CN102992315A - Device for preparing graphene - Google Patents
Device for preparing graphene Download PDFInfo
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- CN102992315A CN102992315A CN2013100169157A CN201310016915A CN102992315A CN 102992315 A CN102992315 A CN 102992315A CN 2013100169157 A CN2013100169157 A CN 2013100169157A CN 201310016915 A CN201310016915 A CN 201310016915A CN 102992315 A CN102992315 A CN 102992315A
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Abstract
A device for preparing graphene is provided with a high pressure kettle. A holder is installed at a material outlet at the upper end of the high pressure kettle, a rupture piece is installed in the holder, a supercritical fluid inlet, a pressure meter connector and a temperature meter connector are further installed on the high pressure kettle and are connected with a feeding valve, a pressure meter or a pressure displayer and a temperature meter, a jacket is installed on the periphery of the high pressure kettle, a hot media inlet and a hot media outlet are arranged on the jacket, the hot media are heat conduction oil and steam, and a product collector is communicated onto the outside of the rupture piece. By means of the device for preparing graphene in a physical method, the prepared graphene is good in quality, free of three waste discharge, simple in process and capable of achieving scale industrial production of graphene.
Description
Technical field
The present invention relates to technical field of new material preparation, be specifically related to a kind of device for the preparation of Graphene.
Background technology
The whole world scientific circles that appear at of Graphene have caused huge repercussion, because it has unusual conductivity, extremely strong intensity and toughness, good light transmission, caused the strong research and development upsurge of a field intensity in modern field of new, although the Graphene discovery time is very short, also be in conceptual phase, but its unique physical structure and excellent mechanics, electric property makes it in nanoelectronics, microtronics, the field such as matrix material and energy storage material is with a wide range of applications, become forward position and the focus of scientific circles' research, be expected at nano electron device, battery, ultracapacitor, hydrogen storage material, the field such as field emmision material and hypersensor is widely used.
At present, the preparation method of Graphene has mechanical process, epitaxial growth method, chemical Vapor deposition process and oxidation reduction process.First three methods is low or condition is harsh because of efficient; or immature; fail in the large-scale production field, to be applied; though oxidation reduction process can be in industrial employing; but the Graphene for preparing is second-rate; wastewater flow rate is large, and this also is the larger weakness of this method, so people urgently wish to develop a kind of environmental friendliness, technique is simple, cost is low, the method for preparing Graphene and the device of good product quality.
Summary of the invention
Technical problem to be solved by this invention is: solve the problem that above-mentioned prior art exists, and provide a kind of adopt physical method, scientific and reasonable, technique is simple, cost is low, good product quality and eco-friendly device for the preparation of Graphene.
The technical solution used in the present invention is:
A kind of device for the preparation of Graphene has autoclave, at the upper end of autoclave discharge port installing holder, rupture disk is installed in the clamper.
In the technique scheme, upper end its structure of discharge port installing holder of described autoclave is: the upper end discharge port of autoclave is connected with flange, and flange is connected and installed clamper.
In the technique scheme, supercutical fluid import, pressure gauge connection and thermometer boss are installed also on the described autoclave, are connected and installed respectively feed valve, tensimeter or pressure display unit, thermometer.
In the technique scheme, described autoclave periphery is equipped with chuck, and the outlet of heating agent import and heating agent is arranged on the chuck.
In the technique scheme, described heating agent is thermal oil or steam.
In the technique scheme, the described rupture disk outside is communicated with the product-collecting device.
In the technique scheme, described rupture disk can be selected right arch shape, antiarch shape or plate shaped, and market is purchased.
In the technique scheme, described autoclave is general-purpose equipment, withstand voltage 5-10MPa or more than the 10MPa.
In the technique scheme, described autoclave places on the vibrator.
The right part of autoclave is discharge port, after supercutical fluid in the still has been realized the infiltration dissolving of graphite raw material, utilizes the rupture disk explosion, formed moment Millisecond pressure release, force supercutical fluid to be vaporized in graphite layers, produce powerful thrust, make graphite peel off into Graphene.Than existing Graphene preparation facilities, the present invention is simple in structure, and it is good to prepare the Graphene quality, and cost is low.Recyclable because of supercritical solvent, so three-waste free discharge, throughput Size-dependent can be realized the scale preparation of Graphene in instrument size, are the new devices that a kind of new physics prepares Graphene.
Description of drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is for adopting the Graphene product transmission electron microscope figure of apparatus of the present invention preparation, and wherein illustration is the FFT image;
Fig. 3 is for adopting the Graphene Product Perspective electron microscope picture of apparatus of the present invention preparation.
Among the figure, 1-rupture disk, 2-clamper, 3-flange, 4-autoclave discharge port, 5-chuck, 6-autoclave, 7-thermal oil outlet (steam is import), 8-heat conductive oil inlet (steam is outlet), 9-thermometer boss, 10-pressure gauge connection, the import of 11-supercutical fluid.
Among above-mentioned Fig. 2, because to cause the image of Graphene be not very clear to the factor of carbon film on the copper mesh, but the FFT image in the illustration shows the number of plies of this Graphene very low (＜5), and electron-diffraction diagram is the hexagon of standard, there are not ghost image or assorted point, the crystalline state that Graphene is described is fine, defective seldom, quality is high;
Among above-mentioned Fig. 3, can observe clearly the thin slice pattern of Graphene, yardstick is near 2 microns; Graphene shows the structure of tulle shape, and its surface folding is high-visible, few surface defects, and integrity is better, does not have folding edge color more shallow, hardly as seen, the very thin thickness of this explanation graphene film.
Embodiment
Device for the preparation of Graphene of the present invention, as shown in Figure 1, comprise autoclave 6, autoclave discharge port 4, autoclave discharge port 4 is equipped with clamper 2 and rupture disk 1, rupture disk is installed in the middle of the clamper, the autoclave left part is equipped with thermometer boss 9, be used for installing thermometer, the autoclave left part is equipped with pressure gauge connection 10, be used for setting pressure table or pressure display unit, the autoclave left part also has supercutical fluid import 11, and the autoclave outside is equipped with chuck 5, interior admittance deep fat or steam are used for autoclave heating and insulation.
During use, autoclave is positioned on the vibrator, opens the flange 3 of discharge port, put into a certain amount of graphite, select suitable rupture disk, be installed in the middle of the clamper, clamper is put in the middle of the flange, screws bolt, makes it sealing.
Feed valve is linked to each other with supercutical fluid import 11, again feed valve is communicated with vacuum pump, be evacuated to 0.098MPa, close feed valve, then connect feed-pipe, open feed valve, pour into successively cosolvent and supercritical solvent, namely pour into supercutical fluid, close feed valve, open vibrator, admittance deep fat or steam heating are warmed up to specified temperature in the chuck, keep certain hour, slightly increase subsequently temperature, when pressure exceeds rupture disk and bears pressure, the rupture disk explosion, material is gone out in the moment Millisecond, and the receptor collection material is so far finished the Graphene preparation process one time.
The unusual effect that uses apparatus of the present invention to produce is as follows:
(1), the present invention can finish pressure release at moment (Millisecond), is better than existing technology:
Use apparatus of the present invention under supercritical state, utilize supercritical solvent perviousness and solvability to raw material graphite under supercritical state, make supercritical solvent enter Graphite Powder 99 inside (between layers), then adopt the quick-fried form of vapour, energy whole releases of moment within the extremely short time (Millisecond) are complete, follow shockwave to produce, its process is finished in the time at Millisecond, moment is finished expansion process, the gas that expands acts on graphite with the form of shockwave, graphite is carried out splitting, finish the preparation of Graphene.This device has realized that the repetitive operation number of times is few to efficiently the peeling off of graphite, and prepared Graphene quality is better, has broad application prospects.
Although and prior art has also adopted the piston fast pressure relief, but not reaching in Millisecond material all goes out, do not produce the Millisecond shockwave, material discharges balance from high pressure to low pressure by the front and back order successively, so can't produce the behavior of moment explosion, thereby do not reach the effect of moment pressure release, decompression process reaches far away in Millisecond reduces to normal pressure fast with the container inner high voltage, these acting processes are longer owing to the time, it is high-power not produce moment, do not have shockwave to produce, just can't reach the desired effect of peeling off to graphite yet.
(2), the present invention peels off the effect height:
As everyone knows, graphite is laminate structure, and 6 carbon atoms in every one deck consist of the plane reticular structure, connects with Van der Waals between layer and the layer.Graphite does not seal between layers, organic solvent can enter graphite between layers under supercritical state, when pressure release, supercritical solvent can be vaporized in graphite layers, also can overflow very soon from graphite layers, therefore supercritical solvent overflows in the graphite layers vaporization or from graphite layers, these two kinds of possibilities exist simultaneously in pressure leak process, overflowing is the main purpose of peeling off graphite that then do not reach, only just can reach the purpose of peeling off graphite to be vaporizated into the master, organic solvent is to overflow as main still to be vaporizated into the master, key is the control of pressure release time, compole is short when only having pressure leak process, finish pressure leak process at Millisecond in time, the organic solvent that enters graphite layers has little time to overflow, so vaporize in graphite layers (after the solvent vaporization, moment rapid expansion, volume can expand tens times to hundred times, produce thrust, graphite is peeled off), the gas that expands acts on graphite with the form of shockwave, graphite is peeled off into Graphene, what existing technostress discharged employing is the piston release, form with hydraulic pressure is opened or closure piston, utilize the release of this kind form to finish moment, adopt quick-opening valve (for example ball valve) release, can not finish moment equally, supercritical solvent enters graphite layers and vaporizes in graphite layers, be two processes that supplement and complement each other, indispensable, existing technology is only finished supercritical solvent and is entered graphite layers, fail to solve supercritical solvent interlayer vaporization (because of release slow, overflow as main take supercritical solvent from graphite layers), therefore that graphite is peeled off effect is very limited for existing technology, and preparation process needs repeatedly repetitive operation.
Not only solved supercritical solvent and entered graphite layers and adopt apparatus of the present invention to prepare Graphene, and solved supercritical solvent and vaporized in graphite layers, because the present invention adopts the rupture disk pressure release, its pressure leak process is finished in Millisecond, supercritical solvent has little time to overflow, can only vaporize in graphite layers, thereby reach the purpose of efficiently peeling off graphite.
(3), adopt apparatus of the present invention technique simple:
Adopt the Graphene technique of apparatus of the present invention preparation simple, domestic abundant raw material, cheap, the Graphene cost of preparation is low, is expected for the large-scale commercial production Graphene, produces larger economic benefit.
(4), adopt apparatus of the present invention without the three wastes:
The present invention has avoided using a large amount of chemical feedstockss, employed supercritical solvent recycle and reuse or make other purposes, three-waste free discharge, environmentally safe.And the present oxidation reduction process that is hopeful the scale operation Graphene most prepares one ton of Graphene and needs tens tons to hundred tons mineral acids, tens tons of inorganic oxidizer, produce a large amount of acid waste water and washes, contaminate environment, its waste water treatment expense is large, has increased production cost.
(5), quality product of the present invention is better:
The present invention does not need graphite is carried out oxide treatment and other chemical treatments, can not destroy the crystal structure of graphite, its preparation process is used physical method, therefore the Graphene quality of preparation is better, it is complete that crystalline structure keeps, can prove from the transmission electron microscope figure of Fig. 3 Graphene of the present invention, and the number of plies of Graphene is low, less than 5 layers.
(6), the present invention has industrialized prospect:
From the technology of the existing Graphene for preparing, can obtain the method for the measured Graphene of matter, such as the mechanically peel method, yield poorly, cost is high, is difficult to industrialization; And method that can the preparation of industrialization Graphene, oxidation reduction process for example, Graphene is second-rate, and its application is restricted; Adopt the Graphene quality of apparatus of the present invention preparation better, cost is low, and technique is simple, for the Graphene with the Physical preparation provides a new approach, has the bright prospects that industrial scale prepares Graphene.
The used rupture disk of the present invention becomes boat industrial safety limited liability company of system or Suzhou An Ligaoke safety equipment development corporation, Ltd. to provide by Chengdu, propane is provided by Changsha Lianhu acetylene company limited, and other employed raw materials and equipment etc. are all bought from market channel.
Claims (8)
1. the device for the preparation of Graphene is characterized in that: have autoclave, at the upper end of autoclave discharge port installing holder, rupture disk is installed in the clamper.
2. the device for the preparation of Graphene according to claim 1, it is characterized in that: upper end its structure of discharge port installing holder of described autoclave is: the upper end discharge port of autoclave is connected with flange, and flange is connected and installed clamper.
3. the device for the preparation of Graphene according to claim 1, it is characterized in that: supercutical fluid import, pressure gauge connection and thermometer boss also are installed on the described autoclave, are connected and installed respectively feed valve, tensimeter or pressure display unit, thermometer.
4. the device for the preparation of Graphene according to claim 1, it is characterized in that: described autoclave periphery is equipped with chuck, and the outlet of heating agent import and heating agent is arranged on the chuck.
5. the device for the preparation of Graphene according to claim 4, it is characterized in that: described heating agent is thermal oil or steam.
6. the device for the preparation of Graphene according to claim 1 is characterized in that: described rupture disk outside connection product-collecting device.
7. the device for the preparation of Graphene according to claim 1, it is characterized in that: described rupture disk is selected positive arch, antiarch shape or plate shaped.
8. the device for the preparation of Graphene according to claim 1, it is characterized in that: autoclave is positioned on the vibrator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100169157A CN102992315A (en) | 2013-01-17 | 2013-01-17 | Device for preparing graphene |
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| CN2013100169157A CN102992315A (en) | 2013-01-17 | 2013-01-17 | Device for preparing graphene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN110156002A (en) * | 2019-06-04 | 2019-08-23 | 新疆弘瑞达纤维有限公司 | A kind of preparation method of graphene oxide composite material |
| CN115124033A (en) * | 2022-06-30 | 2022-09-30 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
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| CN102115078A (en) * | 2011-01-19 | 2011-07-06 | 上海交通大学 | Method for preparing graphene by using supercritical fluid |
| CN102491314A (en) * | 2011-11-24 | 2012-06-13 | 中国科学院化学研究所 | Method for preparing graphene |
| CN102515155A (en) * | 2012-01-05 | 2012-06-27 | 上海交通大学 | Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation |
| CN102765717A (en) * | 2012-08-14 | 2012-11-07 | 余美群 | Method for preparing graphene |
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2013
- 2013-01-17 CN CN2013100169157A patent/CN102992315A/en active Pending
Patent Citations (4)
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| CN102115078A (en) * | 2011-01-19 | 2011-07-06 | 上海交通大学 | Method for preparing graphene by using supercritical fluid |
| CN102491314A (en) * | 2011-11-24 | 2012-06-13 | 中国科学院化学研究所 | Method for preparing graphene |
| CN102515155A (en) * | 2012-01-05 | 2012-06-27 | 上海交通大学 | Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation |
| CN102765717A (en) * | 2012-08-14 | 2012-11-07 | 余美群 | Method for preparing graphene |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN110156002A (en) * | 2019-06-04 | 2019-08-23 | 新疆弘瑞达纤维有限公司 | A kind of preparation method of graphene oxide composite material |
| CN110156002B (en) * | 2019-06-04 | 2023-02-10 | 新疆弘瑞达纤维有限公司 | Preparation method of graphene oxide material |
| CN115124033A (en) * | 2022-06-30 | 2022-09-30 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
| CN115124033B (en) * | 2022-06-30 | 2024-03-29 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
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Application publication date: 20130327 |