CN108069417A - Airflow generation device, graphene dispersion liquid and preparation method thereof - Google Patents
Airflow generation device, graphene dispersion liquid and preparation method thereof Download PDFInfo
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- CN108069417A CN108069417A CN201710350845.7A CN201710350845A CN108069417A CN 108069417 A CN108069417 A CN 108069417A CN 201710350845 A CN201710350845 A CN 201710350845A CN 108069417 A CN108069417 A CN 108069417A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 186
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 title abstract description 26
- 239000006185 dispersion Substances 0.000 title abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 49
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- 238000012545 processing Methods 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 23
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- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
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- 150000001241 acetals Chemical class 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 150000008064 anhydrides Chemical class 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
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- 150000008282 halocarbons Chemical class 0.000 claims description 3
- 239000003049 inorganic solvent Substances 0.000 claims description 3
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- 150000002576 ketones Chemical class 0.000 claims description 3
- -1 nitrogenous compound Chemical class 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
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- 206010021143 Hypoxia Diseases 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
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- 230000032798 delamination Effects 0.000 description 2
- 229940113088 dimethylacetamide Drugs 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
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- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention provides an airflow generation device, a graphene dispersion liquid and a preparation method of the graphene dispersion liquid. The graphene dispersion liquid is prepared from graphene powder and a processing solvent, the average sheet diameter of graphene in the graphene dispersion liquid is 0.5-1 mu m, the number of layers is 3-5, the solid content is 5-50%, the surface oxygen content is less than 1 wt%, the distribution concentration of the graphene dispersion liquid is gradually increased from the upper layer to the bottom layer after the graphene dispersion liquid is stood for 12 hours, the viscosity is 5000-8000 cps, and the graphene concentration is 20 wt%.
Description
Technical field
The present invention relates to a kind of air flow-producing device, graphene dispersing solution and preparation method thereof more particularly to it is a kind of to
Prepare air flow-producing device, graphene dispersing solution of hypoxemia amount graphene powder and preparation method thereof.
Background technology
Graphene has by carbon atom with sp2The two-dimensional structure of covalent bond composition, and it is migrated with quite high carrier
The special natures such as rate, hardness, pyroconductivity, current carrying capacity and great surface-volume ratio.Therefore, graphite in recent years
Alkene has become the goal in research being highly valued in the fields such as the doctor that makes a living, electronics and photoelectric cell.Meanwhile graphene dispersing solution can
It is widely used in paint field, is helped for electrically-conducting paint and related assistant director of a film or play's agent, li-ion electrode assistant director of a film or play agent, anticorrosive coating
Important additive in the products such as agent and graphene samming piece.
However, in existing graphene dispersing solution technology of preparing, chemical treatment processing procedure has soda acid and heavy metal waste liquid
Contaminated wastewaters and toxic useless exhausting problem are waited, and the Physicals such as mechanical stripping method, ultrasonic vibrating or ball-milling method have solid content
Low, the defects of low yield and product sheet footpath and thickness distribution are uneven.In addition, graphene dispersing solution commercially available product common at present is big
Mostly low-solid content wherein excessive solvent will seriously affect subsequent resin characteristics and processability, therefore is unfavorable for graphene point
Dispersion liquid is in the application of paint field.In addition, the common technology of graphene suspension is promoted as surfaction or increases dispersing aid
(being more than 5%), both approaches can all be greatly reduced the physical property of graphene, even improve being manufactured into for graphene dispersing solution
This.
Based on above-mentioned, ecological requirements can be met, promote solid content, increase yield, promoting suspension, by developing one kind
One changes the graphene dispersing solution of product specification and low manufacture cost, for the important topic of required research at present.
The content of the invention
The present invention provide a kind of air flow-producing device for being used to prepare hypoxemia amount graphene powder, graphene dispersing solution and its
Graphene powder made by air flow-producing device is used to prepare graphene dispersing solution, to efficiently solve mesh by preparation method
Before be present in most of technical problem in graphene dispersing solution processing procedure.Thus, it can prepare with certain concentration variation
High concentration graphene dispersion liquid not only conforms to ecological requirements, more can significantly promote solid content, increase yield, promotes suspension
Property and homogenization product specification, and the manufacture cost of graphene dispersing solution can be greatly reduced.
The air flow-producing device of the present invention includes external bushing and rotates awl.External bushing have chamber, air inlet openings with
And outlet opening, air inlet openings are communicated in the lower section of chamber and outlet open communication is in the top of chamber, and middle chamber has neck
Contracting portion.It rotates awl to be arranged in chamber, rotates awl and chamber is conformal, and rotate between awl and the inner wall of chamber with narrow
Spacing is stitched, wherein rotating cone attached bag, which includes, rotates body and a plurality of screw thread, and the bottom direction of screw thread autorotation body rotates body
Top be spirally distributed in rotate body outer surface on.When rotating awl and rotating in the chamber, by screw thread and narrow
Spacing is stitched to generate upwards and there is the cyclone of the component of horizontal direction.
In one embodiment of this invention, the top surface of awl is rotated to flush with the top surface of necking section.
In one embodiment of this invention, in rotating body including bottom, top and between bottom and top
Portion, wherein the diameter for rotating body sequentially successively decreases from bottom to top.In addition, the diameter of the bottom surface of bottom is more than the top surface of bottom
Diameter.Furthermore the diameter of the bottom surface at middle part is more than the diameter of the top surface at middle part, and the diameter of the bottom surface at middle part is equal to bottom
The diameter of top surface.Also, the diameter of the bottom surface at top is more than the diameter of the top surface at top, and the diameter of the bottom surface at top is equal to middle part
Top surface diameter.
In one embodiment of this invention, the section for rotating awl is in asterism shape.
In one embodiment of this invention, the range of speeds of awl is rotated between 3000rpm (Revolution (s) Per
Minute, rotating speed per minute) to 7000rpm.
In one embodiment of this invention, the quantity of screw thread is between 8 to 32；And in another embodiment, screw thread
Quantity is between 12 to 18.
In one embodiment of this invention, the scope of slit spacing is between 0.05 millimeter to 10 millimeters；And in another implementation
In example, the scope of slit spacing is between 0.1 millimeter to 1 millimeter.
The preparation method of the graphene dispersing solution of the present invention comprises the following steps.Graphene powder and processing solvent are carried out
Processing procedure is homogenized, to form graphene thickener.Afterwards, thin layer processing procedure is carried out to graphene thickener, to form graphene dispersion
Liquid, wherein graphene powder are using made by said flow generation device.
In one embodiment of this invention, the preparation method of graphene powder comprises the following steps.Graphite former material is carried out
For continuous high speed toward calendering processing procedure is covered so that graphite predecessor is made, graphite predecessor has difference row's Sliding Structures.Afterwards, level is passed through
Direction compressed air stream makes graphite predecessor carry out intercalation, to form graphene and gas intercalation compound.Then, layer is passed through
Between stream pressure release graphene and gas intercalation compound is made to carry out expansion stripping reaction, to form graphene aggregation.So
Afterwards, graphene aggregation is made to suspend in the gas flow to drift about and mutually collide, to generate graphene powder.
In one embodiment of this invention, each interlayer spacing in graphite predecessor isExtremely
In one embodiment of this invention, the wind speed of horizontal direction compressed air stream is 0.3 Mach to mach one.
In one embodiment of this invention, the air quantity of horizontal direction compressed air stream is 186CMM to 619CMM.
The graphene dispersing solution of the present invention is using the preparation method of above-mentioned graphene dispersing solution by graphene powder and processing
Made by solvent, the average piece footpath of the graphene in graphene dispersing solution is 0.5 μm to 1 μm, and the number of plies is 3 to 5 layers, and solid content is
5% to 50%, surface oxygen content be less than 1wt%, and graphene dispersing solution stand 12 it is small when after distributed density present by upper strata
To the state of bottom increasing concentration, viscosity is 5000cps to 8000cps, and graphene concentration is 20wt%.
In one embodiment of this invention, concentration phase difference of the graphene dispersing solution at the middle and upper levels between bottom is
0.1wt% to 20wt%.
In one embodiment of this invention, the number of plies of graphene powder is 5 to 10 layers.
In one embodiment of this invention, the average piece footpath of graphene powder is 3 μm to 15 μm.
In one embodiment of this invention, the content of surface oxygen of graphene powder is less than 0.1wt%.
In one embodiment of this invention, handling solvent includes varsol, halogenated hydrocarbon solvent, alcohols solvent, phenols
Solvent, ketones solvent, ethers and acetals solvent, acids and anhydride solvent, nitrogenous compound solvent, sulfur-containing compound are molten
Agent, multifunctional group solvent or inorganic solvent.
In one embodiment of this invention, the interfacial tension scope of solvent is handled as 15mN/m to 50mN/m, Hansen dissolving
Degree parameter is 5.0MPa0.5To 15MPa0.5。
In one embodiment of this invention, with the gross weight meter of graphene dispersing solution, the additive amount of graphene powder is
0.001wt% to 30wt%.
Graphite former material is made using direct continuous physical method based on above-mentioned, of the invention air flow-producing device and is contained with low
The graphene powder of oxygen amount feature, and there is this graphene powder the number of plies to fix, piece footpath feature is consistent and be easy at low energies
The features such as structure caused by homogenization and no oxidation is destroyed.Meanwhile the present invention proposes a kind of above-mentioned graphene powder of utilization
Made graphene dispersing solution has many advantages, such as high yield, high solids content and solid content tool adjustability, therefore, can
It solves the problems, such as that low-solid content and the solvent selectivity of graphene dispersing solution commercially available product are few, and then processability and different paintings can be improved
The adaptability of cloth processing procedure is conducive to the application in paint field.
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below, and it is detailed that attached drawing is coordinated to make
Carefully it is described as follows.
Description of the drawings
Fig. 1 is the sectional view of air flow-producing device.
The stereoscopic schematic diagram for the rotation awl that Fig. 2 is Fig. 1.
Fig. 3 A are the rotation top surface at top of awl and the schematic diagram of bottom surface.
Fig. 3 B are the rotation top surface at middle part of awl and the schematic diagram of bottom surface.
Fig. 3 C are the rotation top surface of bottom of awl and the schematic diagram of bottom surface.
Fig. 4 is the flow diagram of the manufacturing method of graphene powder.
Reference sign
100：Air flow-producing device
108：Slit spacing
110：External bushing
112：Chamber
112a：Necking section
114：Air inlet openings
116：Outlet opening
120：Rotate awl
122：Rotate body
124：Screw thread
1221：Bottom
1222：Top
1223：Middle part
120a、112b、1221b、1222b、1223b：Top surface
1221a、1223a、1222a：Bottom surface
130：Screening washer
S：Space
S110、S120、S130、S140：Step
θ1、θ2、θ3：Angle
Specific embodiment
The present invention provides a kind of air flow-producing device, graphene dispersing solution and its preparation side for being used to prepare graphene powder
Method, wherein the graphene powder made by air flow-producing device is used to prepare graphene dispersing solution.Hereinafter, the present invention will be directed to
Air flow-producing device, each details in graphene dispersing solution and preparation method thereof is described in detail.
<Air flow-producing device>
Fig. 1 is the sectional view of air flow-producing device, and the stereoscopic schematic diagram for the rotation awl that Fig. 2 is Fig. 1.It please also refer to
Fig. 1 and Fig. 2, air flow-producing device 100 include external bushing 110 and rotate awl 120, and wherein external bushing 110 has chamber
112nd, air inlet openings 114 and outlet opening 116.Air inlet openings 114 are communicated in the lower section of chamber 112 and outlet opening 116 connects
The top of chamber 112 is passed through, and chamber 112 has necking section 112a.It rotates awl 120 and is conformably arranged at chamber with chamber 112
It in room 112, and rotates with slit spacing 108 between awl 120 and the inner wall of chamber 112, wherein rotating awl 120 includes turning
Dynamic body 122 and a plurality of screw thread 124, the bottom 1221 of 124 autorotation body 122 of screw thread is towards the top for rotating body 122
It is spirally distributed on the outer surface for rotating body 122.
In one embodiment, the quantity of above-mentioned screw thread 124 can be between 8 to 32, and the screw thread 124 in another embodiment
Quantity can be between 12 to 18.The quantity of screw thread 124 and from herein illustrate to be limited, designer can be according to actual
Demand is aided with considering for other factors and changes the quantity of screw thread 124.In addition, rotate the top surface 120a and chamber of awl 120
The top surface 112b of 112 necking section 112a is flushed.
Fig. 3 A are the top surface at top for rotating awl and the top surface that schematic diagram, Fig. 3 B of bottom surface are the middle part for rotating awl
And the schematic diagram of bottom surface, and Fig. 3 C are the rotation top surface of bottom of awl and the schematic diagram of bottom surface.Please also refer to Fig. 3 A,
Fig. 3 B and Fig. 3 C rotate body 122 and can be divided into bottom 1221, top 1222 and between bottom 1221 and top 1222
Middle part 1223, and since screw thread 124 is formed in the outer surface (not indicating) of rotation body 122, along rotation awl 120
Circumferencial direction takes section to rotating awl 120, and the cross sectional shape for rotating awl 120 is substantially in asterism shape.The depth of screw thread 124 with
And width can be set according to actual demand.
Hold it is above-mentioned, rotate body 122 diameter sequentially successively decrease from bottom 1221 to top 1222.More specifically, turn
Diameter of the diameter of the bottom surface 1221a of the bottom 1221 of mantle 120 more than the top surface 1221b of bottom 1221, and middle part 1223
Bottom surface 1223a diameter be equal to bottom 1221 top surface 1221b diameter, and the diameter of the bottom surface 1223a at middle part 1223 is big
In the diameter of the top surface 1223b at middle part 1223, as shown in Fig. 3 B and Fig. 3 C.Also, the diameter of the bottom surface 1222a at top 1222 is equal to
The diameter of the top surface 1223b at middle part 1223, and the diameter of the bottom surface 1222a at top 1222 is more than the top surface 1222b at top 1222
Diameter, as shown in Fig. 3 A and Fig. 3 B.It is different in response to the diameter of bottom 1221, middle part 1223 and top 1222, therefore positioned at each
The quantity of the screw thread 124 in portion is also with difference.
Subsidiary one carries, and foregoing rotation body 122 can be integrally formed or have different-diameter by three
Cylinder assemble.Positioned at rotate body 122 top 1222 screw thread 124 can be identical clearance gap set,
And compared with the top surface 1222b or bottom surface 1222a at top 1222 angle, θ 1 be it is fixed, be, for example, 15 degree to 35 degree；It is located at
The screw thread 124 at middle part 1223 can also be set with identical clearance gap, and compared with middle part 1223 top surface 1223b or
The angle, θ 2 of bottom surface 1223a is fixed, is, for example, 35 degree to 70 degree；And positioned at bottom 1221 screw thread 124 can also be with
Set to identical clearance gap, and compared with the top surface 1221b or bottom surface 1221a of bottom 1221 angle, θ 3 be it is fixed,
For example, 70 degree to 90 degree.But the angle of the screw thread 124 at top 1222, middle part 1223 and bottom 1221 is not exactly the same.
For example, the angle positioned at the screw thread 124 at top 1222 is 25 degree, and the angle positioned at the screw thread 124 of bottom 1221 is 60 degree,
And the angle of the screw thread 124 positioned at middle part 1223 is about 42.5 degree.In addition, top 1222, middle part 1223 and bottom 1221
The angle of the screw thread 124 of junction is adjusted in response to the variation of diameter, and angle can be 35 degree to 85 degree.
When using the air flow-producing device 100 of Fig. 1, make rotation awl 120 with scope between 3000rpm to 7000rpm
Rotating speed rotated in chamber 112.In general, when rotation awl 120 rotates in chamber 112, if rotating awl 120
Outer surface and the surface of inner wall of chamber 112 be smooth, and the gas entered from air inlet openings 114 is subject to rotate awl
120 rotation and drive to generate and swirling eddy and dissipated from the outlet opening 116 positioned at the top of external bushing 110 1222.It is logical
The centrifugal force for rotating and being generated when awl 120 rotates is crossed, swirling eddy can be made to generate the component of a little horizontal direction, but compared
In the strength that air-flow escapes upwards from outlet opening 116, the component of horizontal direction is not obvious, almost can be ignored.
Specifically, the screw thread 124 of Spiral distribution is formed on the outer surface by rotating body 122, therefore works as gas
When being subject to rotate the drive of awl 120 and form the air-flow of rotation after from air inlet openings 114 into chamber 112, centrifugal force adds
The guiding of screw thread 124 is so that the component of the horizontal direction of swirling eddy is apparent.
Although in addition, rotate awl 120 and external bushing 110 it is conformal, the bottom surface of the bottom 1221 of autorotation body 122
To the top surface 1222b at top 1222, the slit spacing 108 rotated between the inner wall of body 122 and chamber 112 become 1221a
Change, such as become smaller.Such design method be according to gas flux equation, allow gas into air flow-producing device 100 to
It is compressed during upper flowing and air-flow accelerates from bottom to up.Due to top surface of the chamber 112 at the top 1222 for rotating body 122
On provide a broad space S, therefore leave and rotate the air-flow of awl 120 enter after this broad space S can be swollen
It is swollen, then dissipated away from outlet opening 116.
Briefly, it is bottom 1221 to the top for the air-flow autorotation awl 120 being inducted into from air inlet openings 114
There is slow, fast, slow flow rate variation on 1222, wherein being rotated since air-flow leaves between awl 120 and the inner wall of chamber 112
To be released to a relatively large space S immediately after slit spacing 108, thus the volume of gas have it is continuous and quick
Expansion variation.
Foregoing air flow-producing device 100 is by the cooperation of screw thread 124 and slit spacing 108 and air-flow can generate
Horizontal component, and can obtain air-flow after air-flow leaves screw thread 124 and continuously and quickly gas volume is generated in unit space S
Variation, therefore, being adapted to production needs to carry out the graphene powder of intercalation processing procedure.
<Graphene powder>
By said flow generation device, the graphene powder with low oxygen content feature can be made into.Fig. 4 is Graphene powder
The flow diagram of the manufacturing method of body.Hereinafter, the graphene powder flocculate of one embodiment of the invention will be described in detail with Fig. 4
Manufacturing method.
First, Fig. 4 is refer to, carries out step S110, continuous high speed is carried out to graphite former material toward calendering processing procedure is covered to be made
Graphite predecessor, graphite predecessor have difference row's Sliding Structures.In the present embodiment, each interlayer spacing in graphite former material is for example
It isEach interlayer spacing in graphite predecessor is, for example,ExtremelyAverage grain diameter be, for example, 10 μm extremely
100 μm, be preferably, for example, 15 μm to 35 μm；Average thickness is, for example, 0.05 μm to 1 μm, is preferably, for example, 0.3 μm to 0.8 μm；
Content of surface oxygen is, for example, to be less than 5%, is preferably, for example, to be less than 1%.Since graphite predecessor has difference row's Sliding Structures, because
This, is conducive to the progress of intercalation in follow-up process.More specifically, the flat of calendering processing procedure can be covered by the way that continuous high speed is past
Face tangential direction stress forms the graphite predecessor plate with difference row's Sliding Structures, then via dry type high speed grinding system
Journey forms graphite forerunner's powder.
Then, Fig. 4 is continued referring to, carries out step S120, carries out graphite predecessor by horizontal direction compressed air stream
Intercalation, to form graphene and gas intercalation compound.In the present embodiment, the wind speed of horizontal direction compressed air stream is for example
Be 0.3 Mach to mach one, be preferably, for example, 0.5 Mach to 0.8 Mach；Air quantity is, for example, 186CMM to 619CMM, preferably for example
It is 310CMM to 495CMM.More specifically, horizontal direction compressed air stream can be subcritical fluids, and since wind speed is, for example,
0.3 Mach or more, therefore horizontal direction compressed air stream is alternatively referred to as subsonic compressible flow.
Afterwards, Fig. 4 is continued referring to, carries out step S130, graphene and gas blanket are made by the release of interlayer stream pressure
Between compound carry out expansion stripping reaction, to form graphene aggregation.Then, as shown in figure 4, carrying out step S140, stone is made
Black alkene aggregation suspends in the gas flow to be drifted about and mutually collides, to generate graphene powder.
In the present embodiment, graphene powder has the advantages that the number of plies is fixed and piece footpath feature is consistent.In more detail, stone
The number of plies of black alkene powder is, for example, 5 to 10 layers；Thickness is, for example, 2.5nm to 4.5nm；Content of surface oxygen is, for example, to be less than
0.1wt%；Bulk density is, for example, 0.001g/cm3To 2.24g/cm3, preferably e.g. 0.01g/cm3To 0.5g/cm3.Graphite
The average piece footpath of alkene powder is, for example, 3 μm to 15 μm, more specifically, average piece footpath be, for example, 3 μm to 5 μm, 5 μm to 10 μm or
10 μm to 15 μm, and be preferably, for example, 3 μm to 5 μm.
<Graphene dispersing solution>
The graphene dispersing solution of the present invention is as made by above-mentioned graphene powder and processing solvent, wherein with graphene point
The gross weight meter of dispersion liquid, the additive amount of graphene powder is, for example, 0.001wt% to 30wt%.Due to the use of having as described above
The few layer hypoxemia amount graphene powder of the specific number of plies and specific modality carries out the preparation of graphene dispersing solution, this graphene powder base
It is fixed in the number of plies and the feature in a piece of footpath, and is easy to homogenization at low energies and not because oxidation causes structure to be destroyed etc.
Feature so that made graphene dispersing solution has many advantages, such as high yield, high solids content and solid content tool adjustability.
More specifically, the preparation method of graphene dispersing solution of the present invention comprises the following steps.First, to graphene powder
And processing solvent carries out homogenization processing procedure, to form graphene thickener.Afterwards, thin layer processing procedure is carried out to graphene thickener, with
Form uniform graphene dispersing solution.It is carried out below for each details in the graphene dispersion liquid and preparation method thereof of the present invention detailed
Explanation.
Handle solvent
In the present embodiment, processing solvent may include varsol, halogenated hydrocarbon solvent, alcohols solvent, phenol solvent, ketone
It is class solvent, ethers and acetals solvent, acids and anhydride solvent, nitrogenous compound solvent, sulfur-containing compound solvent, multifunctional
Group solvent or inorganic solvent.More specifically, it is, for example, toluene, dimethylbenzene (Xyl), ethyl alcohol, isopropanol to handle solvent
(IPA), butanol, acetone, ethyl acetate, butyl acetate (BAC), N,N-dimethylformamide (DMF), N-Methyl pyrrolidone
(NMP), DMAC N,N' dimethyl acetamide (DMAc) or water.
However, the processing solvent that the present invention is applicable in is not limited with the above listed concrete example enumerated, it is possible to use
Other solvents having the following properties that are as processing solvent：Interfacial tension scope is, for example, 15mN/m to 50mN/m, preferably for example
It is 20mN/m to 40mN/m；Hansen Solubility Parameter is, for example, 5.0MPa0.5To 15MPa0.5；Polarity force parameter is, for example,
0.5MPa0.5To 5.5MPa0.5；Scattered force parameter is, for example, 7.0MPa0.5To 9.0MPa0.5；And hydrogen bond force parameter is, for example,
2.0MPa0.5To 7.0MPa0.5.More specifically, with the gross weight meter of graphene dispersing solution, the additive amount for handling solvent is, for example,
70wt% to 99.99wt%.
Homogenize processing procedure
In the preparation method of graphene dispersing solution of the present invention, homogenization processing procedure is carried out to be formed as intermediate process by-product
The graphene thickener of object.This homogenization processing procedure is on the premise of graphene thickness is not changed, by being generated to graphene-structured
The mode of normal direction stress adjusts and changes the average piece footpath scope of graphene powder, to achieve the purpose that piece footpath homogenizes.
Thus, which suspension of the graphene in liquid can be effectively increased, most long suspension time can be reduced up to 150 days or more
Dispersant.
In the present embodiment, homogenization processing procedure can include mixing with disperseing two sections of processes again, and homogenization processing procedure can pass through
Such as direct current machine mixer, planetary-type mixer, mixer, ballmillmixer, three roller mixers, list Kun axis mixer or
The equipment such as double Hun axis mixers carry out mixing homogenizing, therefore, need to pass through scattered, oxidation, stripping compared to using graphite as raw material
And centrifugation processing procedure can just obtain the existing processing procedure of graphene dispersing solution, the present invention can solve that graphene content is low, structure is by oxygen
Change action breaks down and electrical conductivity and the problem of being present in prior art such as decline.
Graphene thickener
In the present embodiment, the feature of graphene thickener includes：The average piece footpath of graphene is, for example, 0.1 μm to 1.5 μm,
Preferably it is, for example, 0.3 μm to 0.8 μm；The thickness of graphene is, for example, 2.5nm to 4.5nm；Surface oxygen content is, for example, to be less than
0.5%, solid content is, for example, 5% to 50%, and optimal is, for example, 15% to 30%.
Thin layer processing procedure
In the preparation method of graphene dispersing solution of the present invention, thin layer processing procedure is carried out to graphene thickener, it is equal to be formed
Even graphene dispersing solution.This thin layer processing procedure is on the premise of graphene film footpath is not changed, by being generated to graphene-structured
The mode of in-plane stress changes the average thickness range of graphene powder, to achieve the purpose that even suspension.Such one
Come, suspension time can be promoted and solid content allows ratio.
In the present embodiment, thin layer processing procedure can include two kinds of different processes, be respectively mixed processes and high energy dispersion work
Sequence.More specifically, mixed processes can be mixed by the methods of five axis mixing methods, ball milling mixing method or shear-mixed method,
And high energy shear process can again be disperseed by the methods of high speed homogenization method or high pressure crush method, to form uniform graphene point
Dispersion liquid.
By the preparation method of graphene dispersing solution of the present invention, the high concentration graphene with certain concentration variation can be made into
Dispersion liquid, and be not required to add any dispersant again, therefore the graphene-structured in graphene dispersion production helps from the scattered of excess
Agent is disturbed and keeps good material property.More specifically, in graphene dispersing solution of the invention, graphene purity is about
100%, and the average piece footpath of the graphene in graphene dispersing solution is, for example, 0.5 μm to 1 μm；The number of plies is, for example, 3 to 5 layers；Gu
Content is, for example, 5% to 50%；Surface oxygen content is, for example, to be less than 1wt%；Thickness is, for example, 0.8nm to 4.5nm, preferably for example
It is 1.0nm to 2.0nm.
In addition, graphene dispersing solution stand 12 it is small when after distributed density shape by upper strata to bottom increasing concentration can be presented
State, viscosity are, for example, 5000cps to 8000cps, and graphene concentration is, for example, 20wt%, at the middle and upper levels the concentration between bottom
Phase difference (C%) is, for example, 0.1wt% to 20wt%, and preferably e.g. 5wt% is to 15wt%, and most long suspension time is reachable
150 days or more.
Hereinafter, the graphene dispersing solution proposed by experimental example come the present invention will be described in detail.However, following experimental examples are simultaneously
It is non-limiting the present invention.
Experimental example
In order to prove that the graphene dispersing solution of the present invention has higher solids content and suspension, especially make this experiment below
Example.
It should be noted that since the preparation method of graphene dispersing solution is in above describing in detail, hereafter
In the preparation in relation to graphene dispersing solution, for ask facilitate illustrate thus omit prepare details narration.
The preparation of graphene dispersing solution
According to the preparation method of the invention described above graphene dispersing solution, every condition is formed with listed in lower section table 1
And process conditions, the graphene dispersing solution of preparating example 1 to example 21.In table 1, mixed proportion (G/S) expression graphene/molten
The ratio of agent (Graphene/Solvent).
Table 1
Assessment 1：The characteristic evaluation of graphene dispersing solution
For the graphene dispersing solution made into example 21 of example 1, the wherein average piece footpath of graphene, the number of plies are measured
And stand 12 it is small when after concentration phase difference (C%) between upper strata and bottom, and will be in assessment result table 2 listed below.
The method for measurement of dispersion liquid concentration difference is adjust the distance when every 24 the is small 1/3 liquid eminence and 2/3 liquid of horizontal plane
The dispersion liquid of eminence carries out solid content analysis, and by the concentration C at 2/32/3Concentration C at % and 1/31/3% subtracts each other to obtain
C% concentration differences, wherein solid content are that liquid is evaporated rear obtained concentration.If concentration difference is more than 20% (that is, (C1/3%-
C2/3%)>20%), then bad dispersibility.
Table 2
It it can be seen that, is averaged by top table 2 using the graphene of example 1 to example 21 made by the preparation method of the present invention
Flake diameter distribution is uniform, therefore, can improve product sheet footpath in the Physicals such as existing machinery stripping method, ultrasonic vibrating or ball-milling method
The problem of being unevenly distributed.In addition, example 1 to example 21 graphene dispersing solution stand 12 it is small when after distributed density present by upper
Layer to bottom increasing concentration state.
Assessment 2：Property comparison between the graphene dispersing solution and commercially available product of the present invention
For the commercially available product of the graphene dispersing solution made into example 21 of example 1 and comparative example 1 to comparative example 6,
Measure the wherein solid content of graphene and most long suspension time, and will be in assessment result table 3 listed below.
Solid content is that liquid is evaporated rear obtained concentration.Suspension time is defined as follows for 150 days, is made in dispersion liquid
Measurement is done in the 150th day afterwards, if concentration difference<20%, then suspension time be at least 150 days.The method for measurement of concentration difference in
It is described above, therefore it will not be described here.
The commercially available product of comparative example 1 to comparative example 6 be made of via existing oxidation process and delamination processing procedure, and using this
Invent proposed homogenization processing procedure and thin layer processing procedure, the wherein raw material of comparative example 1 to comparative example 3 is graphite, comparative example 4 to
The raw material of comparative example 6 is graphene.
Table 3
By top table 3 it can be seen that, compared to using comparative example 1 made of existing oxidation process and delamination processing procedure to comparing
Example 6 has significantly higher graphene solid content using the example 1 made by the preparation method of the present invention to example 21, therefore,
The preparation method of the present invention can solve the problems, such as the low graphene solid content of commercially available product, and then can improve processability, be conducive to applying
The application in material field.In addition, as shown in table 3, compared to comparative example 1 to the commercially available product of comparative example 6, graphene dispersing solution of the present invention
Preparation method can effectively increase suspension of the graphene in liquid, make most long suspension time up to 150 days.
In conclusion the hypoxemia amount Graphene powder with the specific number of plies is mainly made with air flow-producing device by the present invention
Body, then this graphene powder with the specific number of plies and kenel is made to the graphene dispersing solution of high solids content, accordingly, it is possible to resolve
The problems such as low-solid content and solvent selectivity of graphene dispersing solution commercially available product are few, so can improve processability and it is different apply it is fabric
The adaptability of journey is conducive to the application in paint field.In addition, the graphene dispersion liquid and preparation method thereof of the present invention need not make again
With other oxidizing process, surfaction method or a large amount of dispersing aiies of addition (>5%), therefore, graphene-structured is not damaged and can protect
It holds structural integrity and is disturbed from excessive dispersing aid, and then keep its good material property, can more solve existing skill
The contaminated wastewaters such as soda acid and heavy metal waste liquid and toxic useless exhausting problem are generated in art, and then more preferably meets ecological requirements.Such as
This one, the present invention can efficiently solve the most of technical problem currently existed in graphene dispersing solution processing procedure, with increase
Add yield, uniform product specification and increase suspension of the graphene in graphene dispersing solution.
Although the present invention is disclosed as above with embodiment, however, it is not to limit the invention, any technical field
Middle technical staff, without departing from the spirit and scope of the present invention, when can make a little change and retouch, therefore the protection of the present invention
Scope is when subject to as defined in claim.
Claims (26)
1. a kind of air flow-producing device, is used to prepare graphene powder, including：
External bushing, has chamber, air inlet openings and outlet opening, and the air inlet openings are communicated in the lower section of the chamber and institute
Outlet open communication is stated in the top of the chamber, wherein the chamber has necking section；And
Rotate awl, be arranged in the chamber, rotation awl and the chamber are conformal, and it is described rotate awl with it is described
There is slit spacing, wherein the rotating cone attached bag, which includes, rotates body and a plurality of screw thread, the screw thread between the inner wall of chamber
Top from the bottom of the rotation body towards the rotation body is spirally distributed on the outer surface of the rotation body,
When the rotation awl rotates in the cavity, generate upwards and have by the screw thread and the slit spacing
There is the cyclone of the component of horizontal direction.
2. air flow-producing device according to claim 1, wherein the top surface of rotating cone and the top of the necking section
Face flushes.
3. air flow-producing device according to claim 1, wherein the rotation body include the bottom, the top with
And the middle part between the bottom and the top, wherein the diameter for rotating body is from the bottom to the top
Sequentially successively decrease.
4. air flow-producing device according to claim 3, wherein the diameter of the bottom surface of the bottom is more than the bottom
The diameter of top surface.
5. air flow-producing device according to claim 4, wherein the diameter of the bottom surface at the middle part is more than the middle part
The diameter of top surface, and the diameter of the bottom surface at the middle part is equal to the diameter of the top surface of the bottom.
6. air flow-producing device according to claim 5, wherein the diameter of the bottom surface at the top is more than the top
The diameter of top surface, and the diameter of the bottom surface at the top is equal to the diameter of the top surface at the middle part.
7. air flow-producing device according to claim 1, wherein the section of rotating cone is in asterism shape.
8. air flow-producing device according to claim 1, wherein the range of speeds of rotating cone between 3000rpm extremely
7000rpm。
9. air flow-producing device according to claim 1, wherein the quantity of the screw thread is between 8 to 32.
10. air flow-producing device according to claim 9, wherein the quantity of the screw thread is between 12 to 18.
11. air flow-producing device according to claim 1, wherein the scope of the slit spacing is between 0.05 millimeter to 10
Millimeter.
12. air flow-producing device according to claim 11, wherein the scope of the slit spacing is between 0.1 millimeter to 1
Millimeter.
13. a kind of preparation method of graphene dispersing solution, including：
Homogenization processing procedure is carried out to graphene powder and processing solvent, to form graphene thickener；And
Thin layer processing procedure is carried out to the graphene thickener, to form graphene dispersing solution,
Wherein described graphene powder is using made by the air flow-producing device according to claim 1 to 12.
14. the preparation method of graphene dispersing solution according to claim 13, wherein the preparation side of the graphene powder
Method includes：
Continuous high speed is carried out to graphite former material toward calendering processing procedure is covered so that graphite predecessor is made, there is the graphite predecessor difference to arrange
Sliding Structures；
By horizontal direction compressed air stream the graphite predecessor is made to carry out intercalation, to form graphene and gas interlayer
Close object；
By the release of interlayer stream pressure the graphene is made to carry out expansion stripping reaction with gas intercalation compound, to form stone
Black alkene aggregation；And
The graphene aggregation is made to suspend in the gas flow to drift about and mutually collide, to generate graphene powder.
15. the preparation method of graphene dispersing solution according to claim 14, wherein each layer in the graphite predecessor
Between spacing beExtremely
16. the preparation method of graphene dispersing solution according to claim 14, wherein the horizontal direction compressed air stream
Wind speed is 0.3 Mach to mach one.
17. the preparation method of graphene dispersing solution according to claim 14, wherein the horizontal direction compressed air stream
Air quantity is 186CMM to 619CMM.
18. a kind of graphene dispersing solution, using the graphene dispersing solution according to claim 13 to 17 preparation method by
Made by graphene powder and processing solvent, the average piece footpath of the graphene in the graphene dispersing solution is 0.5 μm to 1 μm,
The number of plies is 3 to 5 layers, and solid content is 5% to 50%, and surface oxygen content is less than 1wt%, and the graphene dispersing solution is standing 12
Distributed density is presented by upper strata to the state of bottom increasing concentration after hour, and viscosity is 5000cps to 8000cps, and graphene is dense
It spends for 20wt%.
19. graphene dispersing solution according to claim 18, wherein the graphene dispersing solution is at the middle and upper levels between bottom
Concentration phase difference be 0.1wt% to 20wt%.
20. graphene dispersing solution according to claim 18, wherein the number of plies of the graphene powder is 5 to 10 layers.
21. graphene dispersing solution according to claim 18, wherein the average piece footpath of the graphene powder is 3 μm to 15
μm。
22. graphene dispersing solution according to claim 18, wherein the content of surface oxygen of the graphene powder is less than
0.1wt%.
23. graphene dispersing solution according to claim 18, wherein the processing solvent includes varsol, halogenated hydrocarbon
Solvent, alcohols solvent, phenol solvent, ketones solvent, ethers and acetals solvent, acids and anhydride solvent, nitrogenous compound
Solvent, sulfur-containing compound solvent, multifunctional group solvent or inorganic solvent.
24. graphene dispersing solution according to claim 18, wherein the interfacial tension scope of the processing solvent is 15mN/
M to 50mN/m, Hansen Solubility Parameter 5.0MPa0.5To 15MPa0.5。
25. graphene dispersing solution according to claim 18, wherein with the gross weight meter of the graphene dispersing solution, it is described
The additive amount of graphene powder is 0.001wt% to 30wt%.
26. graphene dispersing solution according to claim 18, wherein the polarity force parameter of the processing solvent is
0.5MPa0.5To 5.5MPa0.5, it is 7.0MPa to disperse force parameter0.5To 9.0MPa0.5, and hydrogen bond force parameter is 2.0MPa0.5Extremely
7.0MPa0.5。
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| TW105137506 | 2016-11-16 | ||
| TW105137512 | 2016-11-16 | ||
| TW105137505 | 2016-11-16 | ||
| TW105137512A TWI633055B (en) | 2016-11-16 | 2016-11-16 | Graphene powder floc and manufacturing method thereof |
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