CN103771401B - A kind of preparation method of few layer graphene and device - Google Patents
A kind of preparation method of few layer graphene and device Download PDFInfo
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- CN103771401B CN103771401B CN201310739904.1A CN201310739904A CN103771401B CN 103771401 B CN103771401 B CN 103771401B CN 201310739904 A CN201310739904 A CN 201310739904A CN 103771401 B CN103771401 B CN 103771401B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a kind of preparation method of few layer graphene.The preparation method of this few layer graphene comprises the following steps: carry out purification process to Graphite Powder 99; Graphite Powder 99 after purifying added in autoclave or disperse to add afterwards in autoclave in a solvent, heating, after reaching preset temp in autoclave, supercutical fluid is pumped in autoclave; After autoclave internal pressure is raised to preset value, stir, graphite is peeled away by the shearing force utilizing swiftly flowing supercutical fluid to produce, reduction of blood pressure in high-speed; Sample in autoclave, obtain described few layer graphene.Present invention also offers a kind of few layer graphene, it is prepared by above-mentioned preparation method.Present invention also offers the device for the production of above-mentioned few layer graphene.Preparation method's environmental protection of few layer graphene provided by the present invention, production cost is low, and reaction time is short, and preparation technology is simple, and the lamella integrity of obtained few layer graphene is good.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene, particularly a kind of preparation method of few layer graphene, belongs to chemical materials preparation field.
Background technology
Since being found from Graphene in 2004, the generally favor of extremely physics and Material Field investigator always.Graphene is a kind of bi-dimensional cellular shape crystalline network carbonaceous material tightly packed by monolayer carbon atom.Although Graphene only has a carbon atomic layer thickness, and is one the thinnest in known materials, very rigid.Graphene is also the material that current known conductive is outstanding.In addition, Graphene also has the performance of many excellences: as higher Young's modulus, thermal conductivity, huge specific surface area etc.Due to the property of Graphene, it is all widely used in electronics, optics, magnetics, biomedicine, sensor, energy storage etc.And how to prepare high quality, research topic that the Graphene of high yield has become this area hot topic.
At present, the method preparing Graphene mainly comprises following several: oxidation reduction process, chemical Vapor deposition process, mechanically peel method, epitaxial growth method, solvent stripping method etc.But aforesaid method all exists familiar lacunas when embody rule, and mostly belong to the preparation method of multi-layer graphene.
As can be seen here, developing a kind of preparation facilities and method of few layer graphene, is one of this area problem demanding prompt solution.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide a kind of preparation method of few layer graphene, the preparation technology of the method is simple, can prepare the Graphene of few layer in a large number, efficiently.
The present invention also aims to provide a kind of few layer graphene and the device for the preparation of above-mentioned few layer graphene.
In order to achieve the above object, the present invention provide firstly a kind of preparation method of few layer graphene, and it comprises the following steps:
Step one: purification process is carried out to Graphite Powder 99;
Step 2: the Graphite Powder 99 after purifying directly added in autoclave or disperse to add afterwards in autoclave in a solvent, heating, after the temperature in autoclave reaches 35-60 DEG C, supercutical fluid is pumped in autoclave;
Step 3: after pumping into supercutical fluid and making autoclave internal pressure be raised to 75atm-300atm, stirs 30min-20h, then by pressure at the preferred 10s of 5s-20s() in reduce to 1atm, concrete step-down mode can conventionally be carried out;
Step 4: sample in autoclave, obtains described few layer graphene.
According to specific embodiment of the invention scheme, preferably, the supercutical fluid adopted is CO
2supercutical fluid.
According to specific embodiment of the invention scheme, preferably, the Graphite Powder 99 adopted comprises crystalline graphite powder and/or expanded graphite powder etc.
According to specific embodiment of the invention scheme, preferably, the solvent adopted comprises sodium lauryl sulphate and/or Sodium dodecylbenzene sulfonate etc.
According to specific embodiment of the invention scheme, preferably, the stirring velocity in described step 3 is 1000-10000r/min.
In the preparation method of above-mentioned few layer graphene, the gas that described supercutical fluid obtains after pressure reduction can be put into gas tank and reclaim storage use to be recycled.
According to specific embodiment of the invention scheme, preferably, the purification process of concrete Graphite Powder 99 comprises the following steps:
Step one: by Graphite Powder 99 ultrasonic cleaning, removes impurity;
Step 2: remove dephasign material and impurity element through chemical treatment or alternate manner.
Present invention also offers a kind of few layer graphene, it is prepared by above-mentioned preparation method.
According to specific embodiment of the invention scheme, the ratio of the few layer graphene of the number of plies prepared by aforesaid method below 10 layers is more than 60%, and preferably, the number of plies of described few layer graphene is 1-10 layer.
Present invention also offers a kind of device for the preparation of above-mentioned few layer graphene, it may be used for the preparation method of above-mentioned few layer graphene.This device comprises agitator motor, heating jacket, autoclave, gas-circulating system, agitator arm, stirring-head, wherein,
Described agitator arm is vertically positioned at the centre of autoclave, and described agitator arm one end outside autoclave connects agitator motor, and the other end extending to described autoclave base connects stirring-head;
The top of described autoclave is provided with injection port and gas inlet; Described injection port and described gas inlet are placed in the both sides of agitator motor;
Described heating jacket is wrapped in the outside of described autoclave;
The bottom of described autoclave is provided with outlet;
Described gas-circulating system comprises gas tank, the first valve, the second valve, under meter, condensing equipment and the 3rd valve, the pipeline of drawing from gas inlet is communicated with the first valve, gas tank, the second valve, under meter, condensing equipment and the 3rd valve successively, the pipeline that end of line is drawn with gas inlet is communicated with, and forms gas-circulating system; Wherein, first valve, the second valve and the 3rd valve are used for opening of pilot piping and close, under meter is used for the amount of meter gaseous, gas tank is for the gas of the gas that stores and recovery, condensing equipment carries out condensation to gas, work with ambient pressure pump one, make gas become supercritical state, any equipment that can realize this function can be adopted;
Described gas-circulating system is communicated with described gas inlet.
When adopting said apparatus to prepare few layer graphene, first, first valve, the second valve, the 3rd valve are in closure state, Graphite Powder 99 after purifying directly joined in autoclave or disperse to add afterwards in a solvent in autoclave, heated by heating jacket, after the temperature in autoclave reaches 35-60 DEG C, open the second valve, the 3rd valve, gas in gas tank is by condensing equipment condensation, working with ambient pressure pump one makes gas reforming be supercutical fluid, is pumped into by supercutical fluid in autoclave; Then, after pumping into supercutical fluid and making autoclave internal pressure be raised to 75atm-300atm, close the second valve and the 3rd valve, open agitator motor to stir, graphite is peeled away by the shearing force utilizing swiftly flowing supercutical fluid to produce, after stirring 30min-20h, pressure is reduced to 1atm in 5s-20s, after opening the first valve gas recovery, closes the first valve again; Finally, sample in autoclave, i.e. obtained few layer graphene.
The preparation method of few layer graphene provided by the present invention is the method for the few layer graphene of efficient preparation, can prepare high-quality few layer graphene in a large number, and the Graphene number of plies prepared by the method is few.
Preparation method's environmental protection of few layer graphene provided by the present invention, production cost is low, can recycle CO
2, reduce CO
2discharge and cost.The advantages such as meanwhile, also have reaction time short, technique is simple, and the lamella integrity of the few layer graphene prepared is good.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of few layer graphene provided by the present invention;
Fig. 2 is the structural representation of the few layer graphene device of preparation provided by the present invention;
Fig. 3 is transmission electron microscope (TEM) figure of few layer graphene prepared by embodiment 1;
Fig. 4 is another transmission electron microscope (TEM) figure of few layer graphene prepared by embodiment 1;
Fig. 5 is transmission electron microscope (TEM) figure of few layer graphene prepared by embodiment 2;
Fig. 6 is another transmission electron microscope (TEM) figure of few layer graphene prepared by embodiment 2.
Main Reference label:
1 autoclave 2 heating jacket 3 agitator motor 4 agitator arm 5 stirring-head 6 injection port 7 gas inlet 8 outlet 9 first valve 10 second valve 11 under meter 12 gas tank 13 condensing equipment 14 the 3rd valve
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, referring now to Figure of description, following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
Present embodiments provide a kind of device for the preparation of few layer graphene, its structure as shown in Figure 2.This device comprises: agitator motor 3, heating jacket 2, autoclave 1, gas-circulating system, agitator arm 4, stirring-head 5, wherein,
Agitator arm 4 is vertically positioned at the centre at autoclave 1 top, and agitator arm 4 one end outside autoclave 1 connects agitator motor 3, and the other end extended to bottom autoclave 1 connects stirring-head 5;
Injection port 6 and gas inlet 7 is provided with at the top of autoclave 1; Injection port 6 and gas inlet 7 are placed in the both sides of agitator motor 3;
Heating jacket 2 is wrapped in the outside of autoclave 1;
The bottom of autoclave 1 is provided with outlet 8;
Gas-circulating system comprises gas tank 12, first valve 9, second valve 10, under meter 11, condensing equipment 13 and the 3rd valve 14, the pipeline of drawing from gas inlet 7 is communicated with the first valve 9, gas tank 12, second valve 10, under meter 11, condensing equipment 13 and the 3rd valve 14 successively, end of line is communicated with the pipeline of drawing from gas inlet 7, forms gas-circulating system; Wherein, first valve 9 and the opening and closing for pilot piping of the second valve 10, under meter 11 is for the amount of meter gaseous, gas tank 12 is for the gas of the gas that stores and recovery, condensing equipment 13 pairs of gases carry out condensation, work with ambient pressure pump one, make gas become supercritical state, any equipment that can realize this function can be adopted; Gas-circulating system is communicated with gas inlet 7.
Utilize said apparatus to prepare few layer graphene, as shown in Figure 1, this preparation process specifically can comprise the following steps preparation flow figure:
Step one, preparation Graphite Powder 99: by 10g crystalline graphite powder ultrasonic cleaning (wash 1 time, ethanol washes 2 times) to remove dephasign material and impurity element;
Step 2, supercritical CO
2intercalation: the first valve 9, second valve 10, the 3rd valve 14 are in closure state, crystalline graphite powder after purifying directly to be joined in autoclave 1 and to heat, after the temperature in autoclave 1 reaches 35 DEG C, open the second valve 10, the 3rd valve 14, by the CO in gas tank 12
2gas, by condensing equipment 13 condensation, works CO with one of ambient pressure pump
2gas reforming is CO
2supercutical fluid, by CO
2supercutical fluid pumps in autoclave 1, CO
2the consumption of supercutical fluid is measured by under meter 11;
Step 3, supercritical CO
2shear: by pumping into CO
2after supercutical fluid makes autoclave 1 internal pressure be raised to 300atm, close the second valve 10 and the 3rd valve 14, open agitator motor 3 and stir, rotating speed is 10000r/min, utilizes swiftly flowing CO
2graphite is peeled away by the shearing force that supercutical fluid produces, and after stirring 30min, pressure is reduced to 1atm in 10s, closes the first valve 9 again after opening the first valve 9 gas recovery;
Step 4, obtain Graphene: sampling in autoclave 1, obtains described few layer graphene.
Obtained few layer graphene is taken pictures by transmission electron microscope (TEM), as shown in Figure 3 and Figure 4.The number of plies of few layer graphene prepared by the present embodiment is can be clearly seen that from Fig. 3 and Fig. 4, the defect simultaneously can observing Graphene is less, by adding up its number of plies, find that the ratio of the number of plies below 10 layers of the Graphene that embodiment 1 is obtained is about 60%.
Embodiment 2
The present embodiment provides a kind of preparation method of few layer graphene, and it utilizes the device described in embodiment 1 to prepare, and the method specifically comprises the following steps:
Step one, preparation Graphite Powder 99: by 1g expanded graphite powder ultrasonic cleaning (wash 1 time, ethanol washes 2 times) to remove dephasign material and impurity element;
Step 2, supercritical CO
2intercalation: the first valve 9, second valve 10, the 3rd valve 14 are in closure state, expanded graphite powder after purifying is dispersed in after in the sodium lauryl sulphate (SDS) that 200ml concentration is 1wt%, to join in autoclave 1 and to heat, after the temperature in autoclave 1 reaches 60 DEG C, open the second valve 10, the 3rd valve 14, by the CO in gas tank 12
2gas, by condensing equipment 13 condensation, works CO with one of ambient pressure pump
2gas reforming is CO
2supercutical fluid, by CO
2supercutical fluid pumps in autoclave 1, CO
2the consumption of supercutical fluid is measured by under meter 11;
Step 3, supercritical CO
2shear: by pumping into CO
2after supercutical fluid makes autoclave 1 internal pressure be raised to 75atm, close the second valve 10 and the 3rd valve 14, open agitator motor 3 and stir, rotating speed is 1000r/min, utilizes swiftly flowing CO
2graphite is peeled away by the shearing force that supercutical fluid produces, and stirs 20h, then pressure is reduced to 1atm in 10s, close the first valve 9 again after opening the first valve 9 gas recovery;
Step 4, obtain Graphene: sampling in autoclave 1, obtains described few layer graphene.
Obtained few layer graphene transmission electron microscope (TEM) is taken pictures, as shown in Figure 5 and Figure 6.The number of plies of few layer graphene prepared by the present embodiment is can be clearly seen that from Fig. 5 and Fig. 6, the defect simultaneously can observing Graphene is less, by adding up its number of plies, find that the ratio of the number of plies below 10 layers of the Graphene that embodiment 2 is obtained is about 80%.
Claims (7)
1. a preparation method for few layer graphene, it comprises the following steps:
Step one: purification process is carried out to Graphite Powder 99;
Step 2: the Graphite Powder 99 after purifying directly added in autoclave or disperse to add afterwards in autoclave in a solvent, heating, after the temperature in autoclave reaches 35-60 DEG C, supercutical fluid is pumped in autoclave;
Step 3: after pumping into supercutical fluid and making autoclave internal pressure be raised to 75atm-300atm, stir 30min-20h, stirring velocity is 1000-10000r/min, then pressure is reduced to 1atm in 5s-20s;
Step 4: sample in autoclave, obtains described few layer graphene.
2. preparation method according to claim 1, wherein, described supercutical fluid is CO
2supercutical fluid.
3. preparation method according to claim 1, wherein, described Graphite Powder 99 comprises crystalline graphite powder and/or expanded graphite powder.
4. preparation method according to claim 1, wherein, described solvent comprises sodium lauryl sulphate and/or Sodium dodecylbenzene sulfonate.
5. preparation method according to claim 1, wherein, puts into gas tank by the gas obtained after described supercutical fluid step-down and stores use to be recycled.
6. preparation method according to claim 1, wherein, the purification process of described Graphite Powder 99 comprises the following steps:
Step one: by Graphite Powder 99 ultrasonic cleaning, removes impurity;
Step 2: remove dephasign material and impurity element through chemical treatment or alternate manner.
7. the device adopted in the preparation method of the few layer graphene described in any one of claim 1-6, it comprises, agitator motor, heating jacket, autoclave, gas-circulating system, agitator arm, stirring-head, wherein,
Described agitator arm is vertically positioned at the centre of autoclave, and described agitator arm one end outside autoclave connects agitator motor, and the other end extending to described autoclave base connects stirring-head;
The top of described autoclave is provided with injection port and gas inlet; Described injection port and described gas inlet are placed in the both sides of agitator motor;
Described heating jacket is wrapped in the outside of described autoclave;
The bottom of described autoclave is provided with outlet;
Described gas-circulating system comprises gas tank, the first valve, the second valve, under meter, condensing equipment and the 3rd valve, the pipeline of drawing from gas inlet is communicated with the first valve, gas tank, the second valve, under meter, condensing equipment and the 3rd valve successively, the pipeline that end of line is drawn with gas inlet is communicated with, and forms gas-circulating system;
Described gas-circulating system is communicated with described gas inlet.
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| CN201310739904.1A CN103771401B (en) | 2013-12-26 | 2013-12-26 | A kind of preparation method of few layer graphene and device |
| PCT/CN2014/075917 WO2015096317A1 (en) | 2013-12-26 | 2014-04-22 | Method for preparing single-layered graphene |
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| CN106986329A (en) * | 2016-01-18 | 2017-07-28 | 上海交通大学 | A kind of method for preparing graphene |
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| CN108948578A (en) * | 2018-06-21 | 2018-12-07 | 多凌新材料科技股份有限公司 | Graphene/PVC anti-static composite material and preparation method thereof |
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| CN110065940A (en) * | 2019-06-19 | 2019-07-30 | 侯梦斌 | A kind of equipment and technology for intervening subcritical solvent pressure changeable removing carbon material |
| CN114426269B (en) * | 2020-10-13 | 2023-10-10 | 中国石油化工股份有限公司 | Graphene and preparation method thereof |
| CN112607728A (en) * | 2020-11-20 | 2021-04-06 | 中国科学院深圳先进技术研究院 | Automatic device for preparing graphene composite material by ultrasonic-assisted supercritical fluid |
| CN113750910A (en) * | 2021-08-27 | 2021-12-07 | 南京公诚节能新材料研究院有限公司 | Alkali metal carbon preparation facilities in supercritical fluid reaction system |
| CN114672156B (en) * | 2022-03-04 | 2023-04-18 | 上海交通大学 | Preparation method of graphene/PA 6 composite material |
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