CN203428916U - Supercritical reaction kettle for nanometer graphene preparation - Google Patents
Supercritical reaction kettle for nanometer graphene preparation Download PDFInfo
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- CN203428916U CN203428916U CN201320232378.5U CN201320232378U CN203428916U CN 203428916 U CN203428916 U CN 203428916U CN 201320232378 U CN201320232378 U CN 201320232378U CN 203428916 U CN203428916 U CN 203428916U
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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
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Abstract
The utility model relates to a supercritical reaction kettle for nanometer graphene preparation. The supercritical reaction kettle comprises a reaction kettle body, a heating system, a pressure control system and a collecting kettle, wherein the reaction kettle body is connected to the heating system, the pressure control system and the collecting kettle. The supercritical reaction kettle adopts a permanent magnetic driving stirrer with a U-shaped end surface, is completely and statically sealed, free of leakage, high at stirring speed, stable in operation, low in noise and convenient to operate and resists high temperature and high pressure; the supercritical reaction kettle is provided with the special product collecting kettle for preventing graphene from aggregating again and is used for the green production of graphene.
Description
Technical field
The utility model relates to a kind of supercritical reaction still of preparing nano-graphene for peeling off natural flake graphite.
Background technology
2004, New Two Dimensional atomic crystal-Graphene (Graphene) that the monoatomic layer that British scientist has been found to be connected with sp2 hydridization by carbon atom forms, its thickness is only 0.35nm, is the thinnest in the world two-dimensional material.Graphene carbon atom intensive by one deck, that be wrapped in honeycomb crystal lattice forms, and this special construction has contained abundant and novel physical phenomenon, makes Graphene show many excellent properties.If the intensity of Graphene is the highest in the material of having measured at present, reach 130GPa, there are 100 times of iron and steel; Its carrier mobility reaches 15000cm2V
-1s
-1, surpass the more than 10 times of commercial silicon chip mobility.Its thermal conductivity can reach 5000Wm
-1k
-1, be adamantine 3 times; And Graphene also has the special propertys such as room temperature quantum hall effect and room-temperature ferromagnetic.Because Graphene has the many merits such as excellent performance, with low cost, workability is good, Graphene will have great application prospect in fields such as electronics, information, the energy, material and biological medicines, is expected to start a new technological revolution in 21 century.In recent years, people, having obtained positive progress aspect the preparation of Graphene, had been developed the several different methods such as mechanically peel, crystal epitaxy, chemistry redox, organic synthesis and chemical vapour deposition.But, adopt these methods to be difficult to realize a large amount of productions of Graphene, but also can in preparing the process of Graphene, introduce defect and impurity.Supercritical fluid method can be realized the complete of Graphene and peel off, preparation structural integrity, and high-quality single-layer graphene, is expected to utilize supercritical fluid method to realize the industrialized mass production of Graphene.
Utility model content
The technical problem that the utility model solves is to provide a kind of supercritical reaction still of preparing for nano-graphene, to solve the shortcoming in above-mentioned background technology.
The technical problem that the utility model solves realizes by the following technical solutions:
A supercritical reaction still prepared by nano-graphene, comprising: reactor, heating system, control pressure system, collection still, described reactor connects heating system, control pressure system, collection still.
Further, reactor is provided with lagging casing outward, and described reactor is provided with kettle cover, and motor is installed on kettle cover, and motor connects agitator.
Further, described control pressure system is comprised of condenser, tensimeter, gas cylinder, and described gas cylinder and reactor connecting tube are provided with tensimeter.
One, technical process:
High-purity natural crystalline flake graphite adds in reactor, adds a certain amount of supercutical fluid, as CO
2water, ethanol, N, N dimethyl formamide etc., magnetic agitation is after for some time, and starting to heat up causes design temperature, is pressurized to setting air pressure, pressure-maintaining and heat-preservation for some time, react complete, material can be emitted from the discharge port at the bottom of still, Graphene product is injected to the product collection container that fills sodium dodecyl sulfate solution.
Two, reactor parameter:
Supercritical fluid method is prepared the reaction unit of Graphene mainly by reactor, heating system, and control pressure system and product acquisition system form.
1, a certain amount of high-purity natural crystalline flake graphite is added in autoclave, reactor is the principal reaction place of material, and attached body liner adopts stainless steel 1Cr18Ni9Ti to make, and reactor volume is 50～2000mL;
2, supercutical fluid injects after autoclave, cover reaction kettle cover, reaction kettle cover is the major parts of this reactor, on kettle cover, there are agitator, precision pressure gauge, the device such as safety valve, air valve, the response situation of controlling and grasp material in still according to these devices, regulates temperature, pressure etc., and assurance reaction safety is carried out; The sealing of kettle and kettle cover adopts without pad arc surface and conical surface linear sealing, relies on higher working accuracy and the screwing force of king bolt, reaches sealing effectiveness;
3, cover after kettle cover, start stirring reaction material.Open magnetic stirring apparatus, this magnetic stirring apparatus is permanent magnet coupling device, by inside-and-outside ring magnet steel, formed, there is the spacer of pressure-bearing centre, magnetic force by servomotor by inside and outside magnet steel transmits mixing torque, without mechanical component, medium completely in the encloses container in static seal, can not produce medium and reveal in operating process;
4, reactor agitator speed control section: drive-motor adopts DC servo motor, power acquisition silicon controlled rectifier, regulate electric machine speed regulation potentiometer, can control inputs electric moter voltage, realize the rotating speed of motor by 0～3000 turn/min stepless speed regulation, by being contained in the magnet steel on interior magnet steel axle top and the induced signal of detecting element, feed back to micro-chip, amplify as calculated, the tachometer gage that is transformed into front panel shows concrete numerical value;
5, open well heater, starting to heat up causes preset temp.The well heater of reactor is the electric heater of rated output 500～3000W, adopts N-8000 type digital temperature controller to control temperature, and temperature control precision is ± 1 ℃;
6, band over-temp and over-pressure warning device;
7, after reaction finishes, by product by still at the bottom of discharge opening directly leak into and fill product and gather in still, this still is polytetrafluoroethyllining lining, the interior Sheng sodium dodecylbenzenesulfonate aqueous solution, the concentration of the aqueous solution be 0.02M～2M for stoping Graphene to be reunited once again, guarantee to collect single or multiple lift Graphene.
Beneficial effect:
The utility model adopts overcritical still to prepare nano-graphene, and the production time is short, and cost is low, pollution-free, and product quality is high; The end face shape of a hoof permanent magnetic drive agitator adopting, completely static seal, without leaking, high temperature resistant, high pressure, mixing speed be high, operate steadily, noise is little, easy to operate; Product-collecting is to be provided with special-purpose product-collecting still, for stoping Graphene to be reunited once again, is mainly used in the green production of Graphene.
Accompanying drawing explanation
Fig. 1 is the utility model structural representation.
Embodiment
As shown in Figure 1 and the organic oils retrieving arrangement of photodegradation, tensimeter 1, motor 2, kettle cover 3 gas cylinders 4, condenser 5, reactor 6, lagging casing 7, well heater 8, collect still 9.
Embodiment 1:
Adopting supercutical fluid reaction unit to prepare Graphene is to carry out according to the following steps:
1, the high-purity natural crystalline flake graphite that is 99.995% by the purity of 10g adds in autoclave 6, and reactor 6 is principal reaction places of material, and attached body liner adopts stainless steel 1Cr18Ni9Ti to make, and reactor 6 volumes are 500mL;
2, supercutical fluid N, N dimethyl formamide 200mL injects after autoclave 6, cover kettle cover 3, kettle cover 3 is major partss of this reactor 6, on kettle cover 3, have agitator, precision pressure gauge 1, the devices such as safety valve, air valve, according to the response situation of material in these device controls and grasp still, regulate temperature, pressure etc., guarantee to react safety and carry out; Reactor 6 adopts without pad arc surface and conical surface linear sealing with the sealing of kettle cover 3, relies on higher working accuracy and the screwing force of king bolt, reaches sealing effectiveness;
3, open magnetic stirring apparatus, stir 2 hours, this magnetic stirring apparatus is permanent magnet coupling device, by inside-and-outside ring magnet steel, formed, there is the spacer of pressure-bearing centre, and the magnetic force by servomotor 2 by inside and outside magnet steel transmits mixing torque, without mechanical component, medium completely in the encloses container in static seal, can not produce medium and reveal in operating process;
4, reactor 6 agitator speed control sections: drive-motor 2 adopts DC servo motor 2, power acquisition silicon controlled rectifier, adjusting motor 2 speed-regulating potentiometers, can control inputs motor 2 voltages, realize the rotating speed of motor 2 by 0～3000;
Turn/min stepless speed regulation, by being contained in the magnet steel on interior magnet steel axle top and the induced signal of detecting element, feeds back to micro-chip, amplifies as calculated, and the tachometer gage that is transformed into front panel shows concrete numerical value;
5, open well heater 8, starting to heat up causes preset temp, and the well heater 8 of reactor 6 is the electric heater 8 of rated output 3000W, adopts N-8000 type digital temperature controller to control temperature, and temperature control precision is ± 1 ℃;
7, after reaction finishes, by product by still at the bottom of discharge opening directly leak into and fill in product-collecting still 9, this still is polytetrafluoroethyllining lining, the interior Sheng sodium dodecylbenzenesulfonate aqueous solution, the concentration of the aqueous solution is 0.05M, for stoping Graphene to be reunited once again, guarantees to collect single or multiple lift Graphene.
Embodiment 2:
Adopting supercutical fluid reaction unit to prepare Graphene is to carry out according to the following steps:
1, the high-purity natural crystalline flake graphite that is 99.995% by the purity of 10g adds in autoclave 6, and reactor 6 is principal reaction places of material, and attached body liner adopts stainless steel 1Cr18Ni9Ti to make, and reactor 6 volumes are 500mL;
2, supercutical fluid ethanol 200mL injects after autoclave 6, cover kettle cover 3, kettle cover 3 is major partss of this reactor 6, on kettle cover 3, there are agitator, precision pressure gauge 1, the device such as safety valve, air valve, the response situation of controlling and grasp reactor 6 interior materials according to these devices, regulates temperature, pressure etc., and assurance reaction safety is carried out; Reactor 6 adopts without pad arc surface and conical surface linear sealing with the sealing of kettle cover 3, relies on higher working accuracy and the screwing force of king bolt, reaches sealing effectiveness;
3, open magnetic stirring apparatus, stir 2 hours, this magnetic stirring apparatus is permanent magnet coupling device, by inside-and-outside ring magnet steel, formed, there is the spacer of pressure-bearing centre, and the magnetic force by servomotor 2 by inside and outside magnet steel transmits mixing torque, without mechanical component, medium completely in the encloses container in static seal, can not produce medium and reveal in operating process;
4, reactor 6 agitator speed control sections: drive-motor 2 adopts DC servo motor 2, power acquisition silicon controlled rectifier, adjusting motor 2 speed-regulating potentiometers, can control inputs motor 2 voltages, realize the rotating speed of motor 2 by 0～3000
Turn/min stepless speed regulation, by being contained in the magnet steel on interior magnet steel axle top and the induced signal of detecting element, feeds back to micro-chip, amplifies as calculated, and the tachometer gage that is transformed into front panel shows concrete numerical value;
5, open well heater 8, starting to heat up causes preset temp, and the well heater 8 of reactor 6 is the electric heater 8 of rated output 3000W, adopts N-8000 type digital temperature controller to control temperature, and temperature control precision is ± 1 ℃;
7, after reaction finishes, by product by still at the bottom of discharge opening directly leak into and fill in product-collecting still 9, this still is polytetrafluoroethyllining lining, the interior Sheng sodium dodecylbenzenesulfonate aqueous solution, the concentration of the aqueous solution is 0.05M, for stoping Graphene to be reunited once again, guarantees to collect single or multiple lift Graphene.
More than show and described ultimate principle of the present utility model and principal character and advantage of the present utility model, the technician of the industry should understand, the utility model is not restricted to the described embodiments, that in above-described embodiment and specification sheets, describes just illustrates principle of the present utility model, do not departing under the prerequisite of the utility model spirit and scope, the utility model also has various changes and modifications, these changes and improvements all fall within the scope of claimed the utility model, the claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (1)
1. a supercritical reaction still of preparing for nano-graphene, comprise: reactor, heating system, control pressure system, collection still, it is characterized in that, described reactor connects heating system, control pressure system, collection still, reactor is provided with lagging casing outward, described reactor is provided with kettle cover, motor is installed on kettle cover, motor connects agitator, agitator is end face shape of a hoof permanent magnetic drive agitator, described control pressure system is comprised of condenser, tensimeter, gas cylinder, and described gas cylinder and reactor connecting tube are provided with tensimeter.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320232378.5U CN203428916U (en) | 2013-05-02 | 2013-05-02 | Supercritical reaction kettle for nanometer graphene preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320232378.5U CN203428916U (en) | 2013-05-02 | 2013-05-02 | Supercritical reaction kettle for nanometer graphene preparation |
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| CN203428916U true CN203428916U (en) | 2014-02-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044765A (en) * | 2016-08-17 | 2016-10-26 | 新奥科技发展有限公司 | Apparatus and method of supercritically preparing graphene |
-
2013
- 2013-05-02 CN CN201320232378.5U patent/CN203428916U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044765A (en) * | 2016-08-17 | 2016-10-26 | 新奥科技发展有限公司 | Apparatus and method of supercritically preparing graphene |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140212 Termination date: 20150502 |
|
| EXPY | Termination of patent right or utility model |