CN106185910A - Prepare the device and method of Graphene - Google Patents
Prepare the device and method of Graphene Download PDFInfo
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- CN106185910A CN106185910A CN201610614095.5A CN201610614095A CN106185910A CN 106185910 A CN106185910 A CN 106185910A CN 201610614095 A CN201610614095 A CN 201610614095A CN 106185910 A CN106185910 A CN 106185910A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 85
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 70
- 239000010439 graphite Substances 0.000 claims abstract description 70
- 239000002002 slurry Substances 0.000 claims abstract description 55
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 42
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 230000000694 effects Effects 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 238000005452 bending Methods 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 3
- UZIQYAYUUNMDMU-UHFFFAOYSA-N N.[Br+] Chemical compound N.[Br+] UZIQYAYUUNMDMU-UHFFFAOYSA-N 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000011859 microparticle Substances 0.000 abstract description 3
- 239000000725 suspension Substances 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 238000001069 Raman spectroscopy Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229960002233 benzalkonium bromide Drugs 0.000 description 2
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The device and method preparing Graphene of the present invention, wherein, prepare the device of Graphene, including the first container, second container and the micro-reaction channel being arranged between the first container, second container, temperature controlled ultrasonic equipment, also include the first peristaltic pump and the second peristaltic pump.The method preparing Graphene of the present invention, including: preparation graphite slurry；Make graphite slurry under the conveying of the first peristaltic pump, enter micro-reaction channel from container, be incubated and after ultrasonic release effect, enter second container.Technical scheme simple in construction, efficiency are higher.Gathering to ultrasonic energy in hydrodynamic shear when technical scheme flows in micro-reaction channel by graphite microparticles suspension and micro-reaction channel, it is achieved the preparation of small flake diameter Graphene.Graphene quality prepared by technical scheme is high.
Description
Technical field
The present invention relates to the preparation of carbon, particularly relate to a kind of device and method preparing Graphene.
Background technology
Graphene is with sp by carbon atom2The monolayer two-dimensional atomic crystal that hybrid orbital is arranged by honeycomb crystal lattice.
Graphene is the thinnest, the most tough and tensile known nano material, and its hardness exceedes diamond；Single-layer graphene is the most fully transparent, only has
The absorbance of 2.3%；Heat conductivity is up to 5300W/m K, and resistivity only has 10-6 Ω cm, is the most excellent heat and electricity
Conductor.Graphene, because of the physicochemical property of its excellence, has important research and using value in many applications.Graphene exists
Being mainly graphene film and two kinds of forms of graphene powder in research and application, wherein the application with graphene powder is the widest
General.Graphene high-efficiency, high-quality, the preparation of low cost are the bases realizing Graphene commercial Application.
The preparation method of graphene powder includes mechanical stripping method, graphene oxide reducing process, electrochemical stripping method at present,
Wherein high with the powder quality prepared by mechanical stripping method, exist almost without oxygen-containing functional group.Ultrasonic wave added is peeled off and mechanical shear
Cutting stripping is the method for main flow in mechanical stripping method, but both approaches all Shortcomings.Mechanical shearing stripping method productivity is low, super
Sound up-stripping method, due to intergranular a large amount of stackings, is peeled off time-consuming, thus efficiency is relatively low.
Summary of the invention
The technical problem to be solved in the present invention is to provide the device and method preparing Graphene that a kind of efficiency is higher.
The device preparing Graphene of the present invention, including:
For containing the first container and the second container of graphite slurry；
The micro-reaction channel being arranged between the first container, second container；
Be arranged between the first container, second container for controlling micro-reaction channel internal temperature and super for sending
Sound wave makes the temperature controlled ultrasonic equipment that the graphite slurry in micro-reaction channel is peeled off；
Being provided with the first peristaltic pump between first container and micro-reaction channel, the first peristaltic pump is for by the first container
Graphite slurry through micro-reaction channel pump to second container；
Being provided with the second peristaltic pump between second container and micro-reaction channel, the second peristaltic pump is for by second container
Graphite slurry through micro-reaction channel pump to the first container.
The device preparing Graphene of the present invention, wherein, temperature controlled ultrasonic equipment includes:
For containing water and the water bath containers of micro-reaction channel；
For the heater heated for the water in water bath containers, it is arranged at the outside of water bath containers；
For controlling the temperature controller of the temperature of the water within water bath containers, it is connected with heater；
For sending the excusing from death wave producer that the graphite slurry in ultrasound wave makes micro-reaction channel is peeled off, it is arranged at water-bath and holds
The inside of device.
The device preparing Graphene of the present invention, wherein, wriggled by pipeline and first in one end of described micro-reaction channel
Pump connects, and the other end of described micro-reaction channel is connected by pipeline and the second peristaltic pump, and described micro-reaction channel includes multiple
The vertical section vertically extended and multiple bending segment, each described bending segment connects adjacent vertical section, so that described
Micro-reaction channel is at the inside bending extension of described water bath containers.
The method preparing Graphene of the present invention, including:
Step one, preparation graphite slurry；
Step 2, make graphite slurry under the conveying of the first peristaltic pump, from first container enter micro-reaction channel, insulation also
After ultrasonic release effect, entering second container, keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic equipment sends
Ultrasound wave makes the graphite slurry in micro-reaction channel peel off, ultrasonic power 360W.
The method preparing Graphene of the present invention, wherein, also includes: step 3, treat in the first container graphite slurry input
Complete, and second container no longer has liquid enter, close the first peristaltic pump, open the second peristaltic pump, make graphite slurry pass through
Second peristaltic pump reaction channel in a subtle way, keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic equipment sends ultrasound wave
Make the graphite slurry in micro-reaction channel peel off, ultrasonic power 360W, make graphite slurry under the conveying of the second peristaltic pump, from
Two containers enter micro-reaction channel, are incubated and after ultrasonic release effect, enter the first container.
The method preparing Graphene of the present invention, wherein, also includes: repeating said steps two, step 3.
The method preparing Graphene of the present invention, wherein, described step one is prepared graphite slurry and is included: isopropanol mixes with water
Cooperation solvent, isopropanol is 3:7 with the volume ratio of water, adds the solvent volume benzalkonium bromide solution than 10% and makees dispersant,
Described solvent and dispersant are added 15000 mesh Graphene powder, and making graphite solid weight content is 5%, and magnetic agitation makes graphite
Slurry is uniformly dispersed.
Technical scheme simple in construction, efficiency are higher.Technical scheme provides a kind of in micro-reaction
The method and apparatus in passage, Graphene being carried out ultrasonic stripping.Technical scheme by graphite microparticles suspension micro-
Gathering to ultrasonic energy in hydrodynamic shear when flowing in reaction channel and micro-reaction channel, it is achieved small flake diameter Graphene
Preparation.Graphene quality prepared by technical scheme is high, almost without oxy radical.
Accompanying drawing explanation
Fig. 1 is the structural representation of the device preparing Graphene of the present invention；
Fig. 2 be the method preparing Graphene of the present invention embodiment in the electron scanning micrograph of graphite raw material；
Fig. 3 is that the scanning electron microscope of the Graphene product in the embodiment of the method preparing Graphene of the present invention is shone
Sheet；
Fig. 4 is the graphite raw material powder body used in the embodiment of the method preparing Graphene of the present invention and prepared by Graphene
The Raman collection of illustrative plates of product.
Detailed description of the invention
As it is shown in figure 1, the device preparing Graphene of the present invention, including:
For containing the first container 11 and the second container 12 of graphite slurry；
It is arranged at the micro-reaction channel 1 between the first container 11, second container 12；
Be arranged between the first container 11, second container 12 for control micro-reaction channel 1 internal temperature and for
Send the temperature controlled ultrasonic equipment 2 that ultrasound wave makes the graphite slurry in micro-reaction channel 1 peel off；
Being provided with the first peristaltic pump 21 between first container and micro-reaction channel, the first peristaltic pump 21 is for by the first container
Graphite slurry in 11 through micro-reaction channel 1 pump to second container 12；
Being provided with the second peristaltic pump 22 between second container and micro-reaction channel, the second peristaltic pump 22 is for by second container
Graphite slurry in 12 through micro-reaction channel 1 pump to the first container 11.
The device preparing Graphene of the present invention, wherein, temperature controlled ultrasonic equipment 2 includes:
For containing the water bath containers 5 of water and micro-reaction channel 1；
For the heater 6 heated for the water in water bath containers 5, it is arranged at the outside of water bath containers 5；
For controlling the temperature controller 7 of the temperature of the water within water bath containers 5, it is connected with heater 6；
For sending the excusing from death wave producer 8 that the graphite slurry in ultrasound wave makes micro-reaction channel 1 is peeled off, it is arranged at water-bath
The inside of container 5.
The device preparing Graphene of the present invention, wherein, pipeline and the first peristaltic pump 21 are passed through in one end of micro-reaction channel 1
Connect.The other end of micro-reaction channel 1 is connected by pipeline and the second peristaltic pump 22.
One end of first flexible pipe 31 is vertically stretched in the first container 11, the other end of the first flexible pipe 31 and the first peristaltic pump 21
Connecting, one end of the second flexible pipe 32 is vertically stretched in second container 12, and the other end of the second flexible pipe 32 and the second peristaltic pump 22 are even
Connect.
Micro-reaction channel 1 includes multiple vertical section 101 vertically extended and multiple bending segment 102, each curved
Trisection 102 connects adjacent vertical section 101, so that micro-reaction channel 1 is at the inside bending extension of water bath containers 5.
The method preparing Graphene of the present invention, including:
Step one, preparation graphite slurry；
Step 2, make graphite slurry under the conveying of the first peristaltic pump, from first container enter micro-reaction channel, insulation also
After ultrasonic release effect, entering second container, keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic equipment sends
Ultrasound wave makes the graphite slurry in micro-reaction channel peel off, ultrasonic power 360W.
The method preparing Graphene of the present invention, wherein, also includes: step 3, treat in the first container graphite slurry input
Complete, and second container no longer has liquid enter, close the first peristaltic pump, open the second peristaltic pump, make graphite slurry pass through
Second peristaltic pump reaction channel in a subtle way, keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic equipment sends ultrasound wave
Make the graphite slurry in micro-reaction channel peel off, ultrasonic power 360W, make graphite slurry under the conveying of the second peristaltic pump, from
Two containers enter micro-reaction channel, are incubated and after ultrasonic release effect, enter the first container.
The method preparing Graphene of the present invention, wherein, also includes: repeating said steps two, step 3.
The method preparing Graphene of the present invention, wherein, step one is prepared graphite slurry and is included: isopropanol mixes work with water
Solvent, isopropanol is 3:7 with the volume ratio of water, adds the solvent volume benzalkonium bromide solution than 10% and makees dispersant, by institute
Stating solvent and add 15000 mesh Graphene powder with dispersant, making graphite solid weight content is 5%, and magnetic agitation makes graphite slurry
It is uniformly dispersed.
The embodiment of the method preparing Graphene of the present invention is as follows:
One, preparation graphite slurry:
Isopropanol mixes with water makees solvent, and isopropanol is 3:7 with the volume ratio of water, adds the solvent volume benzene than 10%
Prick bromine ammonium salt solution and make dispersant, described solvent and dispersant are added 15000 mesh Graphene powder, make the graphite solid weight content be
5%, magnetic agitation makes graphite slurry be uniformly dispersed.
Two, graphite is peeled off: suspended aqueous graphite slurry is under the conveying of the first peristaltic pump, micro-instead from the first container entrance
Answering passage, be incubated and after ultrasonic release effect, enter second container, keeping the temperature in micro-reaction channel is 10 DEG C, temperature
Control ultrasonic device sends the graphite slurry stripping in ultrasound wave makes micro-reaction channel, ultrasonic power 360W, treats stone in the first container
Ink slurry input is complete, and no longer has liquid to enter in second container, closes the first peristaltic pump, opens the second peristaltic pump, make stone
Ink slurry is by the second peristaltic pump reaction channel in a subtle way, and keeping the temperature in micro-reaction channel is 10 DEG C, temperature controlled ultrasonic equipment
Send the graphite slurry stripping in ultrasound wave makes micro-reaction channel, ultrasonic power 360W, make graphite slurry at the second peristaltic pump
Under conveying, enter micro-reaction channel from second container, be incubated and after ultrasonic release effect, enter the first container；On repeating
State conveying, stripping process, until obtaining satisfactory Graphene sample.
Prepared Graphene granule-morphology is as it is shown on figure 3, Fig. 2, Fig. 3 are graphite raw material powder body used and prepared by Graphene
The SEM photograph of product, it can be seen that graphite raw material granule is the irregular blocky-shaped particle of 3-5 μm, prepared Graphene
The sheet number of plies of granule is less than 10 layers, and for multi-layer graphene granule and be flake-shaped particles, < 10nm shows the thickness of graphene film
Graphite granule can effectively be peeled off and prepare graphene powder by technical scheme.
Fig. 4 is the Raman collection of illustrative plates that graphite raw material powder body used and Graphene prepare product, and Raman collection of illustrative plates is to characterize Graphene
The effective means of material.In Raman figure, D, G and 2D peak is the Characteristic Raman peak of graphite and grapheme material, and 2D peak is at transverse axis
Position is to judge the important evidence whether prepared material is Graphene.The 2D peak position of graphite material Raman collection of illustrative plates is set to
2710cm-1, peak type is asymmetric.Grapheme material 2D peak-to-peak position is near 2680cm-1, and peak type is symmetrical, can from figure
Going out, the 2D peak-to-peak position of prepared Graphene product is at 2679cm-1, and peak type symmetry is good, then can determine that prepared product is stone
Ink alkene powder body.Knowable to the intensity at D peak, it is low that Graphene prepares product degree of imperfection, maintains the degree of crystallinity of pure phase graphite composite powder, institute
The quality of the product of preparation is higher.
The method preparing Graphene of the present invention, wherein, graphite raw material can be the graphite powder less than 15000 mesh sheet footpaths,
Expanded graphite, crystalline flake graphite or graphite oxide.
The method preparing Graphene of the present invention, wherein, in the solvent of preparation slurry, isopropanol is alternatively with the ratio of water
Isopropanol: water=7:3.Also can be selected for acetone, N-Methyl pyrrolidone, N,N-dimethylformamide solvent as preparation slurry
Solvent.
The device preparing Graphene of the present invention, wherein, the diameter of micro-reaction channel can in the case of less than 1mm basis
The size of material is replaced, such as 0.8mm, 0.5mm etc..
The device preparing Graphene of the present invention, wherein, micro-reaction channel material preferentially selects corrosion resistant rustless steel steel, gold
Belong to material and can ensure the timely transmission of reaction temperature；Micro-reaction channel length can according to the volume of slurry, micro-reaction channel straight
Footpath increases and decreases.
The device preparing Graphene of the present invention, wherein, water bath containers 5 internal temperature can be according to reality in the range of 5-90 DEG C
Testing requirement regulation, ultrasonic power can need regulation according to material between 0-1200W.
The device preparing Graphene of the present invention can also be used for the stripping of other two-dimensional slice materials, such as molybdenum bisuphide, nitrogen
Change boron etc., solvent classification can be changed according to the different of solid material.
Technical scheme provide a kind of method that in micro-reaction channel, Graphene is carried out ultrasonic stripping and
Device.Hydrodynamic shear when technical scheme flows in micro-reaction channel by graphite microparticles suspension and micro-instead
Answer the gathering to ultrasonic energy in passage, it is achieved the preparation of small flake diameter Graphene.
Used by technical scheme, micro-reaction channel is as the microreactor in graphite powder stripping process, prepared
Graphene quality is high, is greatly improved almost without oxy radical, charge stripping efficiency and productivity.
Micro-reaction channel has great specific surface area, fabulous heat transfer and mass transfer ability due to its micro structure, can realize
The uniform high-efficiency mixing of material, therefore many reactions that cannot realize in conventional reactor all can at micro-reaction channel (micro-instead
Answer device) middle realization.The most micro-reaction channel has high safety, can avoid the generation of experiment accident, and amplify in industry
During without enlarge-effect.
Below it is only the preferred embodiment of the present invention, it is noted that those skilled in the art are come
Saying, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (7)
1. the device preparing Graphene, it is characterised in that including:
For containing the first container and the second container of graphite slurry；
The micro-reaction channel being arranged between the first container, second container；
Be arranged between the first container, second container for controlling micro-reaction channel internal temperature and for sending ultrasound wave
Make the temperature controlled ultrasonic equipment that the graphite slurry in micro-reaction channel is peeled off；
Being provided with the first peristaltic pump between first container and micro-reaction channel, the first peristaltic pump is for by the graphite in the first container
Slurry through micro-reaction channel pump to second container；
Being provided with the second peristaltic pump between second container and micro-reaction channel, the second peristaltic pump is for by the graphite in second container
Slurry through micro-reaction channel pump to the first container.
Prepare the device of Graphene the most as claimed in claim 1, it is characterised in that temperature controlled ultrasonic equipment includes:
For containing water and the water bath containers of micro-reaction channel；
For the heater heated for the water in water bath containers, it is arranged at the outside of water bath containers；
For controlling the temperature controller of the temperature of the water within water bath containers, it is connected with heater；
For sending the excusing from death wave producer that the graphite slurry in ultrasound wave makes micro-reaction channel is peeled off, it is arranged at water bath containers
Internal.
Prepare the device of Graphene the most as claimed in claim 2, it is characterised in that one end of described micro-reaction channel is by pipe
Road is connected with the first peristaltic pump, and the other end of described micro-reaction channel is connected by pipeline and the second peristaltic pump, described micro-reaction
Passage includes multiple vertical sections vertically extended and multiple bending segment, and each described bending segment connects adjacent vertical
Section, so that described micro-reaction channel is at the inside bending extension of described water bath containers.
4. the method preparing Graphene, it is characterised in that including:
Step one, preparation graphite slurry；
Step 2, make graphite slurry under the conveying of the first peristaltic pump, from first container enter micro-reaction channel, be incubated and pass through
After ultrasonic release effect, entering second container, keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic equipment sends ultrasonic
Ripple makes the graphite slurry in micro-reaction channel peel off, ultrasonic power 360W.
The method preparing Graphene the most as claimed in claim 4, it is characterised in that also include: step 3, treat in the first container
Graphite slurry input is complete, and no longer has liquid to enter in second container, closes the first peristaltic pump, opens the second peristaltic pump, make
Graphite slurry passes through the second peristaltic pump reaction channel in a subtle way, and keeping the temperature in micro-reaction channel is 10 DEG C, and temperature controlled ultrasonic sets
Preparation goes out the graphite slurry stripping in ultrasound wave makes micro-reaction channel, ultrasonic power 360W, makes graphite slurry at the second peristaltic pump
Conveying under, from second container enter micro-reaction channel, insulation and after ultrasonic release effect, enter the first container.
The method preparing Graphene the most as claimed in claim 5, it is characterised in that also include: repeating said steps two, step
Three.
The method preparing Graphene the most as claimed in claim 6, it is characterised in that described step one prepares graphite slurry bag
Including: isopropanol mixes with water makees solvent, isopropanol is 3:7 with the volume ratio of water, adds the solvent volume benzene than 10% and pricks bromine
Ammonium salt solution makees dispersant, and described solvent and dispersant are added 15000 mesh Graphene powder, and making graphite solid weight content is 5%,
Magnetic agitation makes graphite slurry be uniformly dispersed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610614095.5A CN106185910A (en) | 2016-07-28 | 2016-07-28 | Prepare the device and method of Graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610614095.5A CN106185910A (en) | 2016-07-28 | 2016-07-28 | Prepare the device and method of Graphene |
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| Publication Number | Publication Date |
|---|---|
| CN106185910A true CN106185910A (en) | 2016-12-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610614095.5A Pending CN106185910A (en) | 2016-07-28 | 2016-07-28 | Prepare the device and method of Graphene |
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| CN (1) | CN106185910A (en) |
Cited By (3)
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| CN107879337A (en) * | 2017-11-14 | 2018-04-06 | 常州第六元素材料科技股份有限公司 | Prepare the method and its equipment of graphene oxide |
| CN111377437A (en) * | 2018-12-31 | 2020-07-07 | 浙江工业大学 | A kind of peeling device and peeling method of layered material |
| CN112592369A (en) * | 2020-12-25 | 2021-04-02 | 安道麦安邦(江苏)有限公司 | Method and device for ultrasonically strengthening ethephon through micro-channel reactor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879337A (en) * | 2017-11-14 | 2018-04-06 | 常州第六元素材料科技股份有限公司 | Prepare the method and its equipment of graphene oxide |
| CN107879337B (en) * | 2017-11-14 | 2023-12-26 | 常州第六元素材料科技股份有限公司 | Method and equipment for preparing graphene oxide |
| CN111377437A (en) * | 2018-12-31 | 2020-07-07 | 浙江工业大学 | A kind of peeling device and peeling method of layered material |
| CN111377437B (en) * | 2018-12-31 | 2024-01-16 | 浙江工业大学 | Stripping device and stripping method for layered material |
| CN112592369A (en) * | 2020-12-25 | 2021-04-02 | 安道麦安邦(江苏)有限公司 | Method and device for ultrasonically strengthening ethephon through micro-channel reactor |
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Application publication date: 20161207 |