CN110193329A - A kind of hypergravity coupling prepares the device of two-dimension nano materials - Google Patents
A kind of hypergravity coupling prepares the device of two-dimension nano materials Download PDFInfo
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- CN110193329A CN110193329A CN201910412425.6A CN201910412425A CN110193329A CN 110193329 A CN110193329 A CN 110193329A CN 201910412425 A CN201910412425 A CN 201910412425A CN 110193329 A CN110193329 A CN 110193329A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention relates to technical field of nanometer material preparation, to solve, inefficient energy consumption, single layer rate existing for conventional two-dimensional nano material preparation process are low, lamella size distribution is wide, the problem of low yield, provide the device that a kind of hypergravity coupling prepares two-dimension nano materials, concentration systems are recycled including cooling recirculation system, hypergravity recirculation gas stripper system and hypergravity, the hypergravity recirculation gas stripper system includes hypergravity coupling machine I, and the hypergravity coupling machine I is connected by pipeline with the first metering device, first driving device and cooling recirculation system；The hypergravity circulation concentration systems include hypergravity coupling machine II, and the hypergravity coupling machine II is connected by pipeline with the second metering device, the second driving device and conductivity measuring apparatus.The device of the invention structure is simple, and cooperation is compact, and efficiently, it can be achieved that three circulation synchronous are run, installation and removal are convenient for production, produces a variety of two-dimensional layer nano materials with can be realized large-scale low-cost.
Description
Technical field
The present invention relates to technical field of nanometer material preparation more particularly to a kind of hypergravity coupling to prepare two-dimension nano materials
Device.
Background technique
High-gravity technology is the new technology for strengthening multiphase flow transmitting and reaction process, due to its broad applicability and tool
Have that traditional equipment do not have it is small in size, light-weight, low energy consumption, Yi Yunzhuan, easy-maintaining, safe and reliable, flexible and more can
The advantages that adapting to environment, so that high-gravity technology has wide commercialization in the industrial circles such as environmental protection, material, biology, chemical industry
Application prospect.The basic principle of high gravity technology is the unique flow row using multiphase flow system under the conditions of super gravity field
To strengthen relative velocity between phase and phase and contacting with each other, to realize efficient momentum, quality and heat transfer process.
The mode for forming super gravity field is to form centrifugal force field by motor rotating machinery entirety or component.
Chinese patent discloses " a kind of method of efficient hypergravity removing two-dimension nano materials ", and notification number is
CN201811420442.6, which, which describes a kind of primary rotation is coupled with secondary rotating, generates once rotation
Positive and negative energy stream couple and be integrated with the positive and negative energy stream that secondary rotating generates, form four step mechanical energy drive systems: one
Secondary rotation negative energy stream → primary rotation positive energy stream → secondary rotating negative energy stream → secondary rotating positive energy stream.The first step is
Primary to rotate generated negative energy stream in material sucking secondary rotating runner, second step to the 4th step is the synchronous machine occurred
Tool energy conversion process, it may be assumed that the hypergravity potential → high-speed rotating kinetic energy of static energy → dien vertex.It is final the result is that hypergravity is latent
Energy almost all is converted into the high-speed rotating kinetic energy of dien vertex, the dissipation of mechanical energy is substantially not present, and then significantly reduce removing
The cooling power of refrigeration machine in the process, the method for realizing efficiently removing two-dimension nano materials.It is typically characterised by two-dimensional layer
The dispersion liquid of material enters the central inlet of high-speed rotating secondary rotating flow reactor by pipeline, from reactor outlet stream
Feed liquid out enters the entrance of tubular heat exchanger by pipeline, is back to and follows from the feed liquid of tubular heat exchanger outlet outflow
In ring storage tank, the number of plies is obtained after so recycling repeatedly in 3 layers of few layer two-dimension nano materials below.But pass through many experiments
This method is proved there are still clearly disadvantageous place, i.e., this dynamic high-speed rotating secondary rotating flow reactor is being removed
A large amount of microvesicle can be generated during graphene, static secondary rotating flow reactor can also generate during removing graphene
Microvesicle, but the amount of microvesicle is seldom.The microvesicle of generation is more, illustrates that the efficiency for removing graphene is lower, this is because graphite slurries
During with reactor wall strong friction, friction generates bubble ratio friction and separates that graphene is much easier, and static two
Secondary rotation flow reactor is to cross secondary rotating flow reactor inner wall by hydrostatic driving graphite slurry streams more than 2 megapascal, this
High static pressure significantly suppresses the generation of bubble, therefore, only in the position that reactor is close to the exit since static pressure very low yield is raw
Minimal amount of microvesicle.For dynamic high-speed rotating secondary rotating flow reactor, hypergravity potential energy difference between import and export
Have also exceeded 2 megapascal, but so high hypergravity potential energy almost all be converted into dien vertex high speed rotation needed for kinetic energy,
So static pressure is very low in reactor, the generation of a large amount of microvesicles can not be restrained.Experimental result shows that dynamic secondary rotating stream is anti-
Device is answered to reduce an order of magnitude or more than static secondary rotating flow reactor charge stripping efficiency.
Chinese patent discloses " a kind of method and apparatus of continuous hypergravity separation two-dimension nano materials ", and notification number is
CN201810575493.X, the invention describe a kind of continuous hypergravity separation two-dimensional nano material according to the design of U-tube principle
The graphite slurries of containing graphene are continuously injected into the central feeding mouth of hypergravity seperator, feed liquid by the method and apparatus of material
It is thrown away outward along U-tube channel, the graphite slurries of high concentration are thrown toward U-tube bottom and spray from outermost upper spout, low
The graphene solution of concentration is flowed against super gravity field direction in U-tube and is sprayed from lower spout in the inner part, upper and lower two kinds
The assignment of traffic of material is controlled by upper spout.But abundant experimental results show to be difficult to adopt traditional technical controlling it is continuously overweight
The assignment of traffic of power seperator, this is because the pressure that upper spout sprays material is more than 2 megapascal, and graphite in graphite slurries
Size distribution reaches mm-scale, this requires spout be also sized to reach mm-scale, 2 megapascal pressure effect under milli
The spout of metrical scale is difficult the flow control of graphite slurries in lower range of flow.
Chinese patent discloses " a kind of device and method of continuous hypergravity diafiltration separation two-dimension nano materials ", bulletin
Number be CN201810752331.9, the invention describe it is a kind of using hypergravity rotating particles bed by two evenly dispersed wieners
The inner surface that rice thin slice is gathered in rotation bed forms soft aggregate and isolates the removing solvent that can be recycled, then by washing lotion
Full of in revolving bed device, in the case where revolving bed low speed rotates and reverse effect, suspension is formed, it is soft to take off wash-off two-dimension nano materials
Soft aggregate aggregation is concentrated and separated out by aggregate with hypergravity centrifugal separating device.But abundant experimental results show to adopt
The graphene product separated in this way, impurity content is high and is difficult to be separated off.
Summary of the invention
The present invention provides hypergravity coupling and prepares two-dimension nano materials to overcome shortcomings existing for foregoing invention
Device, the apparatus structure is simple, cooperate it is compact, can it is quick, energy-efficient, low-cost, high-volume, in high quality produce it is more
Kind two-dimensional layer nano material.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of hypergravity coupling prepares the device of two-dimension nano materials, including cooling recirculation system, hypergravity recirculation gas stripper system
Concentration systems are recycled with hypergravity, the hypergravity recirculation gas stripper system includes hypergravity coupling machine I, the hypergravity coupling machine
I is connected by pipeline with the first metering device, first driving device and cooling recirculation system；The hypergravity circulation concentration system
System includes hypergravity coupling machine II, the hypergravity coupling machine II by pipeline and the second metering device, the second driving device and
Conductivity measuring apparatus is connected.
The device of the invention is applied to hypergravity coupling technique and prepares two-dimension nano materials, and the two-dimensional layer material is the
Four to the 6th main group semiconducting compounds (such as GaSe, SnS), transition metal halide (such as PbI2、MgBr2), metal oxide
(such as MnO2、MoO3), it is hexagonal boron nitride (white graphite alkene), graphite phase carbon nitride, transition metal carbide, carbonitride, the 4th main
Race's graphene analog (semimetal silene, germanium alkene), the honeycomb binary compound (such as SiC, SnGe) of the 4th major element,
Three to the 6th main group compounds (such as InSb, GaN), the 5th major element (such as phosphorus alkene, arsenic alkene and antimony alkene), silicate, aluminosilicate
One of the charge balance diaphragm plate (such as mica, clay) of salt, stratiform hydrotalcite.
The core of apparatus of the present invention is hypergravity coupling technique, and " hypergravity coupling " of the present invention refers to hypergravity point
Be coupled from process and mixed process, although hypergravity coupling machine can be separated but also be mixed, separation with mix it is necessary
Know the secondary from the primary.Therefore, graphene preparation process is divided into two serum recycle processes i.e. by the device of the invention: recirculation gas stripper with follow
Ring concentration process.The present invention is used for recirculation gas stripper process using hypergravity coupling machine I, using hypergravity coupling machine II for recycling
Concentration process.Hypergravity coupling machine I is based on removing, supplemented by separation, because from thermodynamics, efficient stripping process
It is unable to do without efficient separation process.Hypergravity coupling machine II then with separation based on, supplemented by mixing, because going out from aerodynamic point
Hair, efficient separation process be unable to do without efficient mixed process.The present invention is finally by two by the way of a solution systemic circulation
A serum recycle system is unified for an operation architecture, as shown in Figure 5.
Preferably, the hypergravity coupling machine I and hypergravity coupling machine I all have the turntable of streamlined structure, it is described
Turntable includes the hypergravity mixed cell set on internal hypergravity separative unit and set on outside.
Preferably, the hypergravity separative unit is to fasten the U formed by double-sided symmetrical rotary blade and upper and lower lids
Shape pipe structure；The hypergravity mixed cell is the secondary rotating runner knot formed by the groove opened up opposite in upper and lower lids
Structure.
Preferably, the two sides of the bottom of the U-tube are equipped with concentrated slurry discharge port, the concentrated slurry discharge port and two
Secondary eddy channel is connected；The bottom centre of the U-tube is equipped with slurry feed mouth；The U-tube of the hypergravity coupling machine I
Open end two sides are equipped with weak solution discharge port；The open end two sides of the U-tube of the hypergravity coupling machine II go out equipped with stripper
Material mouth.For removing graphene, the weak solution discharge port of the open end two sides of the U-tube of the hypergravity coupling machine I flows out
Be graphene weak solution；The open end two sides of the U-tube of the hypergravity coupling machine II stripper discharge port outflow be
Graphene stripper.
" hypergravity coupling machine " of the present invention is that continuous hypergravity separative unit and mixed cell are coupled
Disc equipment, the hypergravity separative unit be buckled together by double-sided symmetrical rotary blade and upper and lower lids formed it is super
Gravity U-tube structure, the hypergravity mixed cell are that the secondary rotating runner for accelerating rotation is carved out in upper and lower lids,
Separative unit occupy center, and mixed cell occupy outside, as shown in Figure 2.The advantages of this coupled modes, is: first, separation
Unit provides for mixed cell be sufficiently used for removing two-dimension nano materials needed for static pressure, inhibit a large amount of microvesicles in stripping process
Generate and then improve the efficiency of removing two-dimensional layer material；Second, the secondary rotating runner of mixed cell can be with stability contorting point
Assignment of traffic from unit, and pasty material is made to stablize outflow, it not will cause the blocking of pasty material.Material enters overweight couple of force
It is first to separate the order remixed in conjunction machine, with regular turn on the contrary, only circulating, can just returns to regular turn, therefore,
The present apparatus prepares two-dimension nano materials using Matter Transfer mode.
Preferably, the flow area of the secondary rotating runner is the circle of 2 ~ 6mm of diameter, the secondary rotating runner
Radical length be 30 ~ 120mm.Preferably, the radial dimension of secondary rotating runner is greater than super in the hypergravity coupling machine I
One times of radial dimension of secondary rotating runner or more in gravity coupling machine II.This difference determines the different effect of the two, preceding
Person focuses on removing two-dimensional nano stratified material, and the latter focuses on concentration two-dimensional nano stratified material.It is preceding when being run under equal-wattage
Person's radial dimension is big, and revolving speed is low；The latter's radial dimension is small, and revolving speed is high.
Hypergravity coupling machine I is that separative unit structure is identical with something in common of the II in structure, difference
Be that the structure of mixed cell is similar but not identical, the two secondary rotating flow passage structure is similar, but the radial dimension of runner the former
It is one times or more of the latter.
Preferably, if the double-sided symmetrical rotary blade tow sides are radially equipped with dry plate impeller, adjacent fan-wheel it
Between be equipped with liquor inlet.
Preferably, the maximum hypergravity when hypergravity coupling machine I and hypergravity coupling machine II are once rotated
Field intensity is lower than 6000g.
More preferably, maximum super gravity field strength control when hypergravity coupling machine I and II is once rotated exists
2500~5000g。
Preferably, during preparing two-dimension nano materials hypergravity coupling machine I rotating ratio hypergravity coupling machine II
At least low 1000 rpm of revolving speed.When the motor peak power output of hypergravity coupling machine I and II is identical, hypergravity coupling machine
II rotating ratio hypergravity coupling machine I is at least higher by 1000 rpm, i.e. the separating capacity of hypergravity coupling machine II is apparently higher than super
Gravity coupling machine I, but mixed is markedly less than hypergravity coupling machine I.
Preferably, the mode that the method that the hypergravity coupling prepares two-dimension nano materials carries out scale amplification is to divide
It is scaled up under the premise of being remained unchanged from unit super gravity field intensity.
Preferably, the cooling recirculation system includes coolant circulation pump and heat exchanger.
Therefore, the invention has the following beneficial effects: the devices that hypergravity coupling of the invention prepares two-dimension nano materials
Structure is simple, and cooperation is compact, and efficiently, it can be achieved that three circulation synchronous are run, installation and removal are convenient for production, can be realized on a large scale
A variety of two-dimensional layer nano materials are produced at low cost.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram that hypergravity coupling prepares two-dimension nano materials device.
Fig. 2 is the structural schematic diagram of hypergravity coupling machine I and hypergravity coupling machine II.
Fig. 3 is the structural schematic diagram of the secondary rotating runner inside turntable.
Fig. 4 is the schematic perspective view of double-sided symmetrical rotary blade.
Fig. 5 is three circulation theory schematic diagrames.
Fig. 6 is the SEM stereoscan photograph that resulting graphene is removed using the device of embodiment 1.
Fig. 7 is to remove the resulting powerful SEM stereoscan photograph of graphene using the device of embodiment 1.
Fig. 8 is to remove resulting graphene AFM atomic force microscopy using the device of embodiment 1.
Fig. 9 is the correspondence graphene thickness map of Fig. 8.
Figure 10 is graphite raw material, ultrasound removing and removes resulting graphene XRD comparison diagram using the device of embodiment 1.
In figure: double-sided symmetrical rotary blade 1, concentrated slurry discharge port 2, secondary rotating runner 3, stripper (weak solution) go out
Material mouth 4, hypergravity separative unit 5, hypergravity mixed cell 6, refrigerating cycle pump 7, tubular heat exchanger 8, the first magnetic drive pump 9,
First measuring tank 10, hypergravity coupling machine I 11, hypergravity coupling machine II 12, the second measuring tank 13, the second magnetic drive pump 14, electricity
Conductance meter 15, motor 16, fluid flowmeter 17, turntable 18, upper cover plate 19, lower cover plate 20, liquor inlet 21, slurry feed
Mouth 22.
Specific embodiment
Below by specific embodiment, and in conjunction with attached drawing, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
Embodiment 1
As shown in Figure 1, a kind of hypergravity coupling prepares the device of two-dimension nano materials, including by refrigerating cycle pump 7 and shell and tube
Cooling recirculation system, hypergravity recirculation gas stripper system and the hypergravity that heat exchanger 8 is constituted recycle concentration systems, hypergravity circulation stripping
It include the hypergravity coupling being connected by pipeline with the first measuring tank 10, the first magnetic drive pump 9 and cooling recirculation system from system
Machine I 11；It includes passing through pipeline and the second measuring tank 13, the second magnetic drive pump 14 and conductivity measurement that hypergravity, which recycles concentration systems,
The hypergravity coupling machine II 12 that meter 15 is connected.
As shown in Fig. 2, hypergravity coupling machine I and hypergravity coupling machine II all have the turntable 18 of streamlined structure and generate
The motor 16 of power, turntable include the hypergravity mixed cell 6 set on internal hypergravity separative unit 5 and set on outside.It is super
Gravity Separation unit is to fasten the U-tube formed by double-sided symmetrical rotary blade 1 and upper cover plate 19, lower cover plate 20；Hypergravity is mixed
Closing unit is the secondary rotating runner 3(that is formed by the groove opened up opposite on upper cover plate 19, lower cover plate 20 referring to Fig. 3), it is overweight
The bottom centre of the U-tube of power coupling machine I and hypergravity coupling machine II is equipped with slurry feed mouth 22, and the two sides of the bottom of U-tube are set
There is the concentrated slurry discharge port 2 being connected with secondary rotating runner, wherein the open end two sides of I U-tube of hypergravity coupling machine are set
There is weak solution discharge port 4, the open end two sides of I U-tube of hypergravity coupling machine are equipped with stripper discharge port 4；Hypergravity coupling machine I
Secondary rotating runner flow area be 2.5 mm circular cross-section of diameter, radical length be 60 mm；Hypergravity coupling machine II is right
The flow area answered is the circular cross-section of 2.0 mm, and radical length is 30 mm；Separative unit include double-sided symmetrical rotary blade and
Hypergravity disengagement chamber；As shown in figure 4, double-sided symmetrical impeller tow sides are respectively provided with 12 impellers, one is equipped between adjacent fan-wheel
A liquor inlet 21 amounts to 12.Maximum super gravity field strength control when hypergravity coupling machine I and II is once rotated exists
2500~5000g.The revolving speed of the rotating ratio hypergravity coupling machine II of hypergravity coupling machine I during preparing two-dimension nano materials
At least low 1000 rpm.
Hypergravity coupling of the invention prepares the application method of the device of two-dimension nano materials are as follows:
(1) as shown in Figure 1, opening refrigerating cycle step: flake graphite stock dispersion is obtained into graphite slurries in dispersion liquid, it should
Slurries pour into the first measuring tank 10, open refrigerating cycle pump 7 and first magnetic drive pump 9, make slurries in tubular heat exchanger 8 and the
Circulating cooling flows between one measuring tank 10, so that slurry temperature is down to -2 DEG C, the concentration of low temperature graphene slurries is controlled 3.0
g/L。
(2) as shown in figure 5, opening three circulation steps:
The step includes that circulation concentration and one of two partial circulatings, that is, graphite slurries recirculation gas stripper with graphene slurries follow greatly
The circulation of ring, that is, between stripper and graphene solution, three circulation synchronous carry out.
There is the removing balance between graphite and graphene during recirculation gas stripper, graphite slurries are in the first measuring tank
10, it is circulated between tubular heat exchanger 8 and hypergravity coupling machine I 11, graphite slurries enter in hypergravity coupling machine I 11
The graphene solution of low concentration and the graphite slurries of high concentration are first isolated, the two flow is close, the low concentration stone separated
Black alkene solution flows into hypergravity coupling machine II 12 and carries out circulation concentration.
The graphite slurries of high concentration continue flow through the secondary rotating runner in hypergravity coupling machine I 11 and separate new stone
Black alkene is then back in the first measuring tank 10, is flowed out in the first measuring tank 10 and in hypergravity coupling machine II 12
Stripper mixed diluting is updated to recirculation gas stripper, feed liquid every circulation removing in one week balance close to original content, is then constantly carried out
Twice, since graphite concentration can persistently drop, the graphite slurries of new high concentration are required supplementation with, feeding manner can choose continuously
Charging or intermittent feeding.
At the same time, circulation concentration process is also in quick carry out, and graphene slurries are in the second measuring tank 13, liquid flow
Concentration is recycled between meter, conductivity meter 15 and hypergravity coupling machine II 12, there is single point in circulation concentration process
Adsorption equilibrium between scattered graphene and graphene soft aggregate, the flow and conductivity of slurries are synchronized in monitoring, graphite
After alkene slurries enter hypergravity coupling machine II 12, the graphene slurry close to colorless and transparent stripper and high concentration is first isolated
Liquid, stripper flow back into recirculation gas stripper process, and the graphene slurry stream of high concentration enters the secondary rotating of hypergravity coupling machine II
The graphene cluster of very little is dispersed into runner, these graphene clusters and low concentration graphene solution after mixing, jointly
It is imported into the second measuring tank 10, the graphene of the graphene cluster quick adsorption free state dispersed in the process makes graphite
The graphene concentration of free state quickly reduces in alkene slurries, then constantly carries out circulation concentration, and the every circulation of feed liquid is adsorbed for one week
Balance updates twice, and in order to stablize the concentration of graphene slurries, needing to discharge the graphene slurries of some high concentrations, (graphene contains
Measure about 1 g/L), discharge method can choose continuous discharge or intermittent take-off.
In hypergravity coupling machine II, the flow of the graphene slurries and stripper that are concentrated is close；The axis of graphene slurries
To average linear velocity 50m/s.Temperature control is at -2 to -4 DEG C in stripping process；Temperature control is at 2 to 4 DEG C in concentration process.
As shown in Fig. 2, what the concentrated slurry discharge port 2 of hypergravity coupling machine I flowed out is the graphite of concentration in preparation process
Thick slurries, what is entered from the slurry feed mouth 22 of U-tube bottom centre is graphite slurries, is from what weak solution discharge port 4 flowed out
Graphene weak solution.What the concentrated slurry discharge port 2 of the U-tube bottom of hypergravity coupling machine II flowed out be concentration graphene it is thin
Slurries, what is entered from the slurry feed mouth 22 at the top of U-tube is graphene screened stock liquid, and what is flowed out from stripper discharge port 4 is stone
Black alkene stripper.During preparing graphene, the revolving speed of hypergravity coupling machine I and II are respectively 4500 rpm and 5500rpm,
It is normal gravity field that highest super gravity field level, which is respectively 3170 g and 4733 g(g, inside separative unit both under this revolving speed
Acceleration).
The few layer of graphene removed to the device for preparing two-dimension nano materials using the embodiment hypergravity coupling is done
Characterization:
Fig. 6 and Fig. 7 is the SEM electromicroscopic photograph of graphene.
Fig. 8 is the graphene AFM atomic force microscopy of device removing, and Fig. 9 is corresponding graphene sheet layer thickness
Curve graph, as can be seen from Figure 9 the thickness of graphene nanometer sheet is less than 1 nm, and theoretically the graphene of single layer is with a thickness of 0.34
Nm, if the number of plies for counting graphene in interlamellar spacing figure in is two layers.It is characterized by atomic force microscope it can be proved that passing through hypergravity
Coupled method can obtain few layer graphene of the lateral dimension greater than 2 μm (majority is double-deck or three layers of graphene).
Figure 10 is the graphene XRD comparison diagram of graphite raw material, ultrasound removing and device removing, as can be seen from the figure stone
Black alkene almost disappears in (004) face of 55 degree of position graphite, illustrates that it stacks the ordered structure in dimension in longitudinal direction and is disturbed, from
And demonstrate Multi-layer graphite and be stripped as few layer or single-layer graphene, the graphene that ultrasonic method is removed with hypergravity coupled method is surveyed
XRD result is consistent.
Embodiment 2
During preparing graphene, the highest super gravity field level that the separative unit of hypergravity coupling machine I and II once rotates still is divided
It Wei not 3170 g and 4733 g.Embodiment 2 the difference from embodiment 1 is that: the stream of secondary rotating runner in hypergravity coupling machine I
Logical section is the circle of diameter 2mm, radical length 120mm, the radial dimension of secondary rotating stream runner in hypergravity coupling machine I
It is radial dimension of 1.5 times of secondary rotating stream runner in hypergravity coupling machine II.Graphite concentrated slurry and low concentration graphene
The flow-ratio control of solution is in 0.5:1；The axial average linear velocity of graphite concentrated slurry reaches 65 m/s.Temperature in stripping process
Control is at -4 DEG C；Temperature control is at 1 DEG C in concentration process.In step (1), the concentration of low temperature graphene slurries is controlled in 6.0g/
L, remaining processing step and parameter are identical.
Embodiment 3
During preparing graphene, the highest super gravity field level that the separative unit of hypergravity coupling machine I and II once rotates still is divided
It Wei not 3170 g and 4733 g.Embodiment 3 the difference from embodiment 1 is that: the stream of secondary rotating runner in hypergravity coupling machine I
Logical section is the circle of diameter 6mm, radical length 120mm, the radial dimension of secondary rotating stream runner in hypergravity coupling machine I
It is radial dimension of 2 times of secondary rotating stream runner in hypergravity coupling machine II；, graphite underflow liquid and low concentration graphene solution
Flow-ratio control in 2:1；65 m/s of axial average linear velocity of graphene slurries.Temperature control is at -3 DEG C in stripping process；
Temperature control is at 2 DEG C in concentration process.In step (1), the concentration control of low temperature graphene slurries is in 9.0g/L, remaining technique step
Rapid and parameter is identical.The performance and embodiment 1 for the few layer of graphene that embodiment 2-3 is removed are quite, no longer superfluous herein
It states.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, and is not surpassing
There are also other variations and modifications under the premise of technical solution documented by claim out.
Claims (10)
1. the device that a kind of hypergravity coupling prepares two-dimension nano materials, which is characterized in that including cooling recirculation system, hypergravity
Recirculation gas stripper system and hypergravity recycle concentration systems, and the hypergravity recirculation gas stripper system includes hypergravity coupling machine I, described
Hypergravity coupling machine I is connected by pipeline with the first metering device, first driving device and cooling recirculation system；It is described overweight
Power circulation concentration systems include hypergravity coupling machine II, and the hypergravity coupling machine II passes through pipeline and the second metering device, the
Two driving devices are connected with conductivity measuring apparatus.
2. the device that a kind of hypergravity coupling according to claim 1 prepares two-dimension nano materials, which is characterized in that described
Hypergravity coupling machine I and hypergravity coupling machine II all have the turntable of streamlined structure, and the turntable includes surpassing set on internal
Gravity Separation unit and hypergravity mixed cell set on outside.
3. the device that a kind of hypergravity coupling according to claim 2 prepares two-dimension nano materials, which is characterized in that described
Hypergravity separative unit is to fasten the U-tube structure formed by double-sided symmetrical rotary blade and upper and lower lids；The hypergravity is mixed
Closing unit is the secondary rotating flow passage structure formed by the groove opened up opposite in upper and lower lids.
4. the device that a kind of hypergravity coupling according to claim 3 prepares two-dimension nano materials, which is characterized in that described
The two sides of the bottom of U-tube are equipped with concentrated slurry discharge port, and the concentrated slurry discharge port is connected with secondary rotating runner；It is described
The bottom centre of U-tube is equipped with slurry feed mouth；The open end two sides of the U-tube of the hypergravity coupling machine I are equipped with weak solution
Discharge port；The open end two sides of the U-tube of the hypergravity coupling machine II are equipped with stripper discharge port.
5. the device that a kind of hypergravity coupling according to claim 3 prepares two-dimension nano materials, which is characterized in that described
The flow area of secondary rotating runner is the circle of 2 ~ 6mm of diameter, and the radical length of the secondary rotating runner is 30 ~ 120mm.
6. the device that a kind of hypergravity coupling according to claim 3 prepares two-dimension nano materials, which is characterized in that described
The radial dimension of secondary rotating runner is greater than the radial ruler of secondary rotating runner in hypergravity coupling machine II in hypergravity coupling machine I
Very little one times or more.
7. the device that a kind of hypergravity coupling according to claim 3 prepares two-dimension nano materials, which is characterized in that described
If double-sided symmetrical rotary blade tow sides are radially equipped with dry plate impeller, liquor inlet is equipped between adjacent fan-wheel.
8. the device that a kind of hypergravity coupling according to claim 1 prepares two-dimension nano materials, which is characterized in that described
The maximum super gravity field intensity of hypergravity coupling machine I and hypergravity coupling machine II is lower than 6000g.
9. the device that a kind of hypergravity coupling according to claim 1 prepares two-dimension nano materials, which is characterized in that making
During standby two-dimension nano materials, the revolving speed at least low 1000 of the rotating ratio hypergravity coupling machine II of the hypergravity coupling machine I
rpm。
10. a kind of -9 any hypergravity couplings prepare the device of two-dimension nano materials according to claim 1, feature exists
In the cooling recirculation system includes coolant circulation pump and heat exchanger.
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