CN205953534U - Device of preparation graphite alkene - Google Patents

Device of preparation graphite alkene Download PDF

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Publication number
CN205953534U
CN205953534U CN201620816091.0U CN201620816091U CN205953534U CN 205953534 U CN205953534 U CN 205953534U CN 201620816091 U CN201620816091 U CN 201620816091U CN 205953534 U CN205953534 U CN 205953534U
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container
micro
reaction channel
graphite
peristaltic pump
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CN201620816091.0U
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赵栋
宋彦楠
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Beijing Technology Co Ltd Nai Nai
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Beijing Technology Co Ltd Nai Nai
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Abstract

The utility model discloses a device of preparation graphite alkene includes first container, second container and sets up little reaction channel, the control by temperature change supersound equipment between first container, second container, still includes first peristaltic pump and second peristaltic pump. The technical scheme of the utility model with the help of graphite miropowder suspension to ultrasonic energy's gathering in the hydrodynamic shear of little reaction channel midstream measured time and little reaction channel, realize the preparation of small footpath graphite alkene. The technical scheme of the utility model the graphite alkene high quality of preparing.

Description

Prepare the device of Graphene
Technical field
This utility model is related to the preparation of carbon, more particularly to a kind of device 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 known the thinnest, the most tough and tensile nano material, and its hardness exceedes diamond;Single-layer graphene is almost fully transparent, only 2.3% absorbance;Heat conductivity is up to 5300W/m K, and resistivity only has 10-6 Ω cm, is heat the most excellent and electricity Conductor.Graphene, because of its excellent physicochemical property, has important research and using value in many applications.Graphene exists It is mainly graphene film and two kinds of forms of graphene powder in research and application, wherein more wide with the application of graphene powder 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 Cut the method that stripping is main flow in mechanical stripping method, but both approaches all Shortcomings.Mechanical shearing stripping method low yield, surpasses Sound up-stripping method, due to intergranular a large amount of stackings, is peeled off time-consuming, thus efficiency is relatively low.
Utility model content
The technical problems to be solved in the utility model is the device preparing Graphene providing a kind of efficiency higher.
The device preparing Graphene of the present utility model, including:
For containing the first container and the second container of graphite slurry;
It is arranged at the micro- reaction channel between the first container, second container;
It is arranged at super for controlling micro- reaction channel internal temperature and being used for send between the first container, second container Sound wave makes the temperature controlled ultrasonic equipment that the graphite slurry in micro- reaction channel is peeled off;
It is provided with the first peristaltic pump, the first peristaltic pump is used in the first container between first container and micro- reaction channel Graphite slurry is through micro- reaction channel pump to second container;
It is provided with the second peristaltic pump, the second peristaltic pump is used in second container between second container and micro- reaction channel Graphite slurry is through micro- reaction channel pump to the first container.
The device preparing Graphene of the present utility model, wherein, temperature controlled ultrasonic equipment includes:
For containing the water bath containers of water and micro- reaction channel;
For the heater for the water heating 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 ultrasound wave makes the graphite slurry in micro- reaction channel peel off, it is arranged at water-bath and holds The inside of device.
The device preparing Graphene of the present utility model, wherein, pipeline and first is passed through in one end of described micro- reaction channel Peristaltic pump connects, and the other end of described micro- reaction channel is connected with the second peristaltic pump by pipeline, and described micro- reaction channel includes Multiple vertical sections vertically extending and multiple bending segment, each described bending segment connects adjacent vertical section, so that Described micro- reaction channel is in the inside bending extension of described water bath containers.
The technical solution of the utility model structure is simple, efficiency is higher.The technical solution of the utility model provides one kind In micro- reaction channel, Graphene is carried out with the device of ultrasonic stripping.The technical solution of the utility model can be by graphite microparticles Gathering to ultrasonic energy in the hydrodynamic shear when flowing in micro- reaction channel for the suspension and micro- reaction channel, realizes small pieces The preparation of footpath Graphene.Graphene quality prepared by the technical solution of the utility model is high, almost without oxy radical.
Brief description
Fig. 1 is the structural representation of the device preparing Graphene of the present utility model;
Fig. 2 be the device preparing Graphene of the present utility model working Examples in graphite raw material scanning electron microscopy Mirror photo;
Fig. 3 is the scanning electron of the graphite ene product in the working Examples of the device preparing Graphene of the present utility model Microphotograph;
Fig. 4 is graphite raw material powder body used and stone in the working Examples of the device preparing Graphene of the present utility model Black alkene prepares the Raman collection of illustrative plates of product.
Specific embodiment
As shown in figure 1, the device preparing Graphene of the present utility model, 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 controlling micro- reaction channel 1 internal temperature and being used for Send the temperature controlled ultrasonic equipment 2 that ultrasound wave makes the graphite slurry in micro- reaction channel 1 peel off;
It is provided with the first peristaltic pump 21, the first peristaltic pump 21 is used for the first container between first container and micro- reaction channel Graphite slurry in 11 is through micro- reaction channel 1 pump to second container 12;
It is provided with the second peristaltic pump 22, the second peristaltic pump 22 is used for second container between second container and micro- reaction channel Graphite slurry in 12 is through micro- reaction channel 1 pump to the first container 11.
The device preparing Graphene of the present utility model, 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 for the water heating 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 ultrasound wave makes the graphite slurry in micro- reaction channel 1 peel off, it is arranged at water-bath The inside of container 5.
The device preparing Graphene of the present utility model, wherein, pipeline and the first wriggling are passed through in one end of micro- reaction channel 1 Pump 21 connects.The other end of micro- reaction channel 1 is connected with the second peristaltic pump 22 by pipeline.
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 Connect, one end of the second flexible pipe 32 is vertically stretched in second container 12, 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 sections 101 vertically extending and multiple bending segment 102, each curved Trisection 102 connects adjacent vertical section 101, so that micro- reaction channel 1 is in the inside bending extension of water bath containers 5.
The working Examples of the device preparing Graphene of the present utility model are as follows:
First, prepare graphite slurry:
Isopropanol is mixed with water makees solvent, and isopropanol is 3 with the volume ratio of water:7, add the benzene than 10% for the solvent volume Prick bromine ammonium salt solution and make dispersant, described solvent and dispersant are added 15000 mesh Graphene powders, make the graphite solid weight content be 5%, magnetic agitation makes graphite slurry be uniformly dispersed.
2nd, graphite is peeled off:The graphite slurry of suspended liquid, under the conveying of the first peristaltic pump, enters anti-in a subtle way from the first container Answer passage, be incubated and after ultrasonic release effect, enter second container, keep the temperature in micro- reaction channel to be 10 DEG C, temperature Control ultrasonic device sends ultrasound wave makes the graphite slurry in micro- reaction channel peel off, and ultrasonic power 360W treats stone in the first container Black slurry input finishes, and no longer has liquid to enter in second container, closes the first peristaltic pump, opens the second peristaltic pump, make stone Black slurry passes through the second peristaltic pump reaction channel in a subtle way, keeps the temperature in micro- reaction channel to be 10 DEG C, temperature controlled ultrasonic equipment Sending ultrasound wave makes the graphite slurry in micro- reaction channel peel off, and ultrasonic power 360W makes graphite slurry in the second peristaltic pump Under conveying, enter reaction channel in a subtle way 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 particles pattern is as shown in figure 3, Fig. 2, Fig. 3 are graphite raw material powder body used and Graphene preparation The SEM photograph of product, it can be seen that graphite raw material granule is 3-5 μm of irregular blocky-shaped particle, prepared Graphene The piece number of plies of granule be less than 10 layers, be multi-layer graphene granule and be flake-shaped particles, the thickness of graphene film<10nm, shows The technical solution of the utility model can effectively be peeled off to graphite granule and be prepared graphene powder.
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.Raman in figure D, G and 2D peak are the Characteristic Raman peaks of graphite and grapheme material, and 2D peak is at transverse axis Position be judge prepared by material be whether Graphene important evidence.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 Go out, at 2679cm-1, peak type symmetry is good for the 2D peak-to-peak position of prepared graphite ene product, then can determine that prepared product is stone Black alkene powder body.Knowable to the intensity at D peak, Graphene prepares that product degree of imperfection is low, maintains the degree of crystallinity of pure phase graphite composite powder, institute The quality of the product of preparation is higher.
Graphite raw material can be less than the graphite powder in 15000 mesh piece footpaths, expanded graphite, crystalline flake graphite or graphite oxide.
The ratio preparing isopropanol and water in the solvent of slurry is alternatively isopropanol:Water=7:3.Also can be selected for acetone, N- Methyl pyrrolidone, N,N-dimethylformamide solvent are as the solvent preparing slurry.
The device preparing Graphene of the present utility model, wherein, the diameter of micro- reaction channel can be in the case of less than 1mm Changed according to the size of material, for example 0.8mm, 0.5mm etc..
Micro- reaction channel material preferentially selects corrosion resistant rustless steel steel, and metal material can ensure the timely biography of reaction temperature Pass;Micro- reaction channel length can increase and decrease according to the diameter of the volume of slurry, micro- reaction channel.
The device preparing Graphene of the present utility model, wherein, water bath containers 5 internal temperature can in the range of 5-90 DEG C root Adjust according to requirement of experiment, ultrasonic power can need to adjust according to material between 0-1200W.
The device preparing Graphene of the present utility model can also be used for the stripping of other two-dimensional slice materials, such as curing Molybdenum, boron nitride etc., can change solvent classification according to the different of solid material.
The technical solution of the utility model provides a kind of dress that in micro- reaction channel, Graphene is carried out with ultrasonic stripping Put.Hydrodynamic shear when the technical solution of the utility model can flow in micro- reaction channel by graphite microparticles suspension With the gathering to ultrasonic energy in micro- reaction channel, realize the preparation of small flake diameter Graphene.
Used by the technical solution of the utility model, micro- reaction channel is as the microreactor in graphite powder stripping process, made Standby Graphene quality is high, and almost without oxy radical, charge stripping efficiency and yield greatly improve.
Micro- reaction channel has great specific surface area, fabulous heat transfer and mass transfer ability due to its micro structure, can achieve The uniform high-efficiency mixing of material, the reaction that therefore many cannot be realized in conventional reactor all can be (micro- anti-in micro- reaction channel Answer device) middle realization.Micro- reaction channel has high safety simultaneously, can avoid the generation of experiment accident, and amplifies in industry During no enlarge-effect.
The above is only preferred implementation of the present utility model it is noted that ordinary skill people for the art For member, on the premise of without departing from this utility model principle, some improvements and modifications can also be made, these improvements and modifications Also should be regarded as protection domain of the present utility model.

Claims (3)

1. a kind of device preparing Graphene is it is characterised in that include:
For containing the first container and the second container of graphite slurry;
It is arranged at the micro- reaction channel between the first container, second container;
Be arranged between the first container, second container for controlling micro- reaction channel internal temperature and being used for sending ultrasound wave Make the temperature controlled ultrasonic equipment that the graphite slurry in micro- reaction channel is peeled off;
It is provided with the first peristaltic pump, the first peristaltic pump is used for the graphite in the first container between first container and micro- reaction channel Slurry is through micro- reaction channel pump to second container;
It is provided with the second peristaltic pump, the second peristaltic pump is used for the graphite in second container between second container and micro- reaction channel Slurry is through micro- reaction channel pump to the first container.
2. prepare the device of Graphene as claimed in claim 1 it is characterised in that temperature controlled ultrasonic equipment includes:
For containing the water bath containers of water and micro- reaction channel;
For the heater for the water heating 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 ultrasound wave makes the graphite slurry in micro- reaction channel peel off, it is arranged at water bath containers Internal.
3. prepare the device of Graphene as claimed in claim 2 it is characterised in that pipe is passed through in one end of described micro- reaction channel Road is connected with the first peristaltic pump, and the other end of described micro- reaction channel is connected with the second peristaltic pump by pipeline, described micro- reaction Passage includes multiple vertical sections vertically extending and multiple bending segment, and each described bending segment connects adjacent vertical Section, so that described micro- reaction channel is in the inside bending extension of described water bath containers.
CN201620816091.0U 2016-07-28 2016-07-28 Device of preparation graphite alkene Active CN205953534U (en)

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Publications (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106185910A (en) * 2016-07-28 2016-12-07 北京奈泊科技有限公司 Prepare the device and method of Graphene

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106185910A (en) * 2016-07-28 2016-12-07 北京奈泊科技有限公司 Prepare the device and method of Graphene

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