CN106672953A - Internal mixer for preparing graphene through tensile peeling and method for preparing graphene - Google Patents

Internal mixer for preparing graphene through tensile peeling and method for preparing graphene Download PDF

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Publication number
CN106672953A
CN106672953A CN201611243816.2A CN201611243816A CN106672953A CN 106672953 A CN106672953 A CN 106672953A CN 201611243816 A CN201611243816 A CN 201611243816A CN 106672953 A CN106672953 A CN 106672953A
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China
Prior art keywords
graphite
graphene
banbury
banburying
cam followers
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Inventor
陈庆
曾军堂
王镭迪
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Chengdu New Keli Chemical Science Co Ltd
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Chengdu New Keli Chemical Science Co Ltd
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Priority to CN201611243816.2A priority Critical patent/CN106672953A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • 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
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/32Size or surface area

Abstract

The invention provides an internal mixer for preparing graphene through tensile peeling and a method for preparing graphene. The internal mixer comprises a machine barrel, a feeding mechanism, an internal mixing mechanism, a power transmission mechanism and a collection mechanism, wherein the internal mixing mechanism comprises two cam rotors of which the cross sections are curved triangles as stirring shafts, and the two rotors generate relatively small shear force in a rotation process and generate relatively large compressive force and tensile force, so that a pasty graphite mixture is indirectly stretched, sheared and stripped to form a graphene precursor by a viscous additive under the bonding effect of the viscous additive when continuously passing through the stirring shafts, and thus the lattice damage of over-large shearing force to graphene is effectively avoided. The internal mixer is simple in preparation technology, wide in raw material source, free of pollution and low in cost; prepared graphene is high in quality and easy to store and transport; and large-scale industrial production is easy to implement.

Description

A kind of stretch release prepares the banbury of Graphene and prepares the method for Graphene
Technical field
The present invention relates to material processing field, and in particular to a kind of stretch release prepares the banbury of Graphene and prepares stone The method of black 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 applying pressure in the methods such as conventional ball mill, stirring ball-milling, grinding, the graphite to peeling off is produced Huge impulsive force, this impulsive force can make graphene layer produce fault of construction, easily cause graphene layer structural lattice defect, Reduce 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 stone Black alkene;In addition, the crunch of abrasive media can cause graphite Rotating fields to become even closer peeling effect can be caused to drop on the contrary It is low, cause that milling time is long, cost is very high, it is difficult to carry out large-scale industrialized production.
Banbury 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 banbury.At present, China Patent Publication No. 105948028A is disclosed A kind of banbury 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 banbury 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 banburying device 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 banbury Graphene dimensional homogeneity and the limited technological deficiency of charge stripping efficiency, this hair It is bright to propose that a kind of stretch release prepares the banbury of Graphene and prepares the method for Graphene, by the banburying for designing special construction Machine rotor, so as to improve and prepare Graphene quality using banbury and improve Graphene charge stripping efficiency.
To solve the above problems, the present invention uses following technical scheme:
On the one hand the banbury that a kind of stretch release prepares Graphene is provided, including:
Machine barrel, inside sets a temperature regulating device;
Charging mechanism, is arranged on the inside machine barrel, is made up of at least one spout;
Banburying mechanism, is connected with the charging mechanism, including cross section is two cam followers of curved line trangle as stirring Mix axle;
Power drive mechanism, including a motor, are connected conducting, for driving the agitating shaft with the banburying mechanism;
Collecting mechanism, for collecting Graphene presoma;
Wherein, after the paste graphite mixture for graphite raw material, banburying additive and water being mixed adds the charging mechanism Into the banburying mechanism, during the agitating shaft is continued through, two cam followers are produced described in rotation process Compression stress and tensile force, the paste graphite mixture are constantly compressed and are stretched, and graphite is stripped into stone in drawing process Black alkene.
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 1 millimeter;
The banburying additive be the Water-Soluble Glucose with adhesivity, fructose, galactolipin, sorbose, Tagatose, inositol, At least one in mannose.
Preferably, a diameter of 800-1100mm of the machine barrel.
Preferably, under motor driving, described two cam followers are rotate in same direction, wherein, described two Individual cam follower rotate when, two horizontal strokes of two cross section lines of centres of described two cam followers and described two cam followers Tangent plane edge points of tangency is overlapped, and described two rotors are rotated one week, and cavity volume volume is in cyclically-varying, the paste graphite mixing Thing is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process.
Preferably, the ratio between the length of the agitating shaft and length of side of the curved line trangle are more than 4/1.
Preferably, the stirring axis body covering wear-resistant ceramic layer.
Preferably, the collecting mechanism inside sets drum-type cooler or disc type vibratory sieve, for collecting Graphene Presoma.
On the other hand, there is provided a kind of method for preparing Graphene, it is characterised in that comprise the following steps:
(1)By graphite raw material, banburying additive and water according to mass ratio be 1:5-10:2-5 mixing and stirrings, are configured to sticky Paste graphite mixture;
(2)By the charging mechanism of banbury of the paste graphite mixture input as described in claim 1-7 any one, plus Enter the banburying mechanism after entering the charging mechanism, connect power drive mechanism, operating temperature is controlled for 10-30 DEG C, even Continue by the way that during the agitating shaft, two cam followers produce compression stress and tensile force, the cream described in rotation process Shape graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, is collected by collecting mechanism Graphene presoma;
(3)The Graphene presoma that will be collected removes impurity through over cleaning, dries and obtains grapheme material.
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 banburying additive is the water-soluble Portugal with adhesivity At least one in grape sugar, fructose, galactolipin, sorbose, Tagatose, inositol, mannose.
Banburying device 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 that a kind of stretch release prepares stone The banbury of black alkene has two cam followers of the cross section for curved line trangle as agitating shaft, and it is two turns in rotation process Son produces less shearing force, and produces larger compression and tensile force so that paste graphite mixture continue through it is described During agitating shaft, paste graphite mixture is stretched by the additive of viscosity, cut indirectly under the bonding effect of viscosity additives Cut stripping and obtain Graphene presoma, effectively prevent the crystal lattice damage that excessive shearing force is caused to Graphene.The present invention is disclosed Scheme preparation process is simple, raw material sources extensively, pollution-free, low cost, the presoma prepared is stable in properties, easily stores defeated Fortune, it is easy to accomplish scale industrial production.
By Graphene performance prepared by the present invention compared with common banburying equipment prepares Graphene, in Graphene quality, produce The aspects such as amount have the advantage that as shown in table 1.
Table 1:
Performance indications The present invention Common banburying equipment
90% graphene film radial dimension 150-180μm 80-120μm
90% Graphene thickness 0.5-4nm 0.3-6nm
Charge stripping efficiency 70%- 30%
Yield 200kg/h 20-30kg/h
A kind of stretch release of the present invention prepares the banbury of Graphene and prepares the method for Graphene, compared with prior art, its Prominent the characteristics of and excellent effect are:
1st, the banbury that a kind of stretch release for providing of the invention prepares Graphene has two that cross section is curved line trangle Used as agitating shaft, its two rotor in rotation process produces less shearing force to cam follower, and produces larger compression and drawing Stretch so that during the agitating shaft is continued through, paste graphite mixture is in viscosity additives for paste graphite mixture Bonding effect under, indirectly by viscosity additive stretching, shearing stripping obtain Graphene presoma, effectively prevent excessive cutting The crystal lattice damage that shear 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 banbury of Graphene, illustrated by accompanying drawing.
Accompanying drawing 1:A kind of stretch release prepares the structural representation of the banbury 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
As shown in Figure 1 and Fig. 2 shown in, the present invention in a kind of stretch release prepare Graphene banbury include machine barrel 10, machine barrel 10 inside set a temperature regulating device 11, and temperature regulating device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes a thermocouple reality When measurement temperature and feed back, certain interval is maintained with control material processing temperature.A diameter of 1000mm of machine barrel 10.Charger Structure 20, is arranged on machine barrel 10, is made up of at least one spout 21;Banburying mechanism 30, is connected with charging mechanism 20, including Cross section is two cam followers of curved line trangle as agitating shaft 31, the side of the length of agitating shaft and the curved line trangle The ratio between long is 4.5/1, stirring axis body covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with banburying mechanism 30 connection conductings, for driving agitating shaft 31.Collecting mechanism 50, inside sets disc type vibratory sieve, before collecting Graphene Drive body.Under motor driving, described two cam followers are rotate in same direction, wherein, described two cam followers are turning When dynamic, two cross section lines of centres of described two cam followers and two cross sections of described two cam followers edge points of tangency Overlap, described two rotors are rotated one week, cavity volume volume is in cyclically-varying, the paste graphite mixture constantly compressed with Stretching, graphite is stripped into Graphene in drawing process.
During Graphene is prepared, graphite raw material can be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking At least one in graphite, the powder of graphite oxide, banburying additive is the Water-Soluble Glucose with adhesivity, fructose, half At least one in lactose, sorbose, Tagatose, inositol, mannose.In the present embodiment by taking crystalline flake graphite and glucose as an example Illustrate, those skilled in the art can be selected as needed.Prepare Graphene process as follows:
(1)By graphite raw material particle diameter be less than 0.5 millimeter of crystalline flake graphite, glucose and water according to mass ratio be 1:5:2 mixing Stir, be configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into banbury spout, the banbury is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 10 DEG C to control operating temperature, and setting rotating speed is 20r/min, and two cam followers are carried out in the same direction Rotate, during the agitating shaft is continued through, two cam followers produce compression stress and stretching described in rotation process Power, the paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting Collect Graphene presoma;
(3)The Graphene presoma that will be collected removes impurity through over cleaning, dries and obtains grapheme material.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 2
As shown in Figure 1 and Fig. 2 shown in, the present invention in a kind of stretch release prepare Graphene banbury include machine barrel 10, machine barrel 10 inside set a temperature regulating device 11, and temperature regulating device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes a thermocouple reality When measurement temperature and feed back, certain interval is maintained with control material processing temperature.A diameter of 800mm of machine barrel 10.Charger Structure 20, is arranged on machine barrel 10, is made up of at least one spout 21;Banburying mechanism 30, is connected with charging mechanism 20, including Cross section is two cam followers of curved line trangle as agitating shaft 31, the side of the length of agitating shaft and the curved line trangle The ratio between long is 4.5/1, stirring axis body covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with banburying mechanism 30 connection conductings, for driving agitating shaft 31.Collecting mechanism 50, inside sets disc type vibratory sieve, before collecting Graphene Drive body.Under motor driving, described two cam followers carry out in the same direction or incorgruous rotation, wherein, described two cams turn Son when rotating, two cross section lines of centres of described two cam followers and two cross sections of described two cam followers edge Points of tangency is overlapped, and described two rotors are rotated one week, cavity volume volume in cyclically-varying, the continuous quilt of the paste graphite mixture Compression and stretching, graphite is stripped into Graphene in drawing process.
During Graphene is prepared, graphite raw material can be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking At least one in graphite, the powder of graphite oxide, banburying additive is the Water-Soluble Glucose with adhesivity, fructose, half At least one in lactose, sorbose, Tagatose, inositol, mannose.In the present embodiment by taking crystalline flake graphite and galactolipin as an example Illustrate, those skilled in the art can be selected as needed.Prepare Graphene process as follows:
(1)Crystalline flake graphite, galactolipin and water by graphite raw material particle diameter less than 0.5 millimeter are 1 according to mass ratio:6:3 mixing are stirred Mix uniform, be configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into banbury spout, the banbury is entered after adding the charging mechanism Structure, connects power drive mechanism, control operating temperature for 15 DEG C, and setting rotating speed is 50r/min, and two cam followers carry out incorgruous Rotate, during the agitating shaft is continued through, two cam followers produce compression stress and stretching described in rotation process Power, the paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting Collect Graphene presoma;
(3)The Graphene presoma that will be collected is dried and obtains grapheme material through over cleaning.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 3
As shown in Figure 1 and Fig. 2 shown in, the present invention in a kind of stretch release prepare Graphene banbury include machine barrel 10, machine barrel 10 inside set a temperature regulating device 11, and temperature regulating device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes a thermocouple reality When measurement temperature and feed back, certain interval is maintained with control material processing temperature.A diameter of 1100mm of machine barrel 10.Charger Structure 20, is arranged on machine barrel 10, is made up of at least one spout 21;Banburying mechanism 30, is connected with charging mechanism 20, including Cross section is two cam followers of curved line trangle as agitating shaft 31, the side of the length of agitating shaft and the curved line trangle The ratio between long is 7/1, stirring axis body covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with banburying mechanism 40 Connection conducting, for driving agitating shaft 31.Collecting mechanism 50, inside sets disc type vibratory sieve, for collecting Graphene forerunner Body.Under motor driving, described two cam followers carry out in the same direction or incorgruous rotation, wherein, described two cam followers When rotating, two cross section lines of centres of described two cam followers and two cross sections of described two cam followers edge phase Point of contact is overlapped, and described two rotors are rotated one week, and cavity volume volume is in cyclically-varying, and the paste graphite mixture is constantly pressed Contracting and stretching, graphite is stripped into Graphene in drawing process.
During Graphene is prepared, graphite raw material can be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking At least one in graphite, the powder of graphite oxide, banburying additive is the Water-Soluble Glucose with adhesivity, fructose, half At least one in lactose, sorbose, Tagatose, inositol, mannose.In the present embodiment with crystalline flake graphite, highly oriented graphite Illustrated as a example by mixture and sorbose, those skilled in the art can be selected as needed.Prepare Graphene process It is as follows:
(1)By graphite raw material particle diameter be less than 0.8 millimeter of crystalline flake graphite, highly oriented graphite mixture, sorbose and water according to Mass ratio is 1:10:5 mixing and stirrings, are configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into banbury spout, the banbury is entered after adding the charging mechanism Structure, connects power drive mechanism, control operating temperature for 28 DEG C, and setting rotating speed is 80r/min, and two cam followers carry out incorgruous Rotate, during the agitating shaft is continued through, two cam followers produce compression stress and stretching described in rotation process Power, the paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by collecting Collect Graphene presoma;
(3)The Graphene presoma that will be collected is dried and obtains grapheme material through over cleaning.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 4
As shown in Figure 1 and Fig. 2 shown in, the present invention in a kind of stretch release prepare Graphene banbury include machine barrel 10, machine barrel 10 inside set a temperature regulating device 11, and temperature regulating device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes a thermocouple reality When measurement temperature and feed back, certain interval is maintained with control material processing temperature.A diameter of 900mm of machine barrel 10.Charger Structure 20, is arranged on machine barrel 10, is made up of at least one spout 21;Banburying mechanism 30, is connected with charging mechanism 20, including Cross section is two cam followers of curved line trangle as agitating shaft 31, the side of the length of agitating shaft and the curved line trangle The ratio between long is 5/1, stirring axis body covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with banburying mechanism 30 Connection conducting, for driving agitating shaft 31.Collecting mechanism 50, inside sets disc type vibratory sieve, for collecting Graphene forerunner Body.Under motor driving, described two cam followers carry out in the same direction or incorgruous rotation, wherein, described two cam followers When rotating, two cross section lines of centres of described two cam followers and two cross sections of described two cam followers edge phase Point of contact is overlapped, and described two rotors are rotated one week, and cavity volume volume is in cyclically-varying, and the paste graphite mixture is constantly pressed Contracting and stretching, graphite is stripped into Graphene in drawing process.
During Graphene is prepared, graphite raw material can be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking At least one in graphite, the powder of graphite oxide, banburying additive is the Water-Soluble Glucose with adhesivity, fructose, half At least one in lactose, sorbose, Tagatose, inositol, mannose.In the present embodiment with expanded graphite and glucose, fruit Illustrated as a example by sugared mixture, those skilled in the art can be selected as needed.Prepare Graphene process as follows:
(1)It is according to mass ratio less than 0.6 millimeter of expanded graphite, glucose, fructose mixture and water by graphite raw material particle diameter It is 1:8:4 mixing and stirrings, are configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into banbury spout, the banbury is entered after adding the charging mechanism Structure, connects power drive mechanism, and it is 18 DEG C to control operating temperature, and setting rotating speed is 120r/min, and two cam followers are carried out together To rotation, during the agitating shaft is continued through, two cam followers produce compression stress and drawing described in rotation process Stretch, the paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by receiving Collecting mechanism collects Graphene presoma;
(3)The Graphene presoma that will be collected is dried and obtains grapheme material through over cleaning.
After Graphene to being prepared in embodiment carries out performance test, data are obtained as shown in table 2.
Embodiment 5
As shown in Figure 1 and Fig. 2 shown in, the present invention in a kind of stretch release prepare Graphene banbury include machine barrel 10, machine barrel 10 inside set a temperature regulating device 11, and temperature regulating device 11 is arranged on the inwall of machine barrel 10, and temperature regulating device 11 includes a thermocouple reality When measurement temperature and feed back, certain interval is maintained with control material processing temperature.A diameter of 1050mm of machine barrel 10.Charger Structure 20, is arranged on machine barrel 10, is made up of at least one spout 21;Banburying mechanism 30 is connected with charging mechanism 20, including Cross section is two cam followers of curved line trangle as agitating shaft 31, the side of the length of agitating shaft and the curved line trangle The ratio between long is 8/1, stirring axis body covering wear-resistant ceramic layer;Power drive mechanism 40, including a motor, with banburying mechanism 30 Connection conducting, for driving agitating shaft 31.Collecting mechanism 50, inside sets disc type vibratory sieve, for collecting Graphene forerunner Body.Under motor driving, described two cam followers carry out in the same direction or incorgruous rotation, wherein, described two cam followers When rotating, two cross section lines of centres of described two cam followers and two cross sections of described two cam followers edge phase Point of contact is overlapped, and described two rotors are rotated one week, and cavity volume volume is in cyclically-varying, and the paste graphite mixture is constantly pressed Contracting and stretching, graphite is stripped into Graphene in drawing process.
During Graphene is prepared, graphite raw material can be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking At least one in graphite, the powder of graphite oxide, banburying additive is the Water-Soluble Glucose with adhesivity, fructose, half At least one in lactose, sorbose, Tagatose, inositol, mannose.It is with thermal cracking graphite and Tagatose in the present embodiment Example is illustrated, and those skilled in the art can be selected as needed.Prepare Graphene process as follows:
(1)It is that thermal cracking graphite less than 0.9 millimeter, Tagatose and water are 1 according to mass ratio by graphite raw material particle diameter:7:5 mix Conjunction stirs, and is configured to sticky paste graphite mixture;
(2)The paste graphite mixture is put into banbury spout, the banbury is entered after adding the charging mechanism Structure, connects power drive mechanism, control operating temperature for 10 DEG C, and setting rotating speed is 150r/min, and two cam followers carry out different To rotation, during the agitating shaft is continued through, two cam followers produce compression stress and drawing described in rotation process Stretch, the paste graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, by receiving Collecting mechanism collects Graphene presoma;
(3)The Graphene presoma that will be collected is dried and obtains grapheme material through over cleaning.
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 150-160μm 0.5-2nm 72.5%
Embodiment two 160-180μm 1.5-2nm 83.4%
Embodiment three 150-178μm 0.8-1.6nm 80.8%
Example IV 160-180μm 2.5-3.7nm 77.1%
Embodiment five 155-175μm 2.9-4.0nm 82.1%

Claims (8)

1. a kind of stretch release prepares the banbury of Graphene, it is characterised in that including:
Machine barrel, inside sets a temperature regulating device;
Charging mechanism, is arranged on the inside machine barrel, is made up of at least one spout;
Banburying mechanism, is connected with the charging mechanism, including cross section is two cam followers of curved line trangle as stirring Mix axle;
Power drive mechanism, including a motor, are connected conducting, for driving the agitating shaft with the banburying mechanism;
Collecting mechanism, for collecting Graphene presoma;
Wherein, after the paste graphite mixture for graphite raw material, banburying additive and water being mixed adds the charging mechanism Into the banburying mechanism, during the agitating shaft is continued through, two cam followers are produced described in rotation process Compression stress and tensile force, the paste graphite mixture are constantly compressed and are stretched, and graphite is stripped into stone in drawing process Black alkene.
2. a kind of stretch release according to claim 1 prepares the banbury of Graphene, it is characterised in that the graphite is former Expect to be at least one in crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide, the graphite raw material Particle diameter is less than or equal to 1 millimeter;The banburying additive is the Water-Soluble Glucose with adhesivity, fructose, galactolipin, sorb At least one in sugar, Tagatose, inositol, mannose.
3. according to claim a kind of stretch release prepares the banbury of Graphene, it is characterised in that the machine barrel it is straight Footpath is 800-1100mm.
4. a kind of stretch release according to claim 1 prepares the banbury of Graphene, it is characterised in that in the driving Motor drive under, described two cam followers are rotate in same direction, wherein, described two cam followers rotate when, described two Two cross section lines of centres of individual cam follower overlap with two cross sections of described two cam followers edge points of tangency, and described two Individual rotor is rotated one week, and cavity volume volume is in cyclically-varying, and the paste graphite mixture is constantly compressed and stretched, in stretching During graphite be stripped into Graphene.
5. a kind of stretch release according to claim 1 prepares the banbury of Graphene, it is characterised in that the agitating shaft The ratio between length and the length of side of the curved line trangle be more than 4/1.
6. a kind of stretch release according to claim 1 prepares the banbury of Graphene, it is characterised in that the agitating shaft Body covering wear-resistant ceramic layer.
7. a kind of stretch release according to claim 1 prepares the banbury of Graphene, it is characterised in that the collection machine Structure inside sets drum-type cooler or disc type vibratory sieve, for collecting Graphene presoma.
8. a kind of method for preparing Graphene, it is characterised in that comprise the following steps:
(1)By graphite raw material, banburying additive and water according to mass ratio be 1:5-10:2-5 mixing and stirrings, are configured to sticky Paste graphite mixture;
(2)By the charging mechanism of banbury of the paste graphite mixture input as described in claim 1-7 any one, plus Enter the banburying mechanism after entering the charging mechanism, connect power drive mechanism, operating temperature is controlled for 10-30 DEG C, even Continue by the way that during the agitating shaft, two cam followers produce compression stress and tensile force, the cream described in rotation process Shape graphite mixture is constantly compressed and is stretched, and graphite is stripped into Graphene in drawing process, is collected by collecting mechanism Graphene presoma;
(3)The Graphene presoma that will be collected removes impurity through over cleaning, dries and obtains grapheme material;
Wherein, the graphite raw material be crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide in extremely Few one kind, the graphite raw material particle diameter is less than or equal to 1 millimeter;The banburying additive is the water-soluble grape with adhesivity At least one in sugar, fructose, galactolipin, sorbose, Tagatose, inositol, mannose.
CN201611243816.2A 2016-12-29 2016-12-29 Internal mixer for preparing graphene through tensile peeling and method for preparing graphene Pending CN106672953A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107177073A (en) * 2017-05-26 2017-09-19 成都新柯力化工科技有限公司 A kind of method that graphene/glass fiber reinforcement masterbatch is prepared by stretching
CN108163847A (en) * 2018-01-12 2018-06-15 昂星新型碳材料常州有限公司 The preparation method of large stretch of diameter graphene and large stretch of diameter graphene
CN115849354A (en) * 2022-12-12 2023-03-28 中国铝业股份有限公司 Graphene stripping equipment and graphene stripping method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817516A (en) * 2010-05-21 2010-09-01 哈尔滨工业大学 Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping
CN201610419U (en) * 2009-12-23 2010-10-20 沧州市元亨橡胶有限责任公司 Novel machine for desulfuration regeneration and preparation of waste vulcanized butyl rubber
CN105271206A (en) * 2015-11-23 2016-01-27 成都新柯力化工科技有限公司 Method for continuously preparing graphene material in cut mode through screw machine
CN105329886A (en) * 2015-12-08 2016-02-17 成都新柯力化工科技有限公司 Method for preparing graphene through composite shear stress stripping of vibrating screw extruder
CN106185888A (en) * 2016-07-04 2016-12-07 成都新柯力化工科技有限公司 A kind of continuously grinding extrusion prepares the Apparatus for () and method therefor of graphene composite material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201610419U (en) * 2009-12-23 2010-10-20 沧州市元亨橡胶有限责任公司 Novel machine for desulfuration regeneration and preparation of waste vulcanized butyl rubber
CN101817516A (en) * 2010-05-21 2010-09-01 哈尔滨工业大学 Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping
CN105271206A (en) * 2015-11-23 2016-01-27 成都新柯力化工科技有限公司 Method for continuously preparing graphene material in cut mode through screw machine
CN105329886A (en) * 2015-12-08 2016-02-17 成都新柯力化工科技有限公司 Method for preparing graphene through composite shear stress stripping of vibrating screw extruder
CN106185888A (en) * 2016-07-04 2016-12-07 成都新柯力化工科技有限公司 A kind of continuously grinding extrusion prepares the Apparatus for () and method therefor of graphene composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵素合: "《聚合物加工工程》", 31 March 2001, 中国轻工业出版社 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107177073A (en) * 2017-05-26 2017-09-19 成都新柯力化工科技有限公司 A kind of method that graphene/glass fiber reinforcement masterbatch is prepared by stretching
CN107177073B (en) * 2017-05-26 2020-06-09 南京德嘉玻璃钢材料有限公司 Method for preparing graphene/glass fiber reinforced master batch through stretching
CN108163847A (en) * 2018-01-12 2018-06-15 昂星新型碳材料常州有限公司 The preparation method of large stretch of diameter graphene and large stretch of diameter graphene
CN115849354A (en) * 2022-12-12 2023-03-28 中国铝业股份有限公司 Graphene stripping equipment and graphene stripping method
CN115849354B (en) * 2022-12-12 2023-08-15 中国铝业股份有限公司 Graphene peeling device and graphene peeling method

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