CN104925802A - Automatic intelligent production device for preparing single-layer graphene by chemical method - Google Patents
Automatic intelligent production device for preparing single-layer graphene by chemical method Download PDFInfo
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Abstract
The invention belongs to the technical field of equipment for preparing single-layer graphene by a chemical method, and relates to an automatic intelligent production device for preparing single-layer graphene by the chemical method. The upper part of a pre-oxidization reaction kettle is connected with a first chromatography control device; the upper part of the first chromatography control device is connected with a first photoelectric sensor; the upper part of a first horizontal screw centrifuge is connected with a first pH sensor; the upper part of a double-tapered rotary vacuum drying tank is connected with a temperature sensor and a first humidity sensor; the upper part of an oxidization reaction kettle is connected with a second chromatography control device; the upper part of the second chromatography control device is connected with a second photoelectric sensor; the upper part of a second horizontal screw centrifuge is connected with a second pH sensor and a time relay; the upper part of a spray dryer is connected with a second humidity sensor; and the upper part of an industrial microwave heating reduction furnace is connected with a second pressure temperature and vacuum degree sensor. The automatic intelligent production device is reasonable in structure, reliable in principle, environmentally-friendly, low in cost and high in degree of automation.
Description
Technical field:
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 production equipment; be applicable to the large-scale production of single-layer graphene; its automatic intelligent system adopts preparation flow unit key element control program; according to chemical preparation single-layer graphene steps flow chart; automatically the connection of unit is completed, until prepare desired product graphene oxide aqueous dispersion liquid, graphene oxide powder and single-layer graphene powder.
Background technology:
Graphene is the novel material of the individual layer sheet structure be made up of carbon atom, known the thinnest in the world, the hardest nano material, there is unusual electroconductibility, thermal conductivity, exceed the intensity of iron and steel decades of times and fabulous light transmission, solar cell can be widely used in, sensor, nanoelectronics, high performance electronics, matrix material, field emmision material, the field such as gas sensor and stored energy, its appearance is expected to cause one at hyundai electronics sciemtifec and technical sphere and takes turns revolution, but, Graphene low yield, high cost, the problem such as of poor quality seriously constrains its development and apply.At present, Graphene is also in research and development, pilot scale, small serial production stage, and it is immature that suitability for industrialized production exists technical matters, does not have the production line of intelligentized control method.Because Graphene suitability for industrialized production requires high to each link of production; a link is had to go wrong; the product produced is exactly waste product; therefore single-layer graphene automatic intelligent production equipment is prepared in the urgent need to designing a kind of chemical method; realize single-layer graphene produce efficient low-consume, reduce costs, energy-conserving and environment-protective; reduce artificial intensity, the large-scale production of favourable promotion Graphene, has good economic benefit and social value.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence; seeking design provides a kind of chemical method to prepare single-layer graphene automatic intelligent production equipment; realize the large-scale production of single-layer graphene, reach the object of efficient low-consume, cost-saving, energy-conserving and environment-protective.
To achieve these goals, agent structure of the present invention comprises console, pre-oxidation still, first horizontal screw centrifuge, DoubletaperedVacuumdrier, spray-drier, industrial microwave Heating Reduction Furnace for Tungsten, Sewage treatment systems, first chromatogram control device, first pH sensor, temperature sensor, first humidity sensor, photo-sensor, the time relay, pressure and temp and vacuum sensor, first magnetic valve, first controlling elements, second controlling elements, second magnetic valve, 3rd controlling elements, 4th controlling elements, 5th controlling elements, oxidizing reactor, second chromatogram control device, second photo-sensor, second magnetic valve, 6th controlling elements, second horizontal screw centrifuge, 2nd pH sensor, 7th controlling elements, 8th controlling elements, second pressure and temp and vacuum sensor, 9th controlling elements and the second humidity sensor, console connects the 3rd controlling elements control raw material input pre-oxidation still and carries out preoxidation, pre-oxidation still top connects the first chromatogram control device and carries out color comparison, first chromatogram control device top connects the first photo-sensor and carries out Signal transmissions, first photo-sensor is connected to the switch that console controls the first magnetic valve, be connected with the first magnetic valve between console and the first controlling elements, mass transport to the first horizontal screw centrifuge that the first magnetic valve and the first controlling elements control in pre-oxidation still carries out filtration washing, first horizontal screw centrifuge top connects a pH sensor and carries out pH value comparison, one pH sensor is connected to console and carries out Signal transmissions, the second magnetic valve and the second controlling elements is disposed with between console and bipyramid rotary vacuum drying oven, the material input bipyramid rotary vacuum drying oven that second controlling elements controls the first horizontal screw centrifuge output carries out vacuum-drying, and the waste water that the 4th controlling elements and Sewage treatment systems connection control first horizontal screw centrifuge export enters Sewage treatment systems, bipyramid rotary vacuum-drying upper box part is connected with the comparison that temperature sensor and the first humidity sensor carry out temperature and humidity respectively, temperature sensor and the first humidity sensor are connected to console and carry out Signal transmissions, and the 5th controlling elements controls material input oxidizing reactor and is oxidized, oxidizing reactor top connects the second chromatogram control device and carries out color comparison, second chromatogram control device top connects the second photo-sensor and carries out Signal transmissions, second photo-sensor is connected to console and controls the second electromagnetic valve switch, console connects the unlatching of the second magnetic valve controlled 6th controlling elements, and the second horizontal screw centrifuge that the 6th controlling elements controls material input oxidizing reactor lower end carries out filtration washing, second horizontal screw centrifuge top connects the 2nd pH sensor and the time relay carries out pH value comparison and time controling respectively, 2nd pH sensor and the time relay are connected in series to console and carry out Signal transmissions, the partial material input spray-drier that 7th controlling elements controls in the second horizontal screw centrifuge carries out lyophilize, and leftover materials export as finished product graphene oxide aqueous dispersion liquid, spray-drier top connects the psychromatic ratio pair that the second humidity sensor carries out material, the partial material input industrial microwave Heating Reduction Furnace for Tungsten that 8th controlling elements controls in spray-drier carries out thermal reduction, and the partial material in spray-drier exports as finished product graphene oxide powder, industrial microwave Heating Reduction Furnace for Tungsten top connects the second pressure and temp and vacuum sensor carries out pressure and temp and vacuum tightness comparison, and the material in the 9th controlling elements and industrial microwave Heating Reduction Furnace for Tungsten connection control industrial microwave Heating Reduction Furnace for Tungsten exports as finished product single-layer graphene powder.
The automatic intelligent production process that the present invention adopts chemical method to prepare single-layer graphene specifically comprises preoxidation, oxidation, lyophilize, thermal reduction four steps:
(1) preoxidation: raw material is inputted pre-oxidation still and carries out preoxidation by console startup the 3rd controlling elements, after the first chromatogram control device and the first photo-sensor carry out color comparison respectively and signal exports, material in pre-oxidation still is inputted the first horizontal screw centrifuge and carries out filtration washing, carry out, after pH comparison, the material of the first horizontal screw centrifuge input DoubletaperedVacuumdrier is carried out vacuum-drying through a pH sensor, after temperature sensor and the first humidity sensor comparison, by the material input oxidizing reactor in DoubletaperedVacuumdrier, the waste water that 4th controlling elements controls in the first horizontal screw centrifuge enters Sewage treatment systems,
(2) be oxidized: start the 5th controlling elements, by the material input oxidizing reactor in DoubletaperedVacuumdrier, color comparison and signal output is carried out respectively through the second chromatogram control device and the second photo-sensor, material in oxidizing reactor is inputted the second horizontal screw centrifuge and carries out filtration washing, after the 2nd pH sensor and the time relay are compared respectively, export the partial material in the second horizontal screw centrifuge for finished product graphene oxide aqueous dispersion liquid, another part material carries out lyophilize;
(3) lyophilize: start the 7th controlling elements, by the material input spray-drier in two horizontal screw centrifuges, through the second humidity sensor carry out psychromatic ratio to after, partial material in spray-drier exports as finished product graphene oxide powder, and another part material carries out thermal reduction;
(4) thermal reduction: start the 8th controlling elements, by the material input industrial microwave Heating Reduction Furnace for Tungsten in spray-drier, carries out after pressure and temp and vacuum tightness comparison through the second pressure and temp and vacuum sensor, exports as finished product single-layer graphene powder.
Working process of the present invention is: raw material is loaded reactor and carry out preoxidation, treat that raw material reaches expection color and luster, through the comparison of chromatogram control device by photo-sensor feedback to console, magnetic valve is opened controlling elements and automatically feedstock transportation is carried out centrifuge washing to horizontal screw centrifuge, treat that raw material reaches PH requirement, by pH value sensor feedback to console, magnetic valve is opened controlling elements and automatically feedstock transportation is carried out drying to DoubletaperedVacuumdrier, another controlling elements unlatching waste liquid is transported to Sewage treatment systems process and treats that raw material reaches humidity requirement, by humidity sensor feedback to console, controlling elements is opened and is automatically oxidized to reactor by feedstock transportation, treat that raw material reaches expection color and luster, through the comparison of chromatogram control device by photo-sensor feedback to console, magnetic valve is opened controlling elements and automatically feedstock transportation is carried out centrifuge washing to horizontal screw centrifuge, treat that raw material reaches PH requirement, console is fed back to by pH sensor, control automatically partial material directly to be exported to make graphene oxide aqueous dispersion liquid by the time relay, partial material is transported to spray-drier and carries out drying, treat that raw material reaches humidity requirement, by humidity sensor feedback to console, controlling elements is opened automatically partial material directly to be exported and is made graphene oxide powder, partial material is transported to microwave reduction stove and reduces, treat that raw material produces a desired effect, pass through pressure, temperature and vacuum sensor feed back to console, controlling elements is opened automatically directly to be exported by material and is made single-layer graphene powder.
The present invention compared with prior art; console is adopted to control each unit operation in preparation process; set up intelligence manufacture apparatus assembly to be coupled and parameter optimization system step by step; realize the preparation of high-quality Graphene mass-producing low cost and the breakthrough of function modulation technique, thus realize the mass-producing preparation of the graphene powder material number of plies and size control, controlled surface modification and functionalization.By single-layer graphene powder and the related products thereof of Graphene intelligence manufacture mode of manufacture, product quality is high, and annual capacity reaches 1000 tons; Prepare on the basis of single-layer graphene at chemical method, automation system adopts preparation flow node key element control program, realizes single-layer graphene automatic production, the automatization of quality control and functional modification, intellectuality by Controlling System, sensor, controller; Production quality control is by sensor, controller control accurate, and success ratio is high, constant product quality, and production process safety meets the requirement of cleaner production and energy-conserving and environment-protective simultaneously.Achieve single-layer graphene produce efficient low-consume, reduce costs, energy-conserving and environment-protective, reduce artificial intensity, be applicable to industrialization produce, improve competitive power, implemented national energy-saving emission reduction tasks index, improved enterprise clean production image, guaranteed its competitive edge; Its apparatus structure is reasonable, and principle is reliable, environmental friendliness.
Accompanying drawing illustrates:
Fig. 1 is agent structure principle schematic of the present invention.
Embodiment:
By embodiment, further description is made to the present invention below in conjunction with accompanying drawing.
Embodiment:
The agent structure of the present embodiment comprises console 1, pre-oxidation still 2, first horizontal screw centrifuge 3, DoubletaperedVacuumdrier 4, spray-drier 5, industrial microwave Heating Reduction Furnace for Tungsten 6, Sewage treatment systems 7, first chromatogram control device 8, first pH sensor 9, temperature sensor 10, first humidity sensor 11, photo-sensor 12, the time relay 13, pressure and temp and vacuum sensor 14, first magnetic valve 15, first controlling elements 16, second controlling elements 17, second magnetic valve 18, 3rd controlling elements 19, 4th controlling elements 20, 5th controlling elements 21, oxidizing reactor 22, second chromatogram control device 23, second photo-sensor 24, second magnetic valve 25, 6th controlling elements 26, second horizontal screw centrifuge 27, 2nd pH sensor 28, 7th controlling elements 29, 8th controlling elements 30, second pressure and temp and vacuum sensor 31, 9th controlling elements 32 and the second humidity sensor 33, console 1 connects the 3rd controlling elements 19 and controls raw material input pre-oxidation still 2 and carry out preoxidation, pre-oxidation still 2 top connects the first chromatogram control device 8 and carries out color comparison, first chromatogram control device 8 top connects the first photo-sensor 12 and carries out Signal transmissions, first photo-sensor 12 is connected to the switch that console 1 controls the first magnetic valve 15, the first magnetic valve 15 is connected with between console 1 and the first controlling elements 16, mass transport to the first horizontal screw centrifuge 3 that first magnetic valve 15 and the first controlling elements 16 control in pre-oxidation still 2 carries out filtration washing, first horizontal screw centrifuge 3 top connects a pH sensor 9 and carries out pH value comparison, one pH sensor 9 is connected to console 1 and carries out Signal transmissions, the second magnetic valve 18 and the second controlling elements 17 is disposed with between console 1 and bipyramid rotary vacuum drying oven 4, the material input bipyramid rotary vacuum drying oven 4 that second controlling elements 17 controls horizontal screw centrifuge 3 output carries out vacuum-drying, and the waste water that the 4th controlling elements 20 and Sewage treatment systems 7 connection control first horizontal screw centrifuge 3 export enters Sewage treatment systems 7, bipyramid rotary vacuum drying oven 4 top is connected with the comparison that temperature sensor 10 and the first humidity sensor 11 carry out temperature and humidity respectively, temperature sensor 10 and the first humidity sensor 11 are connected to console 1 and carry out Signal transmissions, and the 5th controlling elements 21 controls material input oxidizing reactor 22 and is oxidized, oxidizing reactor 22 top connects the second chromatogram control device 23 and carries out color comparison, second chromatogram control device 23 top connects the second photo-sensor 24 and carries out Signal transmissions, second photo-sensor 24 is connected to console 1 and controls the second magnetic valve 25 switch, console 1 connects the unlatching that the second magnetic valve 15 manipulates the 6th controlling elements 26, and the second horizontal screw centrifuge 27 that the 6th controlling elements 26 controls material input oxidizing reactor 22 lower end carries out filtration washing, second horizontal screw centrifuge 27 top connects the 2nd pH sensor 28 and the time relay 13 carries out pH value comparison and time controling respectively, 2nd pH sensor 28 is connected in series to console 1 with the time relay 13 and carries out Signal transmissions, the partial material input spray-drier 5 that 7th controlling elements 29 controls in the second horizontal screw centrifuge 27 carries out lyophilize, and leftover materials export as finished product graphene oxide aqueous dispersion liquid, spray-drier 5 top connects the psychromatic ratio pair that the second humidity sensor 33 carries out material, the partial material input industrial microwave Heating Reduction Furnace for Tungsten 6 that 8th controlling elements 30 controls in spray-drier 5 carries out thermal reduction, and the partial material in spray-drier 5 exports as finished product graphene oxide powder, industrial microwave Heating Reduction Furnace for Tungsten 6 top connects the second pressure and temp and vacuum sensor 31 carries out pressure and temp and vacuum tightness comparison, and the 9th controlling elements 32 and the material in industrial microwave Heating Reduction Furnace for Tungsten 6 connection control industrial microwave Heating Reduction Furnace for Tungsten 6 export as finished product single-layer graphene powder.
The automatic intelligent production process that the present embodiment adopts chemical method to prepare single-layer graphene specifically comprises preoxidation, oxidation, lyophilize, thermal reduction four steps:
(1) preoxidation: console 1 starts the 3rd controlling elements 19 and raw material inputted pre-oxidation still 2 and carry out preoxidation, after the first chromatogram control device 8 and the first photo-sensor 12 carry out color comparison respectively and signal exports, material in pre-oxidation still 2 is inputted the first horizontal screw centrifuge 3 and carry out filtration washing, after a pH sensor 9 carries out pH comparison, the material of the first horizontal screw centrifuge 3 input DoubletaperedVacuumdrier 4 is carried out vacuum-drying, after temperature sensor 10 and the first humidity sensor 11 comparison, by the material input oxidizing reactor 22 in DoubletaperedVacuumdrier 4, the waste water that 4th controlling elements 20 controls in the first horizontal screw centrifuge 3 enters Sewage treatment systems 7,
(2) be oxidized: start the 5th controlling elements 21, by the material input oxidizing reactor 22 in DoubletaperedVacuumdrier 4, color comparison and signal output is carried out respectively through the second chromatogram control device 23 and the second photo-sensor 24, material in oxidizing reactor 22 is inputted the second horizontal screw centrifuge 27 and carry out filtration washing, after the 2nd pH sensor 28 and the time relay 13 are compared respectively, export the partial material in the second horizontal screw centrifuge 27 for finished product graphene oxide aqueous dispersion liquid, another part material carries out lyophilize;
(3) lyophilize: start the 7th controlling elements 29, by the material input spray-drier 5 in two horizontal screw centrifuges 27, through the second humidity sensor 33 carry out psychromatic ratio to after, partial material in spray-drier 5 exports as finished product graphene oxide powder, and another part material carries out thermal reduction;
(4) thermal reduction: start the 8th controlling elements 30, by the material input industrial microwave Heating Reduction Furnace for Tungsten 6 in spray-drier 5, after the second pressure and temp and vacuum sensor 31 carry out pressure and temp and vacuum tightness comparison, export as finished product single-layer graphene powder.
Claims (2)
1. a chemical method prepares single-layer graphene automatic intelligent production equipment, it is characterized in that agent structure comprises console, pre-oxidation still, first horizontal screw centrifuge, DoubletaperedVacuumdrier, spray-drier, industrial microwave Heating Reduction Furnace for Tungsten, Sewage treatment systems, first chromatogram control device, first pH sensor, temperature sensor, first humidity sensor, photo-sensor, the time relay, pressure and temp and vacuum sensor, first magnetic valve, first controlling elements, second controlling elements, second magnetic valve, 3rd controlling elements, 4th controlling elements, 5th controlling elements, oxidizing reactor, second chromatogram control device, second photo-sensor, second magnetic valve, 6th controlling elements, second horizontal screw centrifuge, 2nd pH sensor, 7th controlling elements, 8th controlling elements, second pressure and temp and vacuum sensor, 9th controlling elements and the second humidity sensor, console connects the 3rd controlling elements control raw material input pre-oxidation still and carries out preoxidation, pre-oxidation still top connects the first chromatogram control device and carries out color comparison, first chromatogram control device top connects the first photo-sensor and carries out Signal transmissions, first photo-sensor is connected to the switch that console controls the first magnetic valve, be connected with the first magnetic valve between console and the first controlling elements, mass transport to the first horizontal screw centrifuge that the first magnetic valve and the first controlling elements control in pre-oxidation still carries out filtration washing, first horizontal screw centrifuge top connects a pH sensor and carries out pH value comparison, one pH sensor is connected to console and carries out Signal transmissions, the second magnetic valve and the second controlling elements is disposed with between console and bipyramid rotary vacuum drying oven, the material input bipyramid rotary vacuum drying oven that second controlling elements controls the first horizontal screw centrifuge output carries out vacuum-drying, and the waste water that the 4th controlling elements and Sewage treatment systems connection control first horizontal screw centrifuge export enters Sewage treatment systems, bipyramid rotary vacuum-drying upper box part is connected with the comparison that temperature sensor and the first humidity sensor carry out temperature and humidity respectively, temperature sensor and the first humidity sensor are connected to console and carry out Signal transmissions, and the 5th controlling elements controls material input oxidizing reactor and is oxidized, oxidizing reactor top connects the second chromatogram control device and carries out color comparison, second chromatogram control device top connects the second photo-sensor and carries out Signal transmissions, second photo-sensor is connected to console and controls the second electromagnetic valve switch, console connects the unlatching of the second magnetic valve controlled 6th controlling elements, and the second horizontal screw centrifuge that the 6th controlling elements controls material input oxidizing reactor lower end carries out filtration washing, second horizontal screw centrifuge top connects the 2nd pH sensor and the time relay carries out pH value comparison and time controling respectively, 2nd pH sensor and the time relay are connected in series to console and carry out Signal transmissions, the partial material input spray-drier that 7th controlling elements controls in the second horizontal screw centrifuge carries out lyophilize, and leftover materials export as finished product graphene oxide aqueous dispersion liquid, spray-drier top connects the psychromatic ratio pair that the second humidity sensor carries out material, the partial material input industrial microwave Heating Reduction Furnace for Tungsten that 8th controlling elements controls in spray-drier carries out thermal reduction, and the partial material in spray-drier exports as finished product graphene oxide powder, industrial microwave Heating Reduction Furnace for Tungsten top connects the second pressure and temp and vacuum sensor carries out pressure and temp and vacuum tightness comparison, and the material in the 9th controlling elements and industrial microwave Heating Reduction Furnace for Tungsten connection control industrial microwave Heating Reduction Furnace for Tungsten exports as finished product single-layer graphene powder.
2. adopt device as claimed in claim 1 to prepare an automatic intelligent production method for single-layer graphene, it is characterized in that specifically comprising preoxidation, oxidation, lyophilize, thermal reduction four steps:
(1) preoxidation: raw material is inputted pre-oxidation still and carries out preoxidation by console startup the 3rd controlling elements, after the first chromatogram control device and the first photo-sensor carry out color comparison respectively and signal exports, material in pre-oxidation still is inputted the first horizontal screw centrifuge and carries out filtration washing, carry out, after pH comparison, the material of the first horizontal screw centrifuge input DoubletaperedVacuumdrier is carried out vacuum-drying through a pH sensor, after temperature sensor and the first humidity sensor comparison, by the material input oxidizing reactor in DoubletaperedVacuumdrier, the waste water that 4th controlling elements controls in the first horizontal screw centrifuge enters Sewage treatment systems,
(2) be oxidized: start the 5th controlling elements, by the material input oxidizing reactor in DoubletaperedVacuumdrier, color comparison and signal output is carried out respectively through the second chromatogram control device and the second photo-sensor, material in oxidizing reactor is inputted the second horizontal screw centrifuge and carries out filtration washing, after the 2nd pH sensor and the time relay are compared respectively, export the partial material in the second horizontal screw centrifuge for finished product graphene oxide aqueous dispersion liquid, another part material carries out lyophilize;
(3) lyophilize: start the 7th controlling elements, by the material input spray-drier in two horizontal screw centrifuges, through the second humidity sensor carry out psychromatic ratio to after, partial material in spray-drier exports as finished product graphene oxide powder, and another part material carries out thermal reduction;
(4) thermal reduction: start the 8th controlling elements, by the material input industrial microwave Heating Reduction Furnace for Tungsten in spray-drier, carries out after pressure and temp and vacuum tightness comparison through the second pressure and temp and vacuum sensor, exports as finished product single-layer graphene powder.
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Cited By (1)
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US20130309162A1 (en) * | 2009-03-20 | 2013-11-21 | Northrop Grumman Systems Corporation | Reduction of graphene oxide to graphene in high boiling point solvents |
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