CN105523550A - Method for preparing graphene nanoplatelets with disk type jet mill - Google Patents
Method for preparing graphene nanoplatelets with disk type jet mill Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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 invention relates to the field of graphene materials, in particular to a method for preparing graphene nanoplatelets with a disk type jet mill. Graphite powder is subjected to heat treatment firstly, then graphene is pretreated with an intercalation agent, Van der Waals's force between graphite layers is decreased, graphite layers are easier to strip, the graphite powder is added to the disk type jet mill, graphite rubs and collides with one another in jet stream collisions to produce shear force serving as the main force, friction force and impact force, graphite layers are stripped, and the graphene nanoplatelets are obtained. Continuous and mass production of the graphene nanoplatelets with uniform layers is realized, the yield is high, the cost is low, pollution is avoided, the layer thickness meets the use requirement in fields of rubber reinforcement, plastic reinforcement, coating corrosion prevention, lubrication and sewage treatment, and large-scale application of graphene is promoted.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to the preparation method of graphene film, particularly relate to a kind of method utilizing disc type micronizer mill to prepare graphene microchip.
Background technology
Graphene is the another Novel Carbon Nanomaterials be found after carbon nanotube, it is a kind of two-dimentional carbon film only having an atomic thickness, it is uniquely a kind of material by individual layer atomic building that people find so far, hexagonal network is connected into by chemical bond-linking between carbon atom in carbon film, because the chemical bond between carbon atom is made up of sp2 hybridized orbital, therefore Graphene is very indomitable, possess the good characteristic that other novel materials such as bent, electroconductibility is strong, physical strength good, light transmission is good do not possess, these characteristics make the preparation method of Graphene receive much concern all the time.
Chinese invention patent application numbers 201410638933.3 discloses the preparation method of graphene oxide and Graphene, comprise the following steps: the preparation method of graphene oxide: by graphite raw material, solvent and oxygenant mix, be placed in closed reaction vessel, stirring reaction 0.5 ~ 6h at 40 ~ 120 DEG C, decompression, suction filtration, after washing, by overanxious thing vacuum-drying, milled processed, product after drying and grinding is dispersed in deionized water, oxygenant is added under acidic conditions, in 0 ~ 4 DEG C of stirring reaction 1 ~ 4h, be warming up to 20 ~ 40 DEG C of stirring reaction 1 ~ 2h, by reacted suspension liquid separating-purifying, be scattered in spraying dry in deionized water and be graphene oxide.Simple and the easy handling of preparation method's technique of this invention, the selection and comparison of supplementary material is common, but the preparation method of this invention is with high costs, is difficult to suitability for industrialized production.
Chinese invention patent application numbers 201410286173.4 discloses a kind of preparation method of Graphene, and it comprises the following steps: the mode of graphite oxide mechanical shearing or ball milling is broken into small shreds by (1); (2) under hydrogen nitrogen or hydrogen argon atmospher, be 1 ~ 19% by hydrogen volume concentration, the concentration of nitrogen or argon gas is 99 ~ 81%, gas flow rate is 10 ~ 100mL/min, with 5 ~ 35 DEG C/min temperature rise rate, above-mentioned graphite oxide small shreds is warming up to 250 ~ 500 DEG C, soaking time is 5 ~ 120min, and hydrogen nitrogen or hydrogen argon gas stream drop to room temperature or naturally cool to room temperature, obtain Graphene.The preparation method of this invention is simple to operate, and the Graphene reducing degree obtained is higher, but Graphene output prepared by the preparation method of this invention is little.
Chinese invention patent application numbers 201410226056.9 discloses the technique and the device that adopt comminution by gas stream stripping means to prepare Graphene presoma two-dimensional nano Graphite Powder 99, and this contrive equipment comprises air supply system, pulverizes the gentle solid separation system of stripping system; In pulverizing stripping system, A return line, B return line and upcast constitute the Matter Transfer loop of comminution by gas stream stripping process; A air entraining pipe, B air entraining pipe and C air entraining pipe constitute the comminution by gas stream passage of comminution by gas stream stripping process.Preparing Graphene presoma two-dimensional nano Graphite Powder 99 adopts three bursts of supersonic jets jointly to carry graphite granule, by collision and the friction of band material jet, realize high-purity pulverizing and the stripping of graphite granule, pulverize stripping continuously by the circulation of graphite granule, obtain two-dimensional nano Graphite Powder 99 thus.This invention utilizes the mutual collision between graphite granule to realize pulverizing and the stripping of Graphite Powder 99 with friction, and obtain highly purified two-dimensional nano Graphite Powder 99, but preparation method's productive rate of this invention is low, quality product is uncontrollable.
Along with the fast development of modern industry, existing graphene preparation method because cost is high, the defect such as complex process, environmental pollution be large, be doomed by market.Therefore, invent a kind of preparation technology simply, production safety environmental protection, production cost is low, and output is high, the graphene preparation method of constant product quality, to the application promoting grapheme material, promotes that the development of Graphene industry is significant.
Summary of the invention
High for current Graphene production cost, complicated process of preparation, the shortcoming that output is little, the present invention proposes a kind of method that low cost prepares graphene microchip.The method utilizes disc type micronizer mill to prepare the graphene microchip that be evenly distributed of the number of plies at 100-300 layer, the graphene microchip of preparation can be applicable in the matrix materials such as rubber, plastics, coating, lubricating oil, sewage disposal, or as preparing the raw material of Graphene further, the preparation cost of current Graphene significantly can be reduced.
For solving the problem, the present invention by the following technical solutions:
A kind of method utilizing disc type micronizer mill to prepare graphene microchip, it is characterized in that: first Graphite Powder 99 is carried out in advance the embrittlement of low pressure intercalation, the shearing force based on shearing force, frictional force and impact force that the air-flow sprayed by disc type micronizer mill eight main jets is again produced peel off graphite, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer, concrete grammar is as follows:
(1) peruscabin of to be the Graphite Powder 99 of 90-100 and weight part by weight part be 0.5-1.5 mixes in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 45-60min of 400-500rpm, obtains mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 2-3:1-1.5:1, then the mixed powder that step (1) obtains is soaked 15h-20h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 50-60KPa, stir with rotating speed 300-500rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, eight main jets are evenly distributed in the side of working cavity, each main jet sprays in working cavity with the pressure of 2.6-4.0MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, powder repeatedly rubs in high velocity air, in the process of collision, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
Described Graphite Powder 99 is any one in crystalline flake graphite, expanded graphite, high orientation graphite, thermo-cracking graphite, and particle diameter is between 100 microns and 400 microns.
Described disc type micronizer mill comprises working medium entrance, liner, working cavity, whirlwind discharge port, residual air relief outlet, opening for feed, main jet, working medium distribution chamber.First Graphite Powder 99 is heat-treated, then intercalator is utilized to carry out pre-treatment to Graphene, reduce Van der Waals force between graphite linings, graphite linings is more easily stripped, Graphite Powder 99 is added in disc type micronizer mill again, in High-speed gas impacting, make phase mutual friction, collision between graphite, produce the shearing force based on shearing force, frictional force and impact force, by graphite delamination, thus obtain graphene microchip.
Described disc type micronizer mill arranges eight main jets, main jet inlet diameter is 6mm-10mm, pressure is produced by the rare gas element of compression, material is made to enter working cavity with high pressure draft, because the main jet arranged exists 35 ° of-50 ° of angles between adjacent two main jets, make Graphite Powder 99 phase mutual friction, collision in working cavity, the shearing force based on shearing force, frictional force and impact force that friction, collision produce, graphite linings is constantly peeled off, obtains the finely dispersed graphene microchip of the number of plies at 100-300 layer.
In order to promote the widespread use of grapheme material, the present invention proposes a kind of method utilizing disc type micronizer mill to prepare graphene microchip, the method can the acquisition number of plies of volume production in the graphene microchip of 100-300 layer, stable production process, and it is pollution-free, be produced into and expect, than in existing graphene preparation method, to only have one of percentage; Not only the number of plies is even for the graphene microchip of preparation, and has excellent physical strength, conduction, heat conductivility concurrently, and good lubrication, high temperature resistant and anticorrosion properties.On the other hand, the thickness of graphene microchip prepared by the present invention is within nanoscale scope, and its radial width is between 5 microns and 50 microns, there is the specific surface area of super large, thus graphene microchip can be applied in rubber, plastics, coating, lubrication wet goods matrix material; Also as the raw material preparing Graphene further, the preparation cost of current Graphene can significantly be reduced.
The graphene microchip that the present invention utilizes disc type micronizer mill to prepare, not only the number of plies is uniformly dispersed, and pollution-free, output is high, cost is low, meet the requirement in fields such as rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage disposals, be conducive to the large-scale application promoting Graphene.Its salient features advantage is as shown in table 1.
Table 1.
A kind of method utilizing disc type micronizer mill to prepare graphene microchip of the present invention, compared with prior art, its outstanding feature and excellent effect are:
1, utilize low pressure intercalation pretreating graphite powder, reduce Van der Waals force between graphite linings, graphite linings is more easily peeled off.
2, the air-flow that the main jet utilizing disc air flow type disintegrating machine eight to there is angle sprays, allows Graphene in working cavity friction, collision, constantly peels off, and obtains the graphene microchip that the number of plies is controlled, be evenly distributed.
3, preparation method of the present invention be easy to control, the closed production of serialization can be realized, drop into little, cost is low, non-environmental-pollution, output are high, has significant market using value.
Accompanying drawing explanation
For further illustrating the method utilizing disc type micronizer mill to prepare graphene microchip, be described by accompanying drawing.
Accompanying drawing 1: be disc type micronizer mill schematic diagram.1-working medium entrance; 2-liner; 3-working cavity; 4-whirlwind discharge port; 5-residual air relief outlet; 6-opening for feed; 7-main jet; 8-working medium distribution chamber.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
embodiment 1
A kind of method utilizing disc type micronizer mill to prepare graphene microchip:
((1) by weight part be 90 high orientation Graphite Powder 99 and weight part be 0.5 peruscabin mix in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 45min of 400rpm, obtain mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 2:1:1, then the mixed powder that step (1) obtains is soaked 15h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 50KPa, stir with rotating speed 300rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 2.6MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
embodiment 2
A kind of method utilizing disc type micronizer mill to prepare graphene microchip:
((1) by weight part be 100 thermo-cracking Graphite Powder 99 and weight part be 1.5 peruscabin mix in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 60min of 500rpm, obtain mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 3:1.5:1, then the mixed powder that step (1) obtains is soaked 20h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 60KPa, stir with rotating speed 500rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 4.0MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
embodiment 3
A kind of method utilizing disc type micronizer mill to prepare graphene microchip:
((1) by weight part be 95 expanded graphite powder and weight part be 0.8 peruscabin mix in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 50min of 450rpm, obtain mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 2.4:1.2:1, then the mixed powder that step (1) obtains is soaked 18h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 55KPa, stir with rotating speed 360rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 3.6MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
embodiment 4
A kind of method utilizing disc type micronizer mill to prepare graphene microchip:
((1) by weight part be 98 crystalline graphite powder and weight part be 1.2 peruscabin mix in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 55min of 480rpm, obtain mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 2.2:1.3:1, then the mixed powder that step (1) obtains is soaked 15h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 56KPa, stir with rotating speed 420rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 2.8MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
embodiment 5
A kind of method utilizing disc type micronizer mill to prepare graphene microchip:
((1) by weight part be 92 crystalline graphite powder and weight part be 0.9 peruscabin mix in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 60min of 500rpm, obtain mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 3:1.4:1, then the mixed powder that step (1) obtains is soaked 18h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 50KPa, stir with rotating speed 320rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 3.4MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
Claims (5)
1. the method utilizing disc type micronizer mill to prepare graphene microchip, it is characterized in that: first Graphite Powder 99 is carried out the embrittlement of low pressure intercalation, the shearing force based on shearing force, frictional force and impact force that the air-flow sprayed by disc type micronizer mill eight main jets is again produced peel off graphite, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer, concrete grammar is as follows:
(1) peruscabin of to be the Graphite Powder 99 of 90-100 and weight part by weight part be 0.5-1.5 mixes in high-speed mixing reaction machine, with the rotating speed dispersed with stirring 45-60min of 400-500rpm, obtains mixed powder;
(2) iron(ic) chloride, diacetyl oxide, acetic acid are mixed with intercalator with mass ratio 2-3:1-1.5:1, then the mixed powder that step (1) obtains is soaked 15h-20h in the airtight high speed agitator that intercalator is housed, invade in bubble process and airtight high speed agitator air pressure is extracted into 50-60KPa, stir with rotating speed 300-500rpm simultaneously; Then be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in disc type micronizer mill, disc type micronizer mill arranges eight main jets, each main jet sprays in working cavity with the pressure of 2.6-4.0MPa, powder in working cavity with the form friction of jet, collision, produce the shearing force based on shearing force of high strength, frictional force and impact force, in the process that powder repeatedly rubs in high velocity air, collide, graphite linings is constantly peeled off, by whirlwind discharge port output, obtain the finely dispersed graphene microchip of the number of plies at 100-300 layer.
2. a kind of method utilizing disc type micronizer mill to prepare graphene microchip according to claim 1, it is characterized in that: Graphite Powder 99 is any one in crystalline flake graphite, expanded graphite, high orientation graphite, thermo-cracking graphite, and particle diameter is between 100 microns and 400 microns.
3. a kind of method utilizing disc type micronizer mill to prepare graphene microchip according to claim 1, is characterized in that: described disc type formula micronizer mill comprises working medium entrance, liner, working cavity, whirlwind discharge port, residual air relief outlet, opening for feed, main jet, working medium distribution chamber.
4. a kind of method utilizing disc type micronizer mill to prepare graphene microchip according to claim 1, it is characterized in that: described disc type micronizer mill arranges eight main jets, eight main jets are evenly distributed in the side of working cavity, main jet inlet diameter is 6mm-10mm, there are 35 ° of-50 ° of angles between two adjacent main jets, make Graphite Powder 99 in the phase mutual friction of flat-disk cavity working spaces, collision, the shearing force based on shearing force, frictional force and impact force that friction, collision produce, make graphite linings constantly peel off.
5. a kind of method utilizing disc type micronizer mill to prepare graphene microchip according to claim 1, is characterized in that: graphene microchip prepared by described method meets the application at rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage treatment area.
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| CN105905888A (en) * | 2016-05-06 | 2016-08-31 | 成都新柯力化工科技有限公司 | Graphene composite microchips stripped by using turbine sander and preparation method for graphene composite microchips |
| CN106044758A (en) * | 2016-06-02 | 2016-10-26 | 上海利物盛企业集团有限公司 | Method and device for preparing graphene by adopting disc type airflow grinder |
| CN106185887A (en) * | 2016-07-04 | 2016-12-07 | 成都新柯力化工科技有限公司 | Method and the grapheme material of grapheme material is prepared in a kind of high-velocity fluid stripping |
| CN106564885A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Jet device for continuous preparation of graphene and method thereof |
| CN107055518A (en) * | 2016-12-27 | 2017-08-18 | 成都新柯力化工科技有限公司 | A kind of application for the method and graphene powder that graphene powder is prepared by crushing |
| CN110054179A (en) * | 2019-05-29 | 2019-07-26 | 张新庄 | Ball shaped nano graphene production technology |
| CN110423494A (en) * | 2019-06-22 | 2019-11-08 | 哈尔滨工业大学（威海） | The preparation method of coupling agent gas-phase modification graphite nano plate composite granule |
| CN111422858A (en) * | 2020-04-13 | 2020-07-17 | 鹤岗市振金石墨烯新材料研究院 | Method for efficiently preparing graphene |
| CN113086975A (en) * | 2021-05-06 | 2021-07-09 | 常州富烯科技股份有限公司 | Graphene microsphere and high-thermal-conductivity gasket prepared from same |
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| CN105905888A (en) * | 2016-05-06 | 2016-08-31 | 成都新柯力化工科技有限公司 | Graphene composite microchips stripped by using turbine sander and preparation method for graphene composite microchips |
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| 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 |
| CN107055518A (en) * | 2016-12-27 | 2017-08-18 | 成都新柯力化工科技有限公司 | A kind of application for the method and graphene powder that graphene powder is prepared by crushing |
| CN110054179A (en) * | 2019-05-29 | 2019-07-26 | 张新庄 | Ball shaped nano graphene production technology |
| CN110423494A (en) * | 2019-06-22 | 2019-11-08 | 哈尔滨工业大学（威海） | The preparation method of coupling agent gas-phase modification graphite nano plate composite granule |
| 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 |
| CN111422858A (en) * | 2020-04-13 | 2020-07-17 | 鹤岗市振金石墨烯新材料研究院 | Method for efficiently preparing graphene |
| 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 |
| CN113086975A (en) * | 2021-05-06 | 2021-07-09 | 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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