CN106115677B - A kind of device and method of volume production graphene - Google Patents
A kind of device and method of volume production graphene Download PDFInfo
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- CN106115677B CN106115677B CN201610490646.1A CN201610490646A CN106115677B CN 106115677 B CN106115677 B CN 106115677B CN 201610490646 A CN201610490646 A CN 201610490646A CN 106115677 B CN106115677 B CN 106115677B
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Abstract
The present invention provides a kind of equipment of volume production graphene, first electrode, second electrode, power supply unit including electrolytic cell, comprising graphite starting material and it is separated by filtration module, it further include fluid infusion pond, the outlet of fluid infusion pond is connected through liquid supplementation channel with fluid infusion column, fluid infusion column is equipped with nozzle group, and bottom of electrolytic tank is provided with stirring rod;The first filter screen is equipped in electrolytic cell;It is separated by filtration module by outlet pipe to be connected with the fluid infusion pond, the first noncorrosive pump, the second noncorrosive pump and third noncorrosive pump is respectively equipped in outlet pipe, liquid supplementation channel and input duct;Magnetic field generation device is equipped on the outside of the electrolytic cell.The present invention also provides a kind of methods of volume production graphene.The present invention really completes the continuous production of graphene, and the present invention is based on the modes of electrochemical stripping can largely be made the few high-graphitized graphene of the number of plies in a short time in conjunction with externally-applied magnetic field, is conducive to industrial mass produce and applied in each field.
Description
Technical field
The invention belongs to the preparing technical field of graphene, especially a kind of device and method of volume production graphene.
Background technology
Graphene is a kind of graphite of monoatomic layer, be one kind by sp2The hexagonal cell shape of hydbridized carbon atoms composition
Two-dimensional material.Graphene has very high specific surface area, electron mobility, Young's modulus and thermal conductance, causes people's
Great interest.Its excellent properties in terms of electricity makes it in conductive nano composites, nano electron device, field effect transistor
Pipe, ultracapacitor and battery etc. are with a wide range of applications.Therefore, the scale of high quality high conduction performance graphene
It is one of graphene practical application critical issue to be solved to change preparation.
The method to manufacture graphene includes mechanical stripping method, chemical vapour deposition technique and chemical stripping in the prior art
Method etc..Wherein, although mechanical stripping method can generate superior in quality graphene, this method can not large area scale chemical combination
At graphene.In the preparation process of chemical vapour deposition technique, it is necessary to using nearly thousand degree of high temperature and the metal substrate of costliness, and need
Expending a few hours could complete.Chemical stripping method is mainly finally to make stone using the step of high temperature reduction first by graphite oxidation
The lattice shape that black alkene restores its script makes it have electric conductivity, however, the process of oxidation can cause the lattice of graphene by
Destroy, and and not all graphene oxide can effectively be reduced.The shortcoming of these above-mentioned methods, all limits stone
The production of black alkene and subsequent application.
How providing a kind of method can produce under room temperature, have both low cost, simple flow and quick production high quality
Graphene is that this field scientific research personnel endeavours the important topic of research all the time, and answers semiconductor, touch panel and the sun
The vast demand of the field technologies development such as energy battery, design prepared by a large amount of, continuous Large-scale graphene are increasingly important.It is existing
In technology, there is a kind of device of scale volume production high-quality graphene, it includes the electrode tip holder of graphite starting material, electrolysis
The module of slot, power supply unit and filtering and separation product, this device can be made quickly and largely based on electrochemical stripping method
Standby graphene, still, disclosed apparatus structure is too simple, and key issues of how being supplemented for electrolyte solution does not relate to
And and its only simply used a rotor to realize the stirring to electrolyte, glass graphite alkene can only be played very limited
Booster action, on the basis of this prior art, exploitation it is a kind of more rapidly it is efficient production high-quality graphene method pole
For it is necessary to.
Invention content
For overcome the deficiencies in the prior art, it the present invention provides a kind of device and method of volume production graphene, solves
Technical problems, the present invention such as the supplement of electrolyte present in the technology of existing electrochemical stripping production graphene and stirring can
Volume production more quickly is carried out to graphene, and proposes a kind of novel auxiliary electrolysis stripping structure, with electric field and magnetic field
In conjunction with achieving the effect that more efficient electrochemical stripping graphene.
The technical solution adopted by the present invention to solve the technical problems is:
Present invention firstly provides a kind of equipment of volume production graphene, including electrolytic cell, first comprising graphite starting material
Electrode, second electrode, power supply unit and it is separated by filtration module, filling electrolyte in electrolytic cell further includes fluid infusion pond, fluid infusion pond
Outlet is connected through liquid supplementation channel with the fluid infusion column for being vertically set on electrolytic cell centre position, and fluid infusion column one end is in bottom of electrolytic tank
Outside, the other end extend to electrolyte bath, and fluid infusion column can rotate under external motor drive around its own axis, the fluid infusion
Column is segmented from bottom to top is equipped with nozzle group, and the bottom of electrolytic cell is provided with lateral stirring rod on fluid infusion column, wrong in stirring rod
It falls and is equipped with upper tooth and lower tooth;The import for being separated by filtration module is connected by input duct with electrolyte bath, input duct
Nozzle be under liquid level of electrolyte, be provided with the first filter screen below the input duct in electrolytic cell;It is separated by filtration mould
The electrolyte outlet of block is connected by outlet pipe with the fluid infusion pond, in the outlet pipe, liquid supplementation channel and input duct
It is respectively equipped with the first noncorrosive pump, the second noncorrosive pump and third noncorrosive pump.
As a kind of optimal technical scheme, first noncorrosive pump, the second noncorrosive pump and third noncorrosive pump and outer
Portion's motor is connected by solenoid valve with controller respectively.
As a kind of optimal technical scheme, the nozzle group is provided with three sections, and every section of nozzle group is by two parallel circle nozzles
Composition, the circumferencial direction for often enclosing nozzle along fluid infusion column are arranged, and the quantity for often enclosing nozzle is 3~6.
As a kind of optimal technical scheme, first filter screen is 500~800 mesh stainless steel filter screens.
As a kind of optimal technical scheme, the module that is separated by filtration includes the filter set gradually, graphene collection
Device and electrolysis collection, are provided with Nanofiber filter film in the filter.
As a kind of optimal technical scheme, magnetic field generation device, the NS in generated magnetic field are equipped on the outside of the electrolytic cell
Perpendicular to the electrolytic cell, the magnetic field generation device access is direct current for pole.
As a kind of optimal technical scheme, the magnetic field generation device is made of iron core and coil, the coil and iron core
It is looped around the electrolysis bath circumference successively from the inside to the outside.
As a kind of optimal technical scheme, thermocouple, the thermocouple and the controller are provided in the electrolytic cell
It is connected, the entrance of the electrolysis collection is equipped with the first electromagnetic switch valve, is equipped at left and right sides of the graphene collector
The flushing pipe of flushing pipe, side is connected with dispersion flow container, and the flushing pipe of the other side is connected with dispersion liquid collecting tank.
The present invention also provides a kind of methods of volume production graphene, include the following steps:
Bu Zhou [1]It is full of electrolyte into electrolytic cell, under the first bias, the embedding of graphite starting material is carried out under stationary state
Enter step;
Bu Zhou [2]To graphite starting material alternately strip operation under the second bias and third bias, open simultaneously
External motor drives agitating device to be stirred clockwise under certain rotating speed;
Bu Zhou [3]Stop stirring, restore the first bias, stands and open first and third noncorrosive pump after a certain period of time, it is right
Graphene is filtered lock out operation, and collects the graphene separated;
Bu Zhou [4]First and third noncorrosive pump are closed, the second noncorrosive pump is opened, while opening external motor, is stirring
Mix and fluid infusion column rotation status under to electrolytic cell carry out fluid infusion;
Bu Zhou [6]After the completion of fluid infusion, Bu Zhou [ is repeated;2]Bu Zhou [4].
As a kind of optimal technical scheme, the Bu Zhou [1]While progress, it is applied with perpendicular to electrolysis on the outside of electrolytic cell
The magnetic field of slot.
The positive effect of the present invention:The present invention really completes the continuous production of graphene, the setting of the first filter screen
The graphene of output can directly be filtered for the first time in the electrolytic solution, which greatly enhances the filterings of follow-up graphene point
From, while but also bulk graphene remains in electrolyte, in certain electric field ring that even electric field magnetic field is combined
Further embedded and stripping is continued to complete under border;Unique fluid infusion and agitating device can rapidly complete uniform fluid infusion behaviour
Make, at the same the fluid infusion under rotation status electric field and magnetic field there are in the environment of be more easily accomplished it is thick in electrolyte to staying in
Grain size graphene is embedded in and is removed, and to form the graphene for meeting size, further increases the production effect of graphene
Rate;Crucial, the application in magnetic field has vital meaning for the present invention, is ceaselessly touched between electrolyte solution intermediate ion
Hit carry out molecular thermalmotion, it is believed that, and magnetic field there are in the environment of, in the starting graphite alkene material week as electrode
It encloses, due to the effect of electrode-magnetic field, the density of the ion of starting graphite alkene surrounding materials can be made to be more than the average ion in solution
The ion that density and this magnetic field electrode mutually collide is comparatively more, and there will be the probabilities of bigger to coarse grain diameter graphene
It is embedded in, in addition to this, under conditions of externally-applied magnetic field, magnetohydrodynamics effect caused by Lorentz force significantly affects
Electrochemical process, when ion stream cutting magnetic line in solution, can be acted on by Lorentz force;Lorentz force makes ion make spiral shell
Spin line directed movement, to promote the embedding operation of ion pair graphene.The present invention also achieve the electrolyte to isolating into
Row recycling avoids waste, also simplifies operating process.In short, the present invention is based on the modes of electrochemical stripping, that is,
The step of embedded and stripping graphite material can be completed through the change of voltage at room temperature, can be in short-term in conjunction with externally-applied magnetic field
It is interior that the few high-graphitized graphene of the number of plies largely is made, it is conducive to industrial mass produce and applied in each field.
Description of the drawings
Fig. 1 is the structural schematic diagram of the embodiment of the present invention 1;
Fig. 2 is the structural schematic diagram of the embodiment of the present invention 2;
Fig. 3 is the structural schematic diagram of the embodiment of the present invention 3;
Specific implementation mode
Below in conjunction with the accompanying drawings to a preferred embodiment of the present invention will be described in detail.
Embodiment 1
Referring to Fig.1, the preferred embodiment of the present invention 1 provides a kind of equipment of volume production graphene, including electrolytic cell 1, includes stone
The first electrode 2 of black original material, second electrode 3, power supply unit 4 and it is separated by filtration module, electrolysis is filled in electrolytic cell 1
Liquid, further includes fluid infusion pond 5, and fluid infusion pond 5 is exported through liquid supplementation channel 6 and 8 phase of fluid infusion column for being vertically set on 1 centre position of electrolytic cell
Even, 8 one end of fluid infusion column is in 1 bottom outside of electrolytic cell, and the other end extends to inside electrolytic cell 1, and fluid infusion column 8 can be in external motor
It is rotated around its own axis under 9 drives, the fluid infusion column 8 is segmented from bottom to top is equipped with nozzle group 10, close to electrolysis on fluid infusion column 8
The bottom of slot 1 is provided with lateral stirring rod 11, straggly in stirring rod 11 to be equipped with upper tooth and lower tooth;It is described be separated by filtration module into
Mouth is connected by input duct 12 and 1 inside of electrolytic cell, and the nozzle of input duct 12 is under liquid level of electrolyte, in electrolytic cell 1
It is provided with the first filter screen 13 below input duct;Be separated by filtration the electrolyte outlet of module by outlet pipe 14 with
5 pond of the fluid infusion be connected, be respectively equipped in the outlet pipe 14, liquid supplementation channel 6 and input duct 12 first noncorrosive pump 15,
Second noncorrosive pump 16 and third noncorrosive pump 17.
First noncorrosive pump 15, the second noncorrosive pump 16 and third noncorrosive pump 17 and external motor 9 pass through respectively
Solenoid valve is connected with controller.
The nozzle group is provided with three sections, and every section of nozzle group is made of two parallel circle nozzles, often encloses nozzle along fluid infusion column 8
Circumferencial direction setting, often enclose nozzle quantity be 5.
First filter screen 13 is 500~800 mesh stainless steel filter screens.
The module that is separated by filtration includes the filter 18 set gradually, graphene collector 19 and electrolysis collection
20, Nanofiber filter film is provided in the filter 18.
The method for carrying out volume production to graphene using the equipment of the present embodiment, includes the following steps:
Bu Zhou [1]It is full of electrolyte into electrolytic cell, under the first bias, the embedding of graphite starting material is carried out under stationary state
Enter step;
Bu Zhou [2]To graphite starting material alternately strip operation under the second bias and third bias, open simultaneously
External motor drives agitating device to be stirred clockwise under certain rotating speed;
Bu Zhou [3]Stop stirring, restore the first bias, stands and open first and third noncorrosive pump after a certain period of time, it is right
Graphene is filtered lock out operation, and collects the graphene separated;
Bu Zhou [4]First and third noncorrosive pump are closed, the second noncorrosive pump is opened, while opening external motor, is stirring
Mix and fluid infusion column rotation status under to electrolytic cell carry out fluid infusion;
Bu Zhou [6]After the completion of fluid infusion, Bu Zhou [ is repeated;2]Bu Zhou [4].
Embodiment 2
With reference to Fig. 2, the preferred embodiment of the present invention 2 provides a kind of equipment of volume production graphene, the i.e. equipment described in embodiment 1
On the basis of, it is equipped with magnetic field generation device 21 in 1 outside of the electrolytic cell, the poles NS in generated magnetic field are perpendicular to the electrolysis
Slot 1, what the magnetic field generation device 21 accessed is direct current.
The magnetic field generation device 21 is made of iron core and coil, and the coil and iron core are looped around institute successively from the inside to the outside
State electrolysis bath circumference.
The method that volume production is carried out to graphene using the equipment of the present embodiment, as described in the preparation method in embodiment 1,
Described in Bu Zhou [1]While progress, it is applied with perpendicular to the magnetic field of electrolytic cell on the outside of electrolytic cell.
Embodiment 3
With reference to Fig. 3, the preferred embodiment of the present invention 3 provides a kind of equipment of volume production graphene, the i.e. equipment described in embodiment 2
On the basis of, thermocouple 22 is set also in the electrolytic cell, and the thermocouple 22 is connected with the controller, the electrolyte
The entrance of collector is equipped with the first electromagnetic switch valve 23, and the left and right sides of the graphene collector 19 is equipped with flushing pipe, and one
The flushing pipe of side is connected with dispersion flow container 24, and the flushing pipe of the other side is connected with dispersion liquid collecting tank 25.
In the present invention, bias system is provided with a current supply, can be direct current or exchange electricity suppl.Wherein
First bias system is between+0.5 volt to+10 volts, preferably between+2.5 volts to+5 volts, about 5 to 10 points of action time
Clock.Second bias system is more than the first bias, and between+10 volts to+25 volts, third bias system uses the negative of the second bias
Value, operating time and respectively 2 seconds and 5 seconds, and alternately continue 5 to 10 minutes.
It is above-described to be merely a preferred embodiment of the present invention, it should be understood that the explanation of above example is only used
In facilitating the understanding of the method and its core concept of the invention, it is not intended to limit the scope of protection of the present invention, it is all the present invention's
Any modification for being made within thought and principle, equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of equipment of volume production graphene, including electrolytic cell, the first electrode comprising graphite starting material, second electrode, electricity
Source power supply unit and it is separated by filtration module, filling electrolyte in electrolytic cell, it is characterised in that:Further include fluid infusion pond, the outlet of fluid infusion pond
It is connected with the fluid infusion column for being vertically set on electrolytic cell centre position through liquid supplementation channel, fluid infusion column one end is in outside bottom of electrolytic tank
Side, the other end extend to electrolyte bath, and fluid infusion column can rotate under external motor drive around its own axis, the fluid infusion column
Segmentation is equipped with nozzle group from bottom to top, and the bottom of electrolytic cell is provided with lateral stirring rod on fluid infusion column, straggly in stirring rod
Equipped with upper tooth and lower tooth;The import for being separated by filtration module is connected by input duct with electrolyte bath, input duct
Nozzle is under liquid level of electrolyte, and the first filter screen is provided with below input duct in electrolytic cell;It is separated by filtration module
Electrolyte outlet be connected with the fluid infusion pond by outlet pipe, in the outlet pipe, liquid supplementation channel and input duct point
It She You not the first noncorrosive pump, the second noncorrosive pump and third noncorrosive pump;
The nozzle group is provided with three sections, and every section of nozzle group is made of two parallel circle nozzles, often encloses circle of the nozzle along fluid infusion column
Circumferential direction is arranged, and the quantity for often enclosing nozzle is 3~6.
2. a kind of equipment of volume production graphene according to claim 1, it is characterised in that:First noncorrosive pump,
Two noncorrosive pumps and third noncorrosive pump and external motor are connected by solenoid valve with controller respectively.
3. a kind of equipment of volume production graphene according to claim 1, it is characterised in that:First filter screen is 500
~800 mesh stainless steel filter screens.
4. a kind of equipment of volume production graphene according to claim 2, it is characterised in that:The module that is separated by filtration includes
The filter that sets gradually, graphene collector and electrolysis collection are provided with Nanofiber filter film in the filter.
5. a kind of equipment of volume production graphene according to claim 1, it is characterised in that:Magnetic is equipped on the outside of the electrolytic cell
Field generation device, perpendicular to the electrolytic cell, the magnetic field generation device access is direct current for the poles NS in generated magnetic field.
6. a kind of equipment of volume production graphene according to claim 5, it is characterised in that:The magnetic field generation device is by iron
Core and coil composition, the coil and iron core are looped around the electrolysis bath circumference successively from the inside to the outside.
7. a kind of equipment of volume production graphene according to claim 4, it is characterised in that:It is provided with heat in the electrolytic cell
Galvanic couple, the thermocouple are connected with the controller, and the entrance of the electrolysis collection is equipped with the first electromagnetic switch valve, institute
It states and is equipped with flushing pipe at left and right sides of graphene collector, the flushing pipe of side is connected with dispersion flow container, the flushing of the other side
Pipeline is connected with dispersion liquid collecting tank.
8. a kind of method of volume production graphene, which is characterized in that utilize the equipment amount of progress of volume production graphene described in claim 1
Production, includes the following steps:
Bu Zhou [1]It is full of electrolyte into electrolytic cell, the embedded step of graphite starting material is carried out under the first bias, under stationary state
Suddenly;
Bu Zhou [2]To graphite starting material alternately strip operation under the second bias and third bias, while opening outside
Motor drives agitating device to be stirred clockwise under certain rotating speed;
Bu Zhou [3]Stop stirring, restore the first bias, stands and open first and third noncorrosive pump after a certain period of time, to graphite
Alkene is filtered lock out operation, and collects the graphene separated;
Bu Zhou [4]Close first and third noncorrosive pump, open the second noncorrosive pump, while opening external motor, in stirring and
Fluid infusion is carried out to electrolytic cell under fluid infusion column rotation status;
Bu Zhou [6]After the completion of fluid infusion, Bu Zhou [ is repeated;2]Bu Zhou [4].
9. a kind of method of volume production graphene according to claim 8, which is characterized in that the Bu Zhou [1]What is carried out is same
When, electrolytic cell outside is applied with perpendicular to the magnetic field of electrolytic cell.
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CN106544690B (en) * | 2017-01-21 | 2018-03-13 | 德阳烯碳科技有限公司 | Prepare the electrolysis reaction device of graphene |
CN109704314A (en) * | 2019-02-28 | 2019-05-03 | 嘉兴学院 | A method of continuously preparing graphene |
CN111304729A (en) * | 2020-03-23 | 2020-06-19 | 江苏中佰纳米新材料科技有限公司 | Magnetoelectric polishing device for flat metal |
CN111924832A (en) * | 2020-09-23 | 2020-11-13 | 广西师范大学 | Device and method for producing graphene by electrochemically stripping graphite from electrode array |
CN114772581A (en) * | 2022-05-11 | 2022-07-22 | 广州大学 | Device for preparing carbon quantum dots by semi-automatic electrochemical stripping method |
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CN1042590C (en) * | 1995-10-26 | 1999-03-24 | 河南万众健康产业有限公司 | Health-care cigarette without nicotine |
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CN201981363U (en) * | 2010-12-01 | 2011-09-21 | 天津赛象科技股份有限公司 | Automatic sewing device for steel wire carcass cord fabric |
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Effective date of registration: 20181229 Address after: 301707 Block 103-10 (Centralized Office District), East Side Development Center, Zhongji Road, Douzhangzhuang Township, Wuqing District, Tianjin Patentee after: Anglo nanoscale Polytron Technologies Inc Address before: 300381 Lida Apartment, Weijin South Road, Nankai District, Tianjin Patentee before: Cui Jianzhong |