CN104556010A - Process for industrially producing graphene by microwaves - Google Patents
Process for industrially producing graphene by microwaves Download PDFInfo
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- CN104556010A CN104556010A CN201410846442.8A CN201410846442A CN104556010A CN 104556010 A CN104556010 A CN 104556010A CN 201410846442 A CN201410846442 A CN 201410846442A CN 104556010 A CN104556010 A CN 104556010A
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Abstract
The invention relates to a process for industrially producing graphene by microwaves. Equipment adopted in the process comprises a spiral feeder, a furnace tube, a microwave cavity, a material discharging pipe and a product collector, wherein the furnace tube is connected to the microwave cavity in a penetrating manner; the input end of the furnace tube is connected with the spiral feeder; the output end of the furnace tube is connected with the product collector through the material discharging pipe; an inert gas inlet and a compressed air inlet are formed in the input end of the furnace pipe. Graphite is oxidized into oxidized graphite under the action of strong acid and strong oxidant such as H2SO4, HNO3 and HClO4s or is hydrolyzed into oxidized graphite under the electrochemical peroxidation effect; the oxidized graphite is prepared after being subjected to filtering, granulation and the like; inert gas is used for replacing air in the furnace tube; under the inert gas atmosphere, the oxidized graphite is dissociated by the microwaves and is reduced into flocculent graphene easy to fly; the compressed air inlet is opened, and the reduced graphene enters the product collector along with the compressed air and is completely absorbed by water pre-stored in the device; suspension is filtered and dried to be solid powder, so that the production process for the graphene is finished.
Description
Technical field
The present invention relates to graphene new material technology of preparing, be specifically related to a kind of equipment and technology utilizing Microwave industrial to produce Graphene.
Background technology
Graphene (Graphene) is the carbon atomic layer of monoatomic thickness, is that carbon atom is only the individual layer two dimensional crystal being arranged in honeycomb lattice (honeycomb crystal lattice) of the hexaplanar of individual layer atom with the thickness that sp2 hydbridized carbon atoms is formed.Graphene is one the thinnest in known materials, also unusual rigid; As simple substance, it at room temperature transmits the speed of electronics than known all conductors and semi-conductor all fast (in Graphene, the travelling speed of electronics reaches 1/300 of the light velocity).Meanwhile, as monolayer carbon atomic structure, the theoretical specific surface area of Graphene is up to 3000m2/g.So high specific surface area makes to become extremely promising energy storage active material based on the material of Graphene, in storage hydrogen, new type lithium ion battery, ultracapacitor or fuel cell etc., have good application prospect.
At present, prepare this special MATERIALS METHODS of Graphene to comprise: slight rubbing manipulation or tear tape method (pasting HOPG), heating SiC method, metal substrate chemical Vapor deposition process, oxidation reduction process etc.First three methods is due to the reason not suitable for mass production Graphene such as productive rate is low or apparatus expensive, process be loaded down with trivial details.The advantage that oxidation reduction process has productive rate higher because of it is more suitable for scale operation comparatively speaking.
But the chemical reducing agent (as hydrazine hydrate) that traditional oxidation reduction process adopts has very large toxicity, to such an extent as to this method of reducing constitutes larger threat to health of human body and environment protection.Thermal reduction method has fast and reduction ratio advantage more thoroughly; But generally need to carry out under the high temperature more than 1000 DEG C owing to heating, add the energy consumption of whole process.And this method needs the costly equipment such as high-temperature heater.It is fast that microwave exposure heating has speed, and cost is low, uses the features such as simple.Irradiation oxidation graphite granule can obtain the fluffy graphene powder of black within one minute.But common microwave exposure carries out in atmosphere, the Graphene that obtains of first reducing very easily burns and even causes fire to suffer under microwave exposure, and the industrial applications of producing Graphene for microwave method brings potential security threat.And the Graphene loft that microwave exposure obtains very high (can reach 100L/g), light weight easily flies upward, and is difficult to collect.These problems become the obstacle of microwave radiation method suitability for industrialized production Graphene.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of structure simple, productive rate is high, is applicable to industrial production, and the Microwave industrial that utilizes of being convenient to collect finished product produces the equipment and technology of Graphene.
The technical solution used in the present invention is:
A kind ofly can produce the equipment of Graphene by industrialized utilization microwave, comprise screw feeder, boiler tube, microwave cavity, discharge nozzle and product-collecting device, described boiler tube is connected in microwave cavity, the input terminus of boiler tube connects screw feeder, the output terminal end of described boiler tube connects product-collecting device through discharge nozzle, and the input terminus of described boiler tube is provided with inert gas import and compressed air inlet.
Further, described microwave cavity inwall is evenly provided with multiple microwave emitter.
Further, the output terminal of described screw feeder extends in the superposition section of boiler tube and microwave cavity.
Further, described product-collecting device is encloses container, establishes absorption water body in product-collecting device, and product-collecting device top is provided with vacuum orifice.
Again further, described screw feeder material is tetrafluoroethylene; Described microwave cavity material is high-boron-silicon glass, corundum or quartz; Described boiler tube, discharge nozzle material are liner polytetrafluoro stainless steel.
Producing the technique of Graphene is: graphite is oxidized to graphite oxide under the effect of the strong acid such as H2SO4, HNO3, HClO4 and strong oxidizer, or under electrochemistry peroxidation, after hydrolysis, forms graphite oxide; Graphite oxide after filtration, the operation such as granulation is prepared into diameter at 0.1-1cm, and length is at the cylindrical particle of 1-5cm; The single inlet amount of graphite oxide is 100-2000 gram, preferred 200-800 gram; Graphite oxide raw material enters boiler tube inside after metering from screw feeder; Open inert gas import, air in displacement boiler tube, graphite oxide dissociates through microwave under an inert atmosphere, graphite oxide is reduced to the cotton-shaped Graphene easily flown upward, open compressed air inlet, the Graphene after reduction enters product-collecting device with flowing pressurized air and is absorbed completely by the water prestored in device.Suspension obtains pressed powder via filtration, drying, thus completes the production technique of Graphene.
Adopt technique scheme, the invention has the beneficial effects as follows:
1. screw feeder is used for the boiler tube that to be quantitatively transported to by graphite oxide in microwave cavity by measuring apparatus, by screw feeder end part flow arrangement, graphite oxide is evenly laid in the middle part of boiler tube, be convenient to even microwave dissociate, control output further and improve the quality of products.
2. screw feeder is tetrafluoroethylene material; Microwave boiler tube is high-boron-silicon glass, corundum or quartzy material; Boiler tube, discharge nozzle are liner polytetrafluoro stainless steel, effectively can prevent the sour gas corrosion that microwave leakage preventing produces in reaction process, extension device work-ing life.
3. large to the treatment capacity of boiler tube internal screw feeding to graphene oxide, continuous print treating processes can be realized, prepare graphene oxide powder incessantly, and filter after collecting water body absorption graphene powder, dry Graphene finished product, 1 gram of graphene oxide powder to a few hectogram can be made at short notice to change Graphene into according to the size of boiler tube, avoid current productive rate low, and rapid thermal process graphite oxide prepares the problem that volume sharply expands and powder difficulty is collected of graphene powder, the Graphene of oxidation output, can directly and polymer directly by Banbury mixer or forcing machine compound, and do not need again through pulverizing or grinding, prepare polymer composite, rear and other materials compound can be disperseed in water or organic solvent, also sensor can be directly used in, photochemical catalysis, absorption, solar cell and nano-device etc.
It is simple that this microwave produces Graphene device structure, and easy to operate, safety non-pollution, achieves the continuous industrial production of graphene product, improves quality product and productive rate.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
In figure: helical screw feeder 1, boiler tube 2, inert gas import 3, compressed air inlet 4, microwave cavity 5, discharge nozzle 6, product-collecting device 7, vacuum orifice 8.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further.
Shown in Fig. 1, a kind ofly can to produce the equipment of Graphene and comprise helical screw feeder 1, boiler tube 2, inert gas import 3, compressed air inlet 4, microwave cavity 5, discharge nozzle 6, product-collecting device 7 and vacuum orifice 8 by industrialized utilization microwave.Described boiler tube 2 is connected in microwave cavity 5, the input terminus of described boiler tube 2 is connected with screw feeder 1, tetrafluoroethylene material selected by described screw feeder 1, the output terminal of described boiler tube 2 connects product-collecting device 7 through discharge nozzle 6, and liner polytetrafluoro stainless steel selected by described boiler tube 2 and discharge nozzle 6; Described microwave cavity 5 inwall is evenly provided with multiple microwave emitter, and described microwave cavity 5 selects the materials such as high-boron-silicon glass, corundum or quartz; The input terminus of described boiler tube 2 is provided with inert gas import 3 and compressed air inlet 4; With gauger on described screw feeder 1, the output terminal of described screw feeder stretches to microwave cavity 5 with in the superposition section of boiler tube 2; Establish absorption water body in described product-collecting device 7, product-collecting device top is provided with vacuum orifice 8, and described discharge nozzle stretches in the water body in product-collecting device 7.
The technique of the production Graphene of the technical program is taked to be: graphite to be oxidized to graphite oxide under the effect of the strong acid such as H2SO4, HNO3, HClO4 and strong oxidizer, or under electrochemistry peroxidation, after hydrolysis, to form graphite oxide; Graphite oxide after filtration, the operation such as granulation is prepared into diameter at 0.1-1cm, and length is at the cylindrical particle of 1-5cm; The single inlet amount of graphite oxide is 100-2000 gram, preferred 200-800 gram; Graphite oxide raw material enters boiler tube inside after metering from screw feeder; Open inert gas import, air in displacement boiler tube, graphite oxide dissociates through microwave under an inert atmosphere, graphite oxide is reduced to the cotton-shaped Graphene easily flown upward, open compressed air inlet, the Graphene after reduction enters product-collecting device with flowing pressurized air and is absorbed completely by the water prestored in device.Suspension obtains pressed powder via filtration, drying, thus completes the production technique of Graphene.
Claims (5)
1. can produce the technique of Graphene by industrialized utilization microwave for one kind, it is characterized in that: equipment: comprise screw feeder, boiler tube, microwave cavity, discharge nozzle and product-collecting device, described boiler tube is connected in microwave cavity, the input terminus of boiler tube connects screw feeder, the output terminal end of described boiler tube connects product-collecting device through discharge nozzle, the input terminus of described boiler tube is provided with inert gas import and compressed air inlet, by graphite at H2SO4, HNO3, graphite oxide is oxidized under the effect of the strong acid such as HClO4 and strong oxidizer, or under electrochemistry peroxidation, graphite oxide is formed after hydrolysis, graphite oxide after filtration, the operation such as granulation is prepared into diameter at 0.1-1cm, and length is at the cylindrical particle of 1-5cm, the single inlet amount of graphite oxide is 100-2000 gram, preferred 200-800 gram, graphite oxide raw material enters boiler tube inside after metering from screw feeder, open inert gas import, air in displacement boiler tube, graphite oxide dissociates through microwave under an inert atmosphere, graphite oxide is reduced to the cotton-shaped Graphene easily flown upward, open compressed air inlet, Graphene after reduction enters product-collecting device with flowing pressurized air and is absorbed completely by the water prestored in device, and suspension obtains pressed powder via filtration, drying, thus completes the production technique of Graphene.
2. according to claim 1ly a kind ofly can produce the technique of Graphene by industrialized utilization microwave, it is characterized in that: described microwave cavity inwall is evenly provided with multiple microwave emitter.
3. according to claim 1 and 2ly a kind ofly can produce the technique of Graphene by industrialized utilization microwave, it is characterized in that: the output terminal of described screw feeder extends in the superposition section of boiler tube and microwave cavity.
4. according to claim 1ly a kind ofly can produce the technique of Graphene by industrialized utilization microwave, it is characterized in that: described product-collecting device is encloses container, establishes absorption water body in product-collecting device, product-collecting device top is provided with vacuum orifice.
5. according to claim 1ly a kind ofly can produce the technique of Graphene by industrialized utilization microwave, it is characterized in that: described screw feeder material is tetrafluoroethylene; Described microwave cavity material is high-boron-silicon glass, corundum or quartz; Described boiler tube, discharge nozzle material are liner polytetrafluoro stainless steel.
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| CN201410846442.8A CN104556010A (en) | 2014-12-31 | 2014-12-31 | Process for industrially producing graphene by microwaves |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108584929A (en) * | 2018-07-01 | 2018-09-28 | 张阳 | A kind of production equipment of graphene |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100301212A1 (en) * | 2009-05-18 | 2010-12-02 | The Regents Of The University Of California | Substrate-free gas-phase synthesis of graphene sheets |
| CN102730678A (en) * | 2012-07-23 | 2012-10-17 | 贵州新碳高科有限责任公司 | Device and method for preparing graphene powder |
| CN203612963U (en) * | 2013-11-22 | 2014-05-28 | 国能纳米科技有限公司 | Expansion furnace provided with rotary quartz tube and capable of being fed continuously |
| CN104085886A (en) * | 2014-07-28 | 2014-10-08 | 嵇天浩 | Graphene and preparation method thereof |
| CN104108701A (en) * | 2014-06-25 | 2014-10-22 | 苏州世优佳电子科技有限公司 | Preparation method of graphene |
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- 2014-12-31 CN CN201410846442.8A patent/CN104556010A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100301212A1 (en) * | 2009-05-18 | 2010-12-02 | The Regents Of The University Of California | Substrate-free gas-phase synthesis of graphene sheets |
| CN102730678A (en) * | 2012-07-23 | 2012-10-17 | 贵州新碳高科有限责任公司 | Device and method for preparing graphene powder |
| CN203612963U (en) * | 2013-11-22 | 2014-05-28 | 国能纳米科技有限公司 | Expansion furnace provided with rotary quartz tube and capable of being fed continuously |
| CN104108701A (en) * | 2014-06-25 | 2014-10-22 | 苏州世优佳电子科技有限公司 | Preparation method of graphene |
| CN104085886A (en) * | 2014-07-28 | 2014-10-08 | 嵇天浩 | Graphene and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108584929A (en) * | 2018-07-01 | 2018-09-28 | 张阳 | A kind of production equipment of graphene |
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Application publication date: 20150429 |