive mechanism, including a motor, conducting central shaft is connected with the draft flowing deformation mechanism, described for driving Central shaft;
Collecting mechanism, is arranged on the machine barrel, is made up of at least one discharging opening, for collecting Graphene presoma;
Wherein, the paste graphite mixture for graphite raw material, plasticity thing and solvent being mixed adds the charging mechanism laggard Enter the drawing mechanism, during the central shaft is continued through, made the chamber in machine barrel in the running by the cam follower Building volume back and forth reduces increase, due to paste have viscosity, by chamber by the reciprocating compression of cam and reed, stretching, Make graphite that Graphene is stripped into drawing process, it is to avoid the damage that extrusion shearing is caused to Graphene, produce compression stress And tensile force, the paste graphite mixture is constantly compressed and is stretched, graphite is stripped into Graphene in drawing process.
4. it is according to claim 1 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the stretching The barrel diameter of mechanism is 800-1100mm.
5. it is according to claim 3 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that in the drive Under dynamic motor drives, wherein the cam follower direction pivots clockwise or counter-clockwise eccentric rotary, the chamber in machine barrel in the running Building volume periodically reduces increase, and the paste, by the periodically compression of cam and reed, stretching, makes stone in chamber Ink is stripped into Graphene in drawing process, it is to avoid the damage that extrusion shearing is caused to Graphene, produces compression stress and drawing Stretch, makes the paste graphite mixture constantly be compressed and stretched, and graphite is stripped into Graphene in drawing process.
6. it is according to claim 3 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the cam Rotor does the rotary motion of bias along central shaft.
7. it is according to claim 3 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the cam Rotor surface covering wear-resistant ceramic layer or wear-resistant plastic layer.
8. it is according to claim 3 it is a kind of based on draft flowing deformation peel off Graphene method, it is characterised in that the collection In-house setting heating arrangements, continue directly to heat paste, moulding treatment.
9. a kind of Graphene rubber, it is characterised in that include:Plastic rubber, and Graphene prepared by claim 1, The Graphene accounts for weight ratio for 0.005 ~ 0.02wt%, is uniformly distributed in the plastic rubber, and solidify afterwards obtain Graphene rubber Glue product.
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