CN110203914A - It is a kind of to prepare few layer of graphene composite material device and method - Google Patents
It is a kind of to prepare few layer of graphene composite material device and method Download PDFInfo
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- CN110203914A CN110203914A CN201910632601.7A CN201910632601A CN110203914A CN 110203914 A CN110203914 A CN 110203914A CN 201910632601 A CN201910632601 A CN 201910632601A CN 110203914 A CN110203914 A CN 110203914A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C01B32/19—Preparation by exfoliation
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Abstract
The present invention relates to a kind of few layer graphene composite material preparation facilities and methods.The present invention designs mill with unique double lift-off structures, when graphite slurry enters electrochemistry groove, salt-DMF ligand enters graphite layers under electric field driven and realizes that intercalation is tentatively removed, mill share zone is rotated into mill after graphite expansion further to remove under mill shearing force into graphene composite material, since the intercalation of graphite makes it easier to be removed by mill shearing force, and pressurizing device can increase mill shearing force, can further effectively improve few layer of graphene composite material yield.At the same time, this method is versatile, and preparation process is controllable, industrial application value with higher.
Description
Technical field
The present invention relates to grapheme material preparation field, in particular to a kind of few layer graphene composite material preparation facilities and
Method.
Background technique
Graphene has excellent photoelectricity, mechanics, thermal property, has been studied extensively since 2004 are found by people,
Materialogy, micro-nano technology, the energy, biomedicine and in terms of it is with important application prospects.Stone is prepared at present
The method of black alkene mainly has mechanical stripping method, oxidation-reduction method, epitaxy method, CVD vapour deposition process, epitaxial growth method, electricity
Chemical stripping method etc., but there are still mechanical stripping method low yield, oxidation-reduction method quality is low, environmental pollution, epitaxy method,
CVD vapour deposition process, epitaxial growth method are at high cost, and electrochemical stripping method raw material require the disadvantages of high.Therefore develop a kind of low
Cost, high yield graphene production equipment and method are of great significance.Chinese patent CN107188162A by plasma and
Ball milling, which combines, prepares graphene, but this method can not continuous production and equipment design complexity；Chinese patent CN106542523A
Graphene composite material is prepared for by the way of screw rod extrusion, this method equally exists the disadvantages of equipment design is complicated；In
State patent CN106044761A designs mill using abrasive rubber, prepares graphene by mill shearing force, but there are still mills
The defects of aging, micelle impurity generates；Chinese patent CN108620175A, by designing the device for combining ball milling and mill to shear
It is prepared for graphene, but the collision between ball is easy to generate large effect to graphene lattice.
Summary of the invention
The technical problem to be solved by the present invention is to develop a kind of layer graphene composite material preparation facilities and method less.Tool
For body, the present invention relates to a kind of few layer graphene composite material preparation facilities and methods.
To achieve the above object, the invention provides the following technical scheme:
A kind of device preparing few layer of graphene composite material, including disc-grinding mechanism, the disc-grinding mechanism is by price fixing, opposite
In the Moving plate of price fixing axis rotation, transmission device, pressurizing device and control device composition, the price fixing includes outer ring groove knot
Structure, centre circle electrochemistry groove structure and inner ring feeding inlet；The outer ring groove structure is fan-shaped skewed slot, and the electrochemistry groove is
Embedded bipolar electrode groove；The Moving plate also has the outer ring of fan-shaped skewed slot, corresponding with price fixing skewed slot direction, and centre circle is three lists
Groove；The control device is that transmission device starts, electrochemistry groove voltage controls, the integrated system of pressurizing device controller,
Transmission device revolving speed can be respectively set, electrochemistry groove applies voltage, and pressurizing device applies pressure and operation hours；
Wherein, the slurry that graphite raw material and other inorganic salts, organic solvent mix enters device by feed inlet, recessed by electrochemistry
Slot is tentatively removed, and rotates further removing followed by mill.
The transmission device is rotary electric machine.
The pressurizing device is hydraulic device.
The present invention also provides the method that any of the above-described kind of device prepares graphene composite material, specific steps include:
(1) natural flake graphite or graphite powder and inorganic salts, organic solvent are mixed and made into slurry；
(2) then by above-mentioned slurry gatherer feed inlet；
(3) pressurizing device is set, electrochemistry groove applies voltage, speed of grinding plate and preparation time；
(4) collecting discharging standing and taking upper layer of material is less that stripping can be repeated in layer graphene composite material, primer
From solvent is recyclable further to be utilized.
The inorganic salts are one or more of salt such as lithium chloride, sodium chloride, potassium chloride, magnesium chloride, calcium chloride.
The organic solvent is DMF.
The feed inlet persistently adds DMF in equipment running process.
It is 10~30V that the electrochemistry groove, which applies voltage,.
The speed of grinding plate is 10~50rpm.
The preparation time is 5~20min, and the time of repose is 1h.
The present invention designs mill with unique double lift-off structures, and salt ion and DMF molecular complexes, work as graphite when configuring slurry
When slurry enters electrochemistry groove, salt-DMF ligand enters graphite layers realization intercalation and tentatively removes under electric field driven, stone
Mill share zone is rotated into mill after ink expansion further to remove under mill shearing force into graphene composite wood
Material, since the intercalation of graphite makes it easier to be removed by mill shearing force, and pressurizing device can increase mill shearing force, can be with
Further effectively improve few layer of graphene composite material yield.
The utility model has the advantages that
Compared with prior art, the device of the invention, technical method novel and unique, be simple and efficient, using inorganic salts as
Electrochemical intercalation agent realizes that graphite tentatively expands, and recycles pressurizing device to improve mill shearing force and further removes, few layer graphite
Alkene composite material high production efficiency, and the recyclable recycling of organic solvent, few layer graphene composite material can after acid cleaning
Pure grapheme material is obtained, this layer graphene composite material few for production of the technical program and few layer graphene have important meaning
Justice.
Graphene composite material according to the present invention, be applied to there is no limit, can be applied to be currently known all
Such as derived energy chemical, thermally conductive, electric field.And it is also easy to think according to its physics and chemical property those skilled in the art
To being applied to other possible fields.
Detailed description of the invention
Fig. 1 is few layer graphene composite material preparation facilities structural schematic diagram；
Wherein: 1, price fixing, 2, Moving plate, 3, inner ring feeding inlet, 4, pressurizing device, 5, outer ring groove, 6, electrochemistry groove, 7,
Transmission device, 8, bracket, 9, control device.
Fig. 2 is few layer graphene composite material preparation facilities mill structural schematic diagram, and Fig. 2A is price fixing top view, and Fig. 2 B is
Moving plate top view；
Fig. 3 is that embodiment 1 produces graphene composite material microscope figure；
Fig. 4 is that embodiment 2 produces graphene transmission electron microscope picture.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
This programme design is as follows, mainly comprising following functional module, as shown in Figure 1,1, price fixing, and 2, Moving plate, 3, interior ensphere
Material mouth, 4, pressurizing device, 5, outer ring groove, 6, electrochemistry groove, 7, transmission device, 8, bracket, 9, control device.The mill
Disk is millstone plate or ceramic millstone, is insulating materials；As shown in Fig. 2, the price fixing includes outer ring groove, centre circle electrochemistry
Groove, inner ring feeding inlet, inner ring are additionally provided with a through-hole, are motor rotation axis through-hole；The outer ring groove structure is sector
Oblique groove；The electrochemistry groove is embedded bipolar electrode groove, and electrode material is the metals such as copper, iron, titanium, and electrode is by burying
Line powers on, and the electrochemistry groove uses DC driven, and 0~30V of voltage is adjustable；The Moving plate outer ring is equally fan
Shape skewed slot, corresponding with price fixing skewed slot direction, centre circle is three single grooves, rotates and is driven after electrochemical expansion convenient for mill
Graphite, inner ring have that center is semi-transparent, use for fixed motor rotation axis, and side through-hole is feeding inlet；The transmission device is
Rotary electric machine, 0~50rpm of speed of grinding plate is adjustable；Pressurizing device is clump weight or hydraulic device, is set as Moving plate center of circle position
It sets；The control device is located on the outside of disc-grinding mechanism, is transmission device starting, the control of electrochemistry groove voltage, pressurized control
Integrated system.The bracket is located at below entire disc-grinding mechanism, plays a supporting role, caused by preventing because of shakiness when device works
It is bad to prepare effect.
In use, slurry is first configured, salt ion and DMF molecular complexes when configuring slurry, when graphite slurry enters electrochemistry
When groove, salt-DMF ligand enters graphite layers realization intercalation and tentatively removes under electric field driven, with mill after graphite expansion
Being rotated into mill share zone, further removing is at graphene composite material under mill shearing force, due to inserting for graphite
Layer makes it easier to be removed by mill shearing force, and pressurizing device can increase mill shearing force, can further effectively improve
Few layer graphene composite material yield.
Embodiment 1
50g natural flake graphite is taken, the DMF solution 100mL being added dissolved with 1g lithium chloride imports feed inlet after mixing,
Setting velocity of rotation is 10rpm, and it is 10V that electrochemistry groove, which applies voltage, and setting preparation time is 15min, takes 200mLDMF molten
Liquid during the preparation process in be slowly added to.It is less layer graphene-lithium chloride composite material that collection material, which stands 1h and takes upper layer,
90% the above are few layers.As shown in figure 3, graphene composite material is well dispersed, lamella size is 1~2 micron.
Embodiment 2
100g graphite powder is taken, the DMF solution 100mL being added dissolved with 1g calcium chloride imports feed inlet after mixing, is arranged
Velocity of rotation is 50rpm, and pressurizing device uses hydraulic device, is pressurised into 0.5 times of Moving plate weight, and electrochemistry groove applies voltage
For 30V, setting preparation time is 30min, take 300mLDMF solution during the preparation process in be slowly added to.Collection material is stood
It is less layer graphene-calcium chloride composite material that 1h, which takes upper layer, and 93% the above are few layers.As shown in figure 4, graphene composite material
Surface is with the presence of calcium salt.
Embodiment 3
100g graphite powder is taken, the DMF solution 100mL being added dissolved with 1g calcium chloride imports feed inlet after mixing, is arranged
Velocity of rotation is 50rpm, and pressurizing device uses hydraulic device, is pressurised into 1 times of Moving plate weight, and electrochemistry groove applies voltage and is
30V, setting preparation time be 30min, take 300mLDMF solution during the preparation process in be slowly added to.Collection material stands 1h
Taking upper layer is less layer graphene-calcium chloride composite material, and 93.5% the above are few layers.
Comparative example 1
50g natural flake graphite is taken, the DMF solution 100mL being added dissolved with 1g lithium chloride imports feed inlet after mixing,
Setting velocity of rotation be 10rpm, setting preparation time be 15min, take 200mLDMF solution during the preparation process in it is interior slowly add
Enter.Collection material stands 1h and upper layer is taken to test, and composite material 20% is few layer.
Claims (10)
1. a kind of device for preparing few layer of graphene composite material, which is characterized in that including disc-grinding mechanism, the disc-grinding mechanism by
Price fixing, the Moving plate relative to the rotation of price fixing axis, transmission device, pressurizing device and control device composition, the price fixing include outer
Enclose groove structure, centre circle electrochemistry groove structure and inner ring feeding inlet；The outer ring groove structure is fan-shaped skewed slot, the electrification
Groove is embedded bipolar electrode groove；The Moving plate also has the outer ring of fan-shaped skewed slot, corresponding with price fixing skewed slot direction, centre circle
For three single grooves；The control device is that transmission device starts, electrochemistry groove voltage controls, the collection of pressurizing device controller
At system, transmission device revolving speed can be respectively set, electrochemistry groove applies voltage, and pressurizing device applies pressure and equipment fortune
The row time；Wherein, the slurry that graphite raw material and other inorganic salts, organic solvent mix enters device by feed inlet, is passing through
Electrochemistry groove is tentatively removed, and rotates further removing followed by mill.
2. a kind of device for preparing few layer of graphene composite material according to claim 1, it is characterised in that: the biography
Dynamic device is rotary electric machine.
3. a kind of device for preparing few layer of graphene composite material according to claim 1, it is characterised in that: the pressurization
Device is hydraulic device.
4. a kind of method for preparing graphene composite material using device any described in claims 1 to 33, feature exist
In:
(1) natural flake graphite or graphite powder and inorganic salts, organic solvent are mixed and made into slurry；
(2) then by above-mentioned slurry gatherer feed inlet；
(3) pressurizing device is set, electrochemistry groove applies voltage, speed of grinding plate and preparation time；
(4) collecting discharging standing and taking upper layer of material is less layer graphene composite material, and removing can be repeated in primer, molten
Agent is recyclable further to be utilized.
5. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: the inorganic salts
For one or more of salt such as lithium chloride, sodium chloride, potassium chloride, magnesium chloride, calcium chloride.
6. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: described is organic molten
Agent is DMF.
7. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: the feed inlet
DMF is persistently added in equipment running process.
8. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: the electrochemistry
It is 10~30V that groove, which applies voltage,.
9. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: the mill turns
Speed is 10~50rpm.
10. a kind of method for preparing graphene composite material according to claim 4, it is characterised in that: the preparation
Time is 5~20min, and the time of repose is 1h.
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| CN201910632601.7A CN110203914B (en) | 2019-07-13 | 2019-07-13 | Device and method for preparing few-layer graphene composite material |
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| CN201910632601.7A CN110203914B (en) | 2019-07-13 | 2019-07-13 | Device and method for preparing few-layer graphene composite material |
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