CN105523550B - A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill - Google Patents
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill Download PDFInfo
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- CN105523550B CN105523550B CN201610057733.8A CN201610057733A CN105523550B CN 105523550 B CN105523550 B CN 105523550B CN 201610057733 A CN201610057733 A CN 201610057733A CN 105523550 B CN105523550 B CN 105523550B
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- C01B2204/00—Structure or properties of graphene
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The present invention relates to grapheme material field, and in particular to a kind of method that graphene microchip is prepared using disc type airslide disintegrating mill.First graphite powder is heat-treated, then graphene is pre-processed using intercalator, Van der Waals force between reduction graphite linings, graphite linings are made to be more easy to be stripped, graphite powder is added in disc type airslide disintegrating mill again, phase mutual friction, collision between graphite are made in High-speed gas impacting, produces shearing force, frictional force and the impact based on shearing force, by graphite delamination, so as to obtain graphene microchip.Realize continuous, the uniform graphene microchip of the large-scale production number of plies; and yield is high, cost is low; pollution-free, thickness meets in rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, the requirement of sewage treatment area, to be advantageous to the large-scale application for promoting graphene.
Description
Technical field
The present invention relates to grapheme material field, and in particular to the preparation method of graphene film, more particularly to a kind of profit
The method that graphene microchip is prepared with disc type airslide disintegrating mill.
Background technology
Graphene is the another Novel Carbon Nanomaterials being found after CNT, is an a kind of only atom thick
The two-dimentional carbon film of degree, is unique a kind of material by individual layer atomic building that people have found so far, in carbon film between carbon atom by
Chemical bond connects into hexagonal network, and because the chemical bond between carbon atom is made up of sp2 hybridized orbits, therefore graphene is very stupid
By force, possesses the good characteristic that other new materials such as bent, electric conductivity is strong, mechanical strength is good, translucency is good do not possess, these are special
Property causes the preparation method of graphene to receive much concern all the time.
Chinese invention patent application number 201410638933.3 discloses the preparation method of graphene oxide and graphene, bag
Include following steps：The preparation method of graphene oxide：Graphite raw material, solvent and oxidant are well mixed, are placed in confined reaction
In container, 0.5~6h of stirring reaction at 40~120 DEG C, decompression, filter, after washing, at the vacuum drying of overanxious thing, grinding
Reason, the product after drying and grinding is dispersed in deionized water, oxidant is added under acid condition, in 0~4 DEG C of stirring
1~4h is reacted, 20~40 DEG C of 1~2h of stirring reaction is warming up to, by reacted suspension separating-purifying, is scattered in deionized water
Middle spray drying is graphene oxide.The preparation method technique of the invention is simple and easily operated, the selection ratio of supplementary material
More typically, but the preparation method of the invention is with high costs, it is difficult to industrialized production.
Chinese invention patent application number 201410286173.4 discloses a kind of preparation method of graphene, and it includes following
Step：（1）Graphite oxide is broken into fractionlet with the mode of mechanical shearing or ball milling；（2）Under hydrogen nitrogen or hydrogen argon atmospher, press
Hydrogen volume concentration is 1~19%, and the concentration of nitrogen or argon gas is 99~81%, and gas flow rate is 10~100mL/min, with 5~
Above-mentioned graphite oxide fractionlet is warming up to 250~500 DEG C by 35 DEG C/min heating rates, and soaking time is 5~120min, hydrogen nitrogen
Or hydrogen argon gas flows down and is down to room temperature or naturally cools to room temperature, obtains graphene.The preparation method of the invention is simple to operate, obtains
Graphene reducing degree it is higher, but the preparation method of the invention prepare graphene yield it is small.
Chinese invention patent application number 201410226056.9 discloses prepares graphene using air-flow crushing stripping means
The technique and device of presoma two-dimensional nano graphite powder, the invention device include air supply system, crush stripping system and gas-solid point
From system；In stripping system is crushed, the material that A return ducts, B return ducts and tedge constitute air-flow crushing stripping process follows
Loop back path；A air entraining pipes, B air entraining pipes and C air entraining pipes constitute the air-flow crushing passage of air-flow crushing stripping process.Prepare graphite
Alkene presoma two-dimensional nano graphite powder carries graphite particle jointly using three bursts of supersonic jets, by the collision of strip jet with
Friction, realize that high-purity crushing of graphite particle with peeling off, continuously crushes stripping by the circulation of graphite particle, is derived from two dimension
Nano graphite powder.The invention realizes the crushing of graphite powder and stripping using the mutual collision between graphite particle with friction, obtains
The two-dimensional nano graphite powder of high-purity is obtained, but the preparation method low yield of the invention, product quality are uncontrollable.
With the fast development of modern industry, existing graphene preparation method is dirty due to cost height, complex process, environment
The defects of big is contaminated, is doomed by market.Therefore, it is simple to invent a kind of preparation technology, production safety environmental protection, production cost
Low, yield is high, the stable graphene preparation method of product quality, the application to promoting grapheme material, promotes graphene industry
Development it is significant.
The content of the invention
It is high for current graphene production cost, the shortcomings that preparation technology is complicated, and yield is small, the present invention propose it is a kind of it is low into
The method of this preparation graphene microchip.This method is equal in the distribution of 100-300 layers using the disc type airslide disintegrating mill preparation number of plies
Even graphene microchip, the graphene microchip of preparation can be applied to the composite woods such as rubber, plastics, coating, lubricating oil, sewage disposal
In material, or as the raw material for further preparing graphene, the preparation cost of current graphene can be greatly reduced.
To solve the above problems, the present invention uses following technical scheme：
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill, it is characterised in that：It is first that graphite powder is pre-
Carry out that low pressure intercalation is brittle, then caused by the air-flow sprayed by eight main jets of disc type airslide disintegrating mill using shearing force as
Main shearing force, frictional force and impact peels off graphite, obtains finely dispersed graphene microchip of the number of plies in 100-300 layers,
Specific method is as follows：
（1）The Ergol for being 0.5-1.5 by graphite powder and parts by weight that parts by weight are 90-100 is anti-in mixed at high speed
Answer in machine and mix, 45-60min is dispersed with stirring with 400-500rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 2-3:1-1.5:1 is configured to intercalator, then by step（1）
Obtained mixed powder soaks 15h-20h in the closed high speed agitator equipped with intercalator, invades closed high speed during steeping
Agitator air pressure is extracted into 50-60KPa, while is stirred with rotating speed 300-500rpm；Then be filtered dry by centrifuge, be dried to obtain it is pre-
Intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Eight main jets are put, eight main jets are evenly distributed in the side of working cavity, and each main jet is with 2.6-
4.0MPa pressure is sprayed into working cavity, powder friction, collision in the form of jet in working cavity, produces high intensity
The shearing force based on shearing force, frictional force and impact, powder rubs repeatedly in high velocity air, collide during,
Graphite linings are constantly peeled off, and by whirlwind discharging opening output, the finely dispersed graphene for obtaining the number of plies in 100-300 layers is micro-
Piece.
The graphite powder is any of crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, and particle diameter is situated between
Between 100 microns and 400 microns.
The disc type airslide disintegrating mill include working medium entrances, liner, working cavity, whirlwind discharging opening, residual air outlet,
Charging aperture, main jet, working medium distributor chamber.First graphite powder is heat-treated, then graphene carried out using intercalator pre-
Processing, reduce Van der Waals force between graphite linings, make graphite linings be more easy to be stripped, then graphite powder is added into disc type airslide disintegrating mill
In, phase mutual friction, collision between graphite are made in High-speed gas impacting, produces shearing force, the frictional force based on shearing force
And impact, by graphite delamination, so as to obtain graphene microchip.
The disc type airslide disintegrating mill sets eight main jets, and main jet inlet diameter is 6mm-10mm, pressure
Produced by the inert gas of compression, material is entered working cavity with high pressure draught, because the main jet of setting is adjacent
Two main jets between 35 ° of -50 ° of angles be present so that graphite powder in working cavity phase mutual friction, collision, rub, touch
Shearing force, frictional force and impact caused by hitting based on shearing force, make graphite linings constantly peel off, obtain the number of plies in 100-
300 layers of finely dispersed graphene microchip.
In order to promote the extensive use of grapheme material, the present invention proposes that one kind prepares stone using disc type airslide disintegrating mill
The method of black alkene microplate, this method are capable of the acquisition number of plies of volume production in the graphene microchip of 100-300 layers, stable production process,
And it is pollution-free, it is produced into and expects than in existing graphene preparation method, only 1 percent；The graphene microchip of preparation is not
Only the number of plies is uniform, and has excellent mechanical strength, conduction, heat conductivility concurrently, and good lubrication, high temperature resistant and anticorrosive
Characteristic.On the other hand, the thickness of graphene microchip prepared by the present invention is within the scope of nanoscale, and its radial width is situated between
Between 5 microns and 50 microns, there is the specific surface area of super large, thus graphene microchip can be applied to rubber, plastics, painting
In the composites such as material, lubricating oil；Current graphene can also can be greatly reduced as the raw material for further preparing graphene
Preparation cost.
The present invention utilizes graphene microchip prepared by disc type airslide disintegrating mill, and not only the number of plies is uniformly dispersed, and without dirt
Dye, yield are high, cost is low, meet the requirement in fields such as rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage disposals,
Be advantageous to promote the large-scale application of graphene.Its main performance advantage is as shown in table 1.
Table 1.
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill of the present invention, compared with prior art, its
The characteristics of prominent and excellent effect are：
1st, using low pressure intercalation pretreating graphite powder, Van der Waals force between graphite linings is reduced so that graphite linings are more easily peelable.
2nd, the air-flow sprayed using eight main jets that angle be present of disc air flow type disintegrating machine, allows graphene in working chamber
Body friction, collision, are constantly peeled off, and obtain the graphene microchip that the number of plies is controllable, is evenly distributed.
3rd, preparation method of the present invention is easily controllable, the closed production of serialization can be achieved, input is small, cost is low, without environment
Pollution, yield are high, have significant market application value.
Brief description of the drawings
To further illustrate the method that graphene microchip is prepared using disc type airslide disintegrating mill, said by accompanying drawing
It is bright.
Accompanying drawing 1：For disc type airslide disintegrating mill schematic diagram.1- working medium entrances；2- liners；3- working cavities；4- whirlwind goes out
Material mouth；5- residual air outlets；6- charging apertures；7- main jets；8- working medium distributor chambers.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill：
（（1）The highly oriented graphite powder that parts by weight are 90 and the Ergol that parts by weight are 0.5 are reacted in mixed at high speed
Mixed in machine, 45min is dispersed with stirring with 400rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 2:1:1 is configured to intercalator, then by step（1）Obtain
Mixed powder soaks 15h in the closed high speed agitator equipped with intercalator, invades closed high speed agitator air pressure during steeping
50KPa is extracted into, while is stirred with rotating speed 300rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Put eight main jets, each main jet is sprayed into working cavity with 2.6MPa pressure, and powder is in working cavity to penetrate
Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed
During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed
The finely dispersed graphene microchip of 100-300 layers.
Embodiment 2
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill：
（（1）The Ergol for being 1.5 by thermal cracking graphite powder and parts by weight that parts by weight are 100 is anti-in mixed at high speed
Answer in machine and mix, 60min is dispersed with stirring with 500rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 3: 1.5:1 is configured to intercalator, then by step（1）Obtain
Mixed powder soak 20h in the closed high speed agitator equipped with intercalator, invade closed high speed agitator gas during bubble
Pressure is extracted into 60KPa, while is stirred with rotating speed 500rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Put eight main jets, each main jet is sprayed into working cavity with 4.0MPa pressure, and powder is in working cavity to penetrate
Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed
During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed
The finely dispersed graphene microchip of 100-300 layers.
Embodiment 3
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill：
（（1）The Ergol that expanded graphite powder and parts by weight that parts by weight are 95 are 0.8 is reacted into machine in mixed at high speed
Middle mixing, 50min is dispersed with stirring with 450rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 2.4:1.2:1 is configured to intercalator, then by step（1）
To mixed powder soak 18h in the closed high speed agitator equipped with intercalator, invade closed high speed agitator during bubble
Air pressure is extracted into 55KPa, while is stirred with rotating speed 360rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Put eight main jets, each main jet is sprayed into working cavity with 3.6MPa pressure, and powder is in working cavity to penetrate
Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed
During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed
The finely dispersed graphene microchip of 100-300 layers.
Embodiment 4
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill：
（（1）The Ergol that crystalline graphite powder and parts by weight that parts by weight are 98 are 1.2 is reacted into machine in mixed at high speed
Middle mixing, 55min is dispersed with stirring with 480rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 2.2:1.3:1 is configured to intercalator, then by step（1）
To mixed powder soak 15h in the closed high speed agitator equipped with intercalator, invade closed high speed agitator during bubble
Air pressure is extracted into 56KPa, while is stirred with rotating speed 420rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Put eight main jets, each main jet is sprayed into working cavity with 2.8MPa pressure, and powder is in working cavity to penetrate
Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed
During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed
The finely dispersed graphene microchip of 100-300 layers.
Embodiment 5
A kind of method that graphene microchip is prepared using disc type airslide disintegrating mill：
（（1）The Ergol that crystalline graphite powder and parts by weight that parts by weight are 92 are 0.9 is reacted into machine in mixed at high speed
Middle mixing, 60min is dispersed with stirring with 500rpm rotating speed, obtains mixed powder；
（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 3:1.4:1 is configured to intercalator, then by step（1）Obtain
Mixed powder soak 18h in the closed high speed agitator equipped with intercalator, invade closed high speed agitator gas during bubble
Pressure is extracted into 50KPa, while is stirred with rotating speed 320rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation powder；
（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill is set
Put eight main jets, each main jet is sprayed into working cavity with 3.4MPa pressure, and powder is in working cavity to penetrate
Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed
During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed
The finely dispersed graphene microchip of 100-300 layers.
Claims (3)
- A kind of 1. method that graphene microchip is prepared using disc type airslide disintegrating mill, it is characterised in that：First graphite powder is carried out Low pressure intercalation is brittle, then caused by the air-flow sprayed by eight main jets of disc type airslide disintegrating mill based on shearing force Shearing force, frictional force and impact peel off graphite, obtain finely dispersed graphene microchip of the number of plies in 100-300 layers, specifically Method is as follows：（1）The Ergol that graphite powder and parts by weight that parts by weight are 90-100 are 0.5-1.5 is reacted into machine in mixed at high speed Middle mixing, 45-60min is dispersed with stirring with 400-500rpm rotating speed, obtains mixed powder；（2）By iron chloride, acetic anhydride, acetic acid with mass ratio 2-3:1-1 .5:1 is configured to intercalator, then by step（1）Obtain Mixed powder soak 15h-20h in the closed high speed agitator equipped with intercalator, invade closed high-speed stirred during bubble Device air pressure is extracted into 50-60KPa, while is stirred with rotating speed 300-500rpm；Then it is filtered dry by centrifuge, is dried to obtain pre- intercalation Powder；（3）By step（2）Obtained pre- intercalation powder is sent into disc type airslide disintegrating mill, and disc type airslide disintegrating mill sets eight Individual main jet, each main jet are sprayed into working cavity with 2.6-4 .0MPa pressure, and powder is in working cavity to penetrate Form friction, the collision of stream, produce the shearing force based on shearing force, frictional force and the impact of high intensity, powder is at a high speed During rubbing, colliding repeatedly in air-flow, graphite linings are constantly peeled off, and by whirlwind discharging opening output, are obtained the number of plies and are existed The finely dispersed graphene microchip of 100-300 layers；Described disc type formula airslide disintegrating mill include working medium entrances, liner, working cavity, whirlwind discharging opening, residual air outlet, Charging aperture, main jet, working medium distributor chamber；Described disc type airslide disintegrating mill sets eight main jets, eight work sprays Mouth is evenly distributed in the side of working cavity, and main jet inlet diameter is 6mm-10mm, adjacent two main jets it Between 35 ° of -50 ° of angles be present so that graphite powder the phase mutual friction of flat-disk cavity operating room, collision, friction, collision produce The shearing force based on shearing force, frictional force and impact, graphite linings is constantly peeled off.
- 2. a kind of method that graphene microchip is prepared using disc type airslide disintegrating mill, its feature are existed according to claim 1 In：Graphite powder is any of crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, and particle diameter is between 100 microns And between 400 microns.
- 3. a kind of method that graphene microchip is prepared using disc type airslide disintegrating mill, its feature are existed according to claim 1 In：Graphene microchip prepared by methods described meets in rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage treatment area Application.
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| CN105905888B (en) * | 2016-05-06 | 2018-01-30 | 成都新柯力化工科技有限公司 | A kind of compound microplate of graphene peeled off using turbine sand mill and preparation method thereof |
| CN106044758B (en) * | 2016-06-02 | 2018-09-25 | 上海利物盛企业集团有限公司 | A kind of method and device preparing graphene using disc type airflow milling |
| CN106185887B (en) * | 2016-07-04 | 2018-03-27 | 成都新柯力化工科技有限公司 | A kind of high-velocity fluid stripping prepares the method and grapheme material of grapheme material |
| CN106564885B (en) * | 2016-10-20 | 2018-07-31 | 成都新柯力化工科技有限公司 | A kind of continuous fluidic device and its method for preparing graphene |
| CN107055518B (en) * | 2016-12-27 | 2019-02-26 | 成都新柯力化工科技有限公司 | A kind of application for the method and graphene powder preparing graphene powder by crushing |
| CN110054179A (en) * | 2019-05-29 | 2019-07-26 | 张新庄 | Ball shaped nano graphene production technology |
| CN110423494B (en) * | 2019-06-22 | 2021-06-22 | 哈尔滨工业大学（威海） | Preparation method of coupling agent gas-phase modified graphite nanosheet composite powder |
| CN111422858B (en) * | 2020-04-13 | 2022-11-08 | 鹤岗市振金石墨烯新材料研究院 | Method for efficiently preparing graphene |
| CN113086975B (en) * | 2021-05-06 | 2022-11-08 | 常州富烯科技股份有限公司 | Graphene microsphere and high-thermal-conductivity gasket prepared from same |
| CN116921033A (en) * | 2023-08-14 | 2023-10-24 | 邹平恒嘉新材料科技有限公司 | Negative-pressure linkage jet milling production process and system for boehmite powder |
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| CN103382026A (en) * | 2012-05-02 | 2013-11-06 | 中国科学院上海硅酸盐研究所 | Low-cost mass preparation method of high-quality graphene |
| CN104030281B (en) * | 2014-06-25 | 2016-04-13 | 南昌大学 | A kind of preparation method of Graphene |
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