CN104925802B - A kind of chemical method prepares single-layer graphene automatic intelligent process units - Google Patents

A kind of chemical method prepares single-layer graphene automatic intelligent process units Download PDF

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CN104925802B
CN104925802B CN201510391663.5A CN201510391663A CN104925802B CN 104925802 B CN104925802 B CN 104925802B CN 201510391663 A CN201510391663 A CN 201510391663A CN 104925802 B CN104925802 B CN 104925802B
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sensor
controls
carries out
horizontal screw
screw centrifuge
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CN104925802A (en
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郭洪云
王福山
施建新
钟成
钱锋
潘东晓
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QINGDAO HUAGAO GRAPHENE TECHNOLOGY CORP., Ltd.
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Qingdao Huagao Ink Material Technology Co Ltd
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Abstract

The invention belongs to chemical method and prepare single-layer graphene equipment technical field, relate to a kind of chemical method and prepare single-layer graphene automatic intelligent process units, pre-oxidation still top connects the first chromatograph and controls device, first chromatograph controls device top and connects the first photoelectric sensor, first horizontal screw centrifuge top connects a pH sensor, bipyramid rotary vacuum drying upper box part connects temperature sensor and the first humidity sensor, oxidizing reactor top connects the second chromatograph and controls device, second chromatograph controls device top and connects the second photoelectric sensor, second horizontal screw centrifuge top connects the 2nd pH sensor and the time relay, spray dryer top connects the second humidity sensor, industrial microwave Heating Reduction Furnace for Tungsten top connects the second pressure and temp and vacuum sensor;It is rational in infrastructure, and principle is reliable, environmental friendliness, low cost, and automaticity is high.

Description

A kind of chemical method prepares single-layer graphene automatic intelligent process units
Technical field:
The invention belongs to chemical method and prepare single-layer graphene equipment technical field, relate to a kind of chemistry Method prepares single-layer graphene automatic intelligent process units, it is adaptable to the scale of single-layer graphene Producing, its automatic intelligent system uses preparation flow unit key element control program, according to chemistry Prepare single-layer graphene steps flow chart, be automatically performed the connection of unit, until preparing institute Need product graphene oxide aqueous dispersion liquid, graphene oxide powder and single-layer graphene powder body.
Background technology:
Graphene is the new material of the monolayer laminated structure being made up of carbon atom, is the most known The thinnest, the hardest nano material, have unusual electric conductivity, heat conductivity, beyond steel The intensity of ferrum decades of times and fabulous light transmission, can be widely applied to solaode, sensor, Nanoelectronics, high performance electronics, composite, field emmision material, gas sensor And the field such as energy storage, its appearance is expected to cause one to take turns leather at hyundai electronics sciemtifec and technical sphere Life, but, Graphene low yield, high cost, the problem such as of poor quality seriously constrain its development With application.At present, Graphene is also in research and development, pilot scale, small lot batch manufacture stage, industrialization It is immature to there is technical matters in production, does not has the production line of intelligentized control method.Due to Graphene work Industry metaplasia is produced producing each link requirement height, has a link to go wrong, and the product of production is just It is waste product, therefore prepares single-layer graphene automatic intelligent in the urgent need to a kind of chemical method of design raw Produce device, it is achieved the efficient low-consume of single-layer graphene production, reduction cost, energy-conserving and environment-protective, fall Low artificial intensity, favourable promotion Graphene large-scale production, there is good economic benefit and society Can be worth.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, seeking design provides one Chemical method prepares single-layer graphene automatic intelligent process units, it is achieved the scale of single-layer graphene Metaplasia is produced, and reaches efficient low-consume, cost-effective, the purpose of energy-conserving and environment-protective.
To achieve these goals, the agent structure of the present invention includes console, pre-oxidation Still, the first horizontal screw centrifuge, double conic rotary vacuum dryer, spray dryer, industrial microwave Heating Reduction Furnace for Tungsten, sewage disposal system, first chromatograph control device, the first pH sensor, Temperature sensor, the first humidity sensor, photoelectric sensor, the time relay, pressure temperature Degree and vacuum sensor, the first electromagnetic valve, first control element, second control element, the Two electromagnetic valves, the 3rd control element, the 4th control element, the 5th control element, oxidation reaction Still, the second chromatograph control device, the second photoelectric sensor, the second electromagnetic valve, the 6th control unit Part, the second horizontal screw centrifuge, the 2nd pH sensor, the 7th control element, the 8th control unit Part, the second pressure and temp and vacuum sensor, the 9th control element and the second humidity sensing Device;Console connects the 3rd control element control raw material input pre-oxidation still and carries out pre-oxygen Changing, pre-oxidation still top connects the first chromatograph control device and carries out color comparison, the first color Spectrum control device top connects the first photoelectric sensor and carries out signal transmission, the first photoelectric sensor Being connected to console and control the switch of the first electromagnetic valve, console and first controls to connect between element Being connected to the first electromagnetic valve, the first electromagnetic valve and first controls element and controls in pre-oxidation still Material is delivered to the first horizontal screw centrifuge and carries out filtration washing;First horizontal screw centrifuge top connects Oneth pH sensor carries out pH value comparison, and a pH sensor is connected to console and carries out letter Number transmission, be disposed with between console and bipyramid rotary vacuum drying oven the second electromagnetic valve and Second controls element, and second controls element controls the material input pair of the first horizontal screw centrifuge output Cone revolution vacuum drying oven is vacuum dried, and the 4th controls element is connected with sewage disposal system The waste water controlling the first horizontal screw centrifuge output enters sewage disposal system;Bipyramid rotary vacuum is done Dry upper box part connects has temperature sensor and the first humidity sensor to carry out temperature and wet respectively The comparison of degree, temperature sensor and the first humidity sensor are connected to console and carry out signal biography Defeated, the 5th controls element control material input oxidizing reactor aoxidizes;In oxidizing reactor Portion connects the second chromatograph control device and carries out color comparison, and the second chromatograph controls device top and connects Second photoelectric sensor carries out signal transmission, and the second photoelectric sensor is connected to console and controls the Two electromagnetic valve switch, console connects the second the magnetic valve controlled 6th unlatching controlling element, the Six the second horizontal screw centrifuges controlling element control material input oxidizing reactor lower end were carried out Filter washing;Second horizontal screw centrifuge top connects the 2nd pH sensor and time relay difference Carrying out pH value comparison and the time controls, the 2nd pH sensor is connected in series to the time relay Console carries out signal transmission, and the 7th controls element controls the part thing in the second horizontal screw centrifuge Material input spray dryer carries out lyophilization, and leftover materials are output as finished product graphene oxide water Phase dispersant liquid;Spray dryer top connects the second humidity sensor and carries out the humidity ratio of material Right, the 8th partial material input industrial microwave heating controlled in element control spray dryer is gone back Former stove carries out thermal reduction, and the partial material in spray dryer is output as finished product graphene oxide powder Body;Industrial microwave Heating Reduction Furnace for Tungsten top connects the second pressure and temp and carries out with vacuum sensor Pressure and temp and vacuum comparison, the 9th controls element is connected control with industrial microwave Heating Reduction Furnace for Tungsten Material in industrial microwave Heating Reduction Furnace for Tungsten processed is output as finished product single-layer graphene powder body.
It is concrete that the present invention uses chemical method to prepare the automatic intelligent production process of single-layer graphene Including pre-oxidation, oxidation, lyophilization, four steps of thermal reduction:
(1) pre-oxidation: console starts the 3rd control element and raw material is inputted pre-oxidation Still pre-oxidizes, and carries out color respectively through the first chromatograph control device and the first photoelectric sensor After comparison and signal output, the material in pre-oxidation still is inputted the first horizontal screw centrifuge and enters Row filtration washing, by the thing of the first horizontal screw centrifuge after a pH sensor carries out pH comparison Material input double conic rotary vacuum dryer is vacuum dried, through temperature sensor and the first dry and wet Material in double conic rotary vacuum dryer, to rear, is inputted oxidizing reactor by degree sensor ratio, 4th controls the waste water entrance sewage disposal system that element controls in the first horizontal screw centrifuge;
(2) oxidation: start the 5th control element, by the thing in double conic rotary vacuum dryer Material input oxidizing reactor, is carried out respectively through the second chromatograph control device and the second photoelectric sensor Color comparison and signal output, input the second horizontal screw centrifuge by the material in oxidizing reactor and enter Row filtration washing, after the 2nd pH sensor and the time relay are compared respectively, by Partial material in two horizontal screw centrifuges is output as finished product graphene oxide aqueous dispersion liquid, another Partial material carries out lyophilization;
(3) lyophilization: start the 7th control element, by the material in two horizontal screw centrifuges Input spray dryer, through the second humidity sensor carry out humidity ratio to after, spray dryer Interior partial material is output as finished product graphene oxide powder, and another part material carries out heat also Former;
(4) thermal reduction: start the 8th control element, the material in spray dryer is inputted Industrial microwave Heating Reduction Furnace for Tungsten, carries out pressure and temp through the second pressure and temp and vacuum sensor After vacuum comparison, it is output as finished product single-layer graphene powder body.
The work process of the present invention is: raw material is loaded reactor and pre-oxidizes, and treats that raw material reaches To expection color and luster, control device comparison by photo-sensor feedback to console, electricity through chromatograph Magnet valve is opened control element and feedstock transportation to horizontal screw centrifuge is centrifuged washing automatically, treats former Material reaches PH requirement, and by pH value sensor feedback to console, electromagnetic valve is opened and controlled unit Feedstock transportation is dried by part automatically to double conic rotary vacuum dryer, and another controls element and opens Open waste liquid be transported to sewage disposal system process treat that raw material reaches humidity requirement, pass through humidity Sensor feedback, to console, controls element unlatching and automatically feedstock transportation to reactor is carried out oxygen Change, treat that raw material reaches expection color and luster, control device comparison through chromatograph and pass through photo-sensor feedback To console, electromagnetic valve open control element automatically feedstock transportation to horizontal screw centrifuge is carried out from The heart washs, and treats that raw material reaches PH requirement, feeds back to console by pH sensor, pass through The time relay controls automatically partial material directly to be exported to make graphene oxide Aqueous dispersions Liquid, partial material is transported to spray dryer and is dried, and treats that raw material reaches humidity requirement, By humidity sensor feedback to console, control element and open partial material is the most direct Graphene oxide powder is made in output, and partial material is transported to microwave reduction stove and carries out also Former, treat that raw material produces a desired effect, in being fed back to by pressure, temperature and vacuum sensor Control platform, controls automatic directly the output by material of element unlatching and makes single-layer graphene powder body.
The present invention compared with prior art, uses console to control each unit behaviour in preparation process Make, set up intelligence manufacture apparatus assembly and couple and optimize system with parameter step by step, it is achieved high-quality stone Ink alkene scale low cost preparation and the breakthrough of function modulation technique, thus realize graphene powder Prepared by number of layers and size Control, modified and functionalization the scale of controlled surface.Pass through stone The single-layer graphene powder body of ink alkene intelligence manufacture mode of manufacture and Related product, product quality Height, annual capacity reaches 1000 tons;On the basis of chemical method prepares single-layer graphene, automatization System uses preparation flow node key element control program, by control system, sensor, control Device realizes the automatization of single-layer graphene automated production, quality control and functional modification, intelligence Energyization;Control of product quality passes through sensor, controller control accurate, and success rate is high, product Steady quality, production process safety, meet cleaning simultaneously and produce and the requirement of energy-conserving and environment-protective.Real Show efficient low-consume, reduction cost, energy-conserving and environment-protective that single-layer graphene produces, reduced artificial strong Degree, is suitable for industrialization and produces, improve competitiveness, implemented national energy-saving emission reduction tasks index, Improve enterprise clean production image, it is ensured that its competitive advantage;Its apparatus structure is reasonable, principle Reliably, environmental friendliness.
Accompanying drawing illustrates:
Fig. 1 is the agent structure principle schematic of the present invention.
Detailed description of the invention:
Below in conjunction with the accompanying drawings and by embodiment the present invention is made further description.
Embodiment:
The agent structure of the present embodiment includes console 1, pre-oxidation still 2, first crouches spiral shell The heating of centrifuge 3, double conic rotary vacuum dryer 4, spray dryer 5, industrial microwave is also Former stove 6, sewage disposal system the 7, first chromatograph control device the 8, first pH sensor 9, Temperature sensor the 10, first humidity sensor 11, photoelectric sensor 12, the time relay 13, pressure and temp and vacuum sensor the 14, first electromagnetic valve 15, first control element 16, Second controls element the 17, second electromagnetic valve the 18, the 3rd controls element the 19, the 4th control element 20, the 5th controls element 21, oxidizing reactor the 22, second chromatograph control device 23, second Photoelectric sensor the 24, second electromagnetic valve the 25, the 6th controls element the 26, second horizontal screw centrifuge 27, the 2nd pH sensor the 28, the 7th controls element the 29, the 8th and controls element 30, second Pressure and temp controls element 32 and the second humidity sensor with vacuum sensor the 31, the 9th 33;Console 1 connect the 3rd control element 19 control raw material input pre-oxidation still 2 enter Row pre-oxidation, pre-oxidation still 2 top connects the first chromatograph control device 8 and carries out color ratio Right, the first chromatograph control device 8 top connects the first photoelectric sensor 12 and carries out signal transmission, First photoelectric sensor 12 is connected to console 1 and controls the switch of the first electromagnetic valve 15, middle control Platform 1 controls to be connected between element 16 have the first electromagnetic valve 15 with first, the first electromagnetic valve 15 With first control element 16 control the material in pre-oxidation still 2 be delivered to first crouch spiral shell from Scheming 3 carries out filtration washing;First horizontal screw centrifuge 3 top connects a pH sensor 9 Carrying out pH value comparison, a pH sensor 9 is connected to console 1 and carries out signal transmission, in The second electromagnetic valve 18 and the it is disposed with between control platform 1 and bipyramid rotary vacuum drying oven 4 Two control element 17, and second controls element 17 controls the material input of horizontal screw centrifuge 3 output Bipyramid rotary vacuum drying oven 4 is vacuum dried, and the 4th controls element 20 and sewage disposal System 7 connects the waste water entrance sewage disposal system 7 controlling the first horizontal screw centrifuge 3 output; Bipyramid rotary vacuum drying oven 4 top connects temperature sensor 10 and the first humidity sensing Device 11 carries out the comparison of temperature and humidity, temperature sensor 10 and the first humidity sensing respectively Device 11 is connected to console 1 and carries out signal transmission, and the 5th controls element 21 controls material input Oxidizing reactor 22 aoxidizes;Oxidizing reactor 22 top connects the second chromatograph and controls device 23 carry out color comparison, and the second chromatograph controls device 23 top and connects the second photoelectric sensor 24 Carrying out signal transmission, the second photoelectric sensor 24 is connected to console 1 and controls the second electromagnetic valve 25 switches, console 1 connects the second electromagnetic valve 15 and manipulates the unlatching of the 6th control element 26, 6th controls element 26 controls the second horizontal screw centrifuge of material input oxidizing reactor 22 lower end 27 carry out filtration washing;Second horizontal screw centrifuge 27 top connects the 2nd pH sensor 28 He The time relay 13 carries out pH value comparison and time respectively and controls, the 2nd pH sensor 28 with The time relay 13 is connected in series to console 1 and carries out signal transmission, and the 7th controls element 29 Control the input spray dryer 5 of the partial material in the second horizontal screw centrifuge 27 and carry out freezing dry Dry, leftover materials are output as finished product graphene oxide aqueous dispersion liquid;Spray dryer 5 top Connecting the second humidity sensor 33 and carry out the humidity ratio pair of material, the 8th controls element 30 controls Partial material input industrial microwave Heating Reduction Furnace for Tungsten 6 in spray dryer 5 processed carries out heat also Former, the partial material in spray dryer 5 is output as finished product graphene oxide powder;Industry is micro- Wave heating reduction furnace 6 top connects the second pressure and temp and carries out pressure with vacuum sensor 31 Temperature and vacuum comparison, the 9th controls element 32 is connected with industrial microwave Heating Reduction Furnace for Tungsten 6 The material controlled in industrial microwave Heating Reduction Furnace for Tungsten 6 is output as finished product single-layer graphene powder body.
The present embodiment uses chemical method to prepare the automatic intelligent production process tool of single-layer graphene Body includes pre-oxidation, oxidation, lyophilization, four steps of thermal reduction:
(1) pre-oxidation: console 1 starts the 3rd control element 19 by raw material input pre-oxidation Reactor 2 pre-oxidizes, and controls device 8 and the first photoelectric sensor 12 through the first chromatograph After carrying out color comparison and signal output respectively, the material in pre-oxidation still 2 is inputted the One horizontal screw centrifuge 3 carries out filtration washing, will after a pH sensor 9 carries out pH comparison The material input double conic rotary vacuum dryer 4 of the first horizontal screw centrifuge 3 is vacuum dried, After temperature sensor 10 and the first humidity sensor 11 comparison, bipyramid rotary vacuum is done Material input oxidizing reactor 22 in dry machine 4, the 4th controls element 20 controls first and crouches spiral shell Waste water in centrifuge 3 enters sewage disposal system 7;
(2) oxidation: start the 5th control element 21, by double conic rotary vacuum dryer 4 Material input oxidizing reactor 22, control device 23 and the second photoelectric sensing through the second chromatograph Device 24 carries out color comparison and signal output respectively, is inputted by the material in oxidizing reactor 22 Second horizontal screw centrifuge 27 carries out filtration washing, through the 2nd pH sensor 28 and time relay After device 13 is compared respectively, the partial material in the second horizontal screw centrifuge 27 is output as into Product graphene oxide aqueous dispersion liquid, another part material carries out lyophilization;
(3) lyophilization: start the 7th control element 29, by two horizontal screw centrifuges 27 Material input spray dryer 5, through the second humidity sensor 33 carry out humidity ratio to after, Partial material in spray dryer 5 is output as finished product graphene oxide powder, another part thing Material carries out thermal reduction;
(4) thermal reduction: start the 8th control element 30, by the material in spray dryer 5 Input industrial microwave Heating Reduction Furnace for Tungsten 6, enters with vacuum sensor 31 through the second pressure and temp After row pressure and temp and vacuum comparison, it is output as finished product single-layer graphene powder body.

Claims (2)

1. chemical method prepares a single-layer graphene automatic intelligent process units, and its feature exists Console, pre-oxidation still, the first horizontal screw centrifuge, bipyramid rotary is included in agent structure Vacuum drier, spray dryer, industrial microwave Heating Reduction Furnace for Tungsten, sewage disposal system, One chromatograph controls device, the first pH sensor, temperature sensor, the first humidity sensing Device, photoelectric sensor, the time relay, pressure and temp and vacuum sensor, the first electromagnetism Valve, first control element, second control element, the second electromagnetic valve, the 3rd control element, the Four control elements, the 5th control element, oxidizing reactor, second chromatograph control device, second Photoelectric sensor, the second electromagnetic valve, the 6th control element, the second horizontal screw centrifuge, second PH sensor, the 7th control element, the 8th control element, the second pressure and temp and vacuum Sensor, the 9th control element and the second humidity sensor;Console connects the 3rd control unit Part controls raw material input pre-oxidation still and pre-oxidizes, and pre-oxidation still top connects the One chromatograph controls device and carries out color comparison, and the first chromatograph controls device top and connects the first photoelectricity Sensor carries out signal transmission, and the first photoelectric sensor is connected to console and controls the first electromagnetic valve Switch, console and first controls to connect between element have the first electromagnetic valve, the first electromagnetic valve It is delivered to the first horizontal screw centrifuge with the first material controlled in element control pre-oxidation still Carry out filtration washing;First horizontal screw centrifuge top connects a pH sensor and carries out pH value ratio Right, a pH sensor is connected to console and carries out signal transmission, console and bipyramid rotary Being disposed with the second electromagnetic valve and second between vacuum drying oven and control element, second controls unit Part controls the material input bipyramid rotary vacuum drying oven of the first horizontal screw centrifuge output and carries out very Empty dry, the 4th controls element is connected control the first horizontal screw centrifuge output with sewage disposal system Waste water enter sewage disposal system;Bipyramid rotary vacuum drying upper box part connects temperature sensing Device and the first humidity sensor carry out the comparison of temperature and humidity, temperature sensor and respectively One humidity sensor is connected to console and carries out signal transmission, and the 5th controls element controls material Input oxidizing reactor aoxidizes;Oxidizing reactor top connects the second chromatograph control device and enters Row color comparison, the second chromatograph control device top connects the second photoelectric sensor and carries out signal biography Defeated, the second photoelectric sensor is connected to console and controls the second electromagnetic valve switch, and console connects Second the magnetic valve controlled 6th unlatching controlling element, the 6th controls element controls material input oxygen The second horizontal screw centrifuge changing reactor lower end carries out filtration washing;Second horizontal screw centrifuge top Connect the 2nd pH sensor and the time relay carries out pH value comparison respectively and the time controls, the Two pH sensors and the time relay are connected in series to console and carry out signal transmission, the 7th control The partial material input spray dryer that element processed controls in the second horizontal screw centrifuge carries out freezing Being dried, leftover materials are output as finished product graphene oxide aqueous dispersion liquid;Spray dryer top Connecting the second humidity sensor and carry out the humidity ratio pair of material, the 8th controls element controls spraying Partial material input industrial microwave Heating Reduction Furnace for Tungsten in drying machine carries out thermal reduction, is spray-dried Partial material in machine is output as finished product graphene oxide powder;In industrial microwave Heating Reduction Furnace for Tungsten Portion connects the second pressure and temp and carries out pressure and temp and vacuum comparison with vacuum sensor, the Nine control element is connected with industrial microwave Heating Reduction Furnace for Tungsten in control industrial microwave Heating Reduction Furnace for Tungsten Material be output as finished product single-layer graphene powder body.
2. one kind uses automatization's intelligence that device as claimed in claim 1 prepares single-layer graphene Energy production method, it is characterised in that specifically include pre-oxidation, oxidation, lyophilization, thermal reduction Four steps:
(1) pre-oxidation: console starts the 3rd control element and raw material is inputted pre-oxidation Still pre-oxidizes, and treats that raw material reaches expection color and luster, controls device and the first light through the first chromatograph After electric transducer carries out color comparison and signal output respectively, by the material in pre-oxidation still Input the first horizontal screw centrifuge and carry out filtration washing, treat that raw material reaches PH requirement, through a pH The material of the first horizontal screw centrifuge is inputted bipyramid rotary vacuum after carrying out pH comparison and does by sensor Dry machine is vacuum dried, and treats that raw material reaches humidity requirement, dry through temperature sensor and first After humidity sensor comparison, the material in double conic rotary vacuum dryer is inputted oxidation reaction Still, the 4th controls the waste water entrance sewage disposal system that element controls in the first horizontal screw centrifuge;
(2) oxidation: start the 5th control element, by the thing in double conic rotary vacuum dryer Material input oxidizing reactor, treats that raw material reaches to expect color and luster, controls device and the through the second chromatograph Two photoelectric sensors carry out color comparison and signal output respectively, by the material in oxidizing reactor Input the second horizontal screw centrifuge and carry out filtration washing, treat that raw material reaches PH requirement, through the 2nd pH After sensor and the time relay are compared respectively, by the part thing in the second horizontal screw centrifuge Material is output as finished product graphene oxide aqueous dispersion liquid, and another part material carries out lyophilization;
(3) lyophilization: start the 7th control element, by the material in two horizontal screw centrifuges Input spray dryer, treats that raw material reaches humidity requirement, carries out through the second humidity sensor Humidity ratio is to rear, and the partial material in spray dryer is output as finished product graphene oxide powder, Another part material carries out thermal reduction;
(4) thermal reduction: start the 8th control element, the material in spray dryer is inputted Industrial microwave Heating Reduction Furnace for Tungsten, treats that raw material produces a desired effect, through the second pressure and temp and vacuum After degree sensor carries out pressure and temp and vacuum comparison, it is output as finished product single-layer graphene powder Body.
CN201510391663.5A 2015-07-06 2015-07-06 A kind of chemical method prepares single-layer graphene automatic intelligent process units Active CN104925802B (en)

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CN103880002A (en) * 2014-04-04 2014-06-25 厦门凯纳石墨烯技术有限公司 Industrial device for continuously producing graphene powder and method thereof

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US8147791B2 (en) * 2009-03-20 2012-04-03 Northrop Grumman Systems Corporation Reduction of graphene oxide to graphene in high boiling point solvents

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CN102275908A (en) * 2011-07-07 2011-12-14 中南大学 Preparation method of graphene material
CN103880002A (en) * 2014-04-04 2014-06-25 厦门凯纳石墨烯技术有限公司 Industrial device for continuously producing graphene powder and method thereof

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