CN107253717A - A kind of graphene production system - Google Patents

A kind of graphene production system Download PDF

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Publication number
CN107253717A
CN107253717A CN201710605688.XA CN201710605688A CN107253717A CN 107253717 A CN107253717 A CN 107253717A CN 201710605688 A CN201710605688 A CN 201710605688A CN 107253717 A CN107253717 A CN 107253717A
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CN
China
Prior art keywords
heater
ultrasonic
production system
graphene production
ultrasonic reaction
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Pending
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CN201710605688.XA
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Chinese (zh)
Inventor
李丽萍
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Chenzhou Guosheng New Material Technology Co Ltd
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Chenzhou Guosheng New Material Technology Co Ltd
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Priority to CN201710605688.XA priority Critical patent/CN107253717A/en
Publication of CN107253717A publication Critical patent/CN107253717A/en
Pending legal-status Critical Current

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Abstract

The present invention relates to graphene production field, disclose a kind of graphene production system, the graphene production system includes conserving graphite expanding furnace, twice ultrasonic device and filter, and the conserving graphite expanding furnace is connected with twice ultrasonic device, and the twice ultrasonic device is connected with filter;Using intercalated graphite as raw material, pass sequentially through conserving graphite expanding furnace and obtain expanded graphite, expanded graphite is then finally given into graphene by twice ultrasonic device and filter.The present invention combines puffing furnace and twice ultrasonic device, the expanded graphite of high magnification numbe is prepared by puffing furnace, then carry out prestripping as raw material and ultrasound is peeled off, carry out circular response, charge stripping efficiency can be greatly improved by coordinating twice ultrasonic to peel off, it is achieved thereby that graphene is extensive, high efficiency, the production of low cost.

Description

A kind of graphene production system
Technical field
The present invention relates to graphene production field, more particularly, to a kind of graphene production system.
Background technology
Expanded graphite is to insert the class New type atom, compound on molecular scale that is formed after foreign substance in graphite layers Material, it has also become new developing direction in graphite industry.It had both remained the excellent physicochemical property of graphite, simultaneously because carbon atom Plane and the interaction of insertion material, generate a series of new physicochemical properties, such as high conductivity, superconductivity, catalyst property, Hydrogen storage property etc..Through the similar worm of expanded graphite outward appearance made from high temperature puffing, macroscopic property is stable, with very big ratio Surface area and abundant pore structure, can be used as the sorbing material of the organic pollutions such as oil.The graphite paper that is made up of expanded graphite, Plate, band and various seal members have excellent compressibility, resilience and flexibility, are widely used in oil, chemical industry, smelting The sciemtifec and technical spheres such as gold, aerospace and nuclear reactor.
High temperature puffing method is the conventional method that expanded graphite is prepared by fast heating at high temperature, often using graphite expansion Stove, its principle is can expanded graphite(That is intercalated graphite)Be put into charging aperture, by blower fan can expanded graphite be blown into burner hearth, High temperature puffing is carried out, expanded graphite is blown into discharging opening by the expanded complete blower fan with rear hearth by certain wind speed(Discharging opening The top of charging aperture is arranged on, and with being connected in burner hearth)Place completes to collect, and incomplete expanded graphite is then because weight is more than Expanded graphite and drop and reach separation purpose, but there is problems with the said equipment:1. the non-uniform temperature in body of heater, burner hearth The temperature of inwall is apparently higher than in burner hearth, so that intercalated graphite is heated uneven when causing expanded, reaction efficiency is relatively low;2. reaction Complete expanded graphite later is fewer due to mesh number, is easily got stuck in transportation inside equipment, have impact on yield.3. due to Mainly influenceed in puffing process by puffing time and swelling temperature, intercalated graphite can not be all precisely controlled in existing equipment swollen Change the reaction time in stove and reaction temperature.
Graphene, is a kind of carbon atom by sp2 hydridization bonding in the form of hexagon grid, the two dimension of the carbon formed Planar monolayer structure, is the allotrope of carbon.Graphene is the elementary cell for building other dimension carbon materials, when it is with bag When the mode wrapped up in, wind and piled up changes, the stone of the fullerene, one-dimensional CNT and three-dimensional of zero dimension can be formed respectively Ink.Graphene has good electricity-optics performance, mechanical property, heat-conductive characteristic and high electric charge carrier migration Rate, while also outstanding mechanical strength and pliability.These properties of graphene, allow it to be rapidly become by numerous concerns The focus of research.The graphene and its derivative handled by chemical modification is even more the material with specific function, available for crystalline substance Body pipe, liquid-crystal apparatus, electrochemica biological sensor, ultracapacitor, fuel cell, solar cell etc..Ground past During studying carefully, people generally prepare graphite with mechanical stripping method, chemical vapour deposition technique, epitaxial growth method, oxidation-reduction method etc. Alkene.At present, the preparation of graphene mostly rests on laboratory stage, and its production equipment efficiency is low, it is difficult to meet extensive prepare Requirement, it is too high that this results in graphene production cost.
The content of the invention
The technical problem to be solved in the present invention is in view of the shortcomings of the prior art, offer one kind is low-cost, high-volume to prepare stone The production system of black alkene.
The purpose of the present invention is achieved by the following technical programs:
A kind of graphene production system, including conserving graphite expanding furnace, twice ultrasonic device and filter, the graphite expansion are provided Stove is connected with twice ultrasonic device, and the twice ultrasonic device is connected with filter;
The conserving graphite expanding furnace includes body of heater, feeding device and drawing mechanism, and then raw material is passed through by feeding device to body of heater Drawing mechanism is collected, and the drawing mechanism is located above body of heater, and the feeding device is located at below body of heater;It is provided with the body of heater Heater;The body of heater inner bottom part is additionally provided with above air-flow shower nozzle, the air-flow shower nozzle and is provided with feeding device;
The twice ultrasonic device includes prestripping device and ultrasonic stripping off device, and the prestripping device includes the first batch mixing pond The first circulation system constituted with multiple first ultrasonic reaction kettles, the first cycle system is provided with dog-house and the first discharging Mouthful;The ultrasonic stripping off device includes the second circulation system that the second batch mixing pond and multiple second ultrasonic reaction kettles are constituted, described Second circulation system is provided with charging aperture and the second discharge port.
Preferably, the first circulation system also includes the first reflux line and the first connecting pipe, first backflow Pipeline connects the first ultrasonic reaction kettle and the first batch mixing pond, the first connecting tube connection batch mixing pond and the first discharge port.
Preferably, it is additionally provided with the first drainage conduit between the multiple first ultrasonic reaction kettles and the first connecting pipe.
Preferably, the second circulation system also includes the second reflux line and the second connecting tube, second connecting tube On be sequentially connected charging aperture, the second batch mixing pond, the second ultrasonic reaction kettle, the second return duct and the second discharge port, described second time Flow tube road connects the second batch mixing pond and the second ultrasonic reaction kettle.
Preferably, it is additionally provided with the second drainage conduit between the second ultrasonic reaction kettle and the second connecting pipe
Preferably, the first ultrasonic reaction kettle or/and the second ultrasonic reaction kettle are provided with air bleeding valve.
Preferably, the difference in height of horizontal direction is provided between the first ultrasonic reaction kettle or/and the second ultrasonic reaction kettle.
Preferably, the filter is plate and frame type filter-press.
Preferably, the furnace interior is additionally provided with agitator, the agitator for the spiral agitator that moves up and down or For the centrifugal stirrer of rotary motion.
Preferably, control device is additionally provided with the body of heater, the control device includes processor and controller, the place Reason device is connected with controller, and the controller is connected with air-flow shower nozzle, feeding device and heater respectively.
Compared with prior art, beneficial effects of the present invention:
The present invention adds agitator in body of heater so that the formation convection current of air-flow in body of heater, it is ensured that intercalated graphite it is heated It is even, it is to avoid inboard wall of furnace body it is different with center section temperature so as to cause heated uneven the problem of, be greatly improved reaction Efficiency.
The present invention can prepare expanded graphite on a large scale, reaction temperature of the intelligentized control method intercalated graphite in puffing furnace and Reaction time so that intercalated graphite is fully expanded, its popping fold of the expanded graphite prepared is solved at 200~300 times The problem of traditional puffed stove can not accurately control puffing time and temperature.
Present device is placed using two floors, is heat exchanger tube and connection from the bottom up according to the processing sequence of raw material Pipeline and horizontal line have certain angle, by the cooperation of gravity and wind speed, that is, solve expanded graphite and get stuck problem, improve anti- Yield is answered, while also solving floor space compared to being disposed vertically.
The present invention is by the way that by the setting of ultrasonic reaction kettle, horizontally different height is poor, so as to be followed beneficial to exhaust and material Ring, in the reaction time for setting multiple ultrasonic reaction kettles to extend during circular response, improves reaction efficiency;And it is ultrasonic anti- Answer kettle to be additionally provided with drainage conduit, be conducive to after circular response completion, the quick discharge of ultrasonic reaction kettle realized, so as to quick Lower secondary response is carried out, production efficiency is greatly improved.
The present invention combines puffing furnace and twice ultrasonic device, and the expanded graphite of high magnification numbe is prepared by puffing furnace, Then carry out prestripping as raw material and ultrasound is peeled off, carry out circular response, stripping can be greatly improved by coordinating twice ultrasonic to peel off From efficiency, it is achieved thereby that graphene is extensive, high efficiency, the production of low cost.
Brief description of the drawings
Fig. 1 graphene production system schematic diagrames.
The conserving graphite expanding furnace schematic diagram of Fig. 2 embodiments 1.
Fig. 3 prestripping schematic devices.
Fig. 4 ultrasound stripping off device schematic diagrames.
The conserving graphite expanding furnace schematic diagram of Fig. 5 embodiments 2.
Fig. 6 spiral agitator schematic diagrames.
Fig. 7 centrifugal stirrer schematic diagrames.
Wherein, 1- bodies of heater, 2- feeding devices, 3- drawing mechanisms, 4- air-flow shower nozzles, 5- processors, 6- gas atmosphere inlets, 7- cooling devices, 8- agitators, the first batch mixings of 9- pond, the reflux lines of 10- first, 11- heaters, 12- Vltrasonic devices, 13- First ultrasonic reaction pipeline, the connecting pipes of 14- first, the drainage conduits of 15- first, 16- ball valves, 17- ball valves, 18- ball valves, 19- balls Valve, the discharge ports of 20- first, 21- flowmeters, 22- centrifugal pumps, the second batch mixings of 23- pond, 24- charging apertures, the reflux lines of 25- second, 26- reactors, 27- Vltrasonic devices, the connecting tubes of 28- second, the discharge ports of 29- second, the drainage conduits of 30- second, 31- reserves storehouse, 32- Connecting pipe, 33- cyclone separators, 34- exhaust outlets, 35- subtubes, 36- ball valves, 37- ball valves, 41- sources of the gas, 42- gas flow tubes Road, 43- control dampers, the controllers of 51- the 3rd, 52- second controllers, the controllers of 51- first, 71- heat exchanger tubes, 72- water coolings Pipe, 81- puddlers, 82- mixing parts, 91- centrifugal pumps, 92- flowmeters, 93- ball valves, 94- charging apertures, 95- ball valves, 96- first Batch mixing pond, 101- conserving graphite expanding furnaces, 102- prestripping devices, 103- ultrasound glass devices, 104- filters.
Embodiment
With reference to embodiment, the present invention is further illustrated.Wherein, being given for example only property of accompanying drawing illustrates, What is represented is only schematic diagram, rather than pictorial diagram, it is impossible to be interpreted as the limitation to this patent;In order to which the reality of the present invention is better described Example is applied, some parts of accompanying drawing have omission, zoomed in or out, and do not represent the size of actual product;To those skilled in the art For, some known features and its explanation may be omitted and will be understood by accompanying drawing.
Embodiment 1
As shown in figures 1-4, the present embodiment provides a kind of graphene production system, including conserving graphite expanding furnace 101, twice ultrasonic dress Put and be connected with filter 104, conserving graphite expanding furnace 101 with twice ultrasonic device, twice ultrasonic device connects with filter 104 Connect;
Conserving graphite expanding furnace 101 include body of heater 1, feeding device 2, drawing mechanism 3 and control device, raw material by feeding device 2 to Body of heater 1, is then collected by drawing mechanism 3;Drawing mechanism 3 is located above body of heater, and feeding device 2 is located at below body of heater;Body of heater 1 Interior to be provided with heater 11, the present embodiment uses Resistant heating, and the inner bottom part of body of heater 1 is additionally provided with air-flow shower nozzle 4, air-flow shower nozzle 4 Also include source of the gas 41, airflow line 42 and control damper 43, the connection airflow line 42 of source of the gas 41, the connection air-flow of airflow line 42 Shower nozzle 4, control damper 43 is located in airflow line 42, and the top of air-flow shower nozzle 4 is provided with feeding device 2, specific to be entered using spiral Material machine, control device includes processor 5 and controller, and processor 5 be connected provided with control panel and with control, and controller includes the One controller 53, the controller 51 of second controller 52 and the 3rd, the control damper 43 of the first controller 53 and air-flow shower nozzle 4 connect Connect, second controller 52 is connected with feeding device 2, the 3rd controller 51 is connected with heater 11, protection is additionally provided with body of heater 1 Gas access 6, gas atmosphere inlet 6 is connected 61 with inertia gas cylinder;Cooling device 7 is additionally provided between drawing mechanism 3 and body of heater 1, Cooling device 7 includes heat exchanger tube 71 and water cooling tube 72, and one end connection body of heater 1 of heat exchanger tube 71, the other end connects drawing mechanism 3, Heat exchanger tube 71 and horizontal angle are 45 DEG C~90 DEG C, and water cooling tube 72 is arranged on heat exchanger tube 71 in the shape of a spiral;Drawing mechanism 3 Including multiple reserves storehouses 31 and connecting pipe 32, the one end of connecting pipe 32 is connected with heat exchanger tube 71, and provided with cyclone separator 33, The other end is connected with exhaust outlet 34, and multiple subtubes 35 are additionally provided with connecting pipe 32 and are connected respectively with reserves storehouse 31;Connecting tube Road and 32 horizontal angles are 45 DEG C~90 DEG C;As shown in fig. 6, being additionally provided with agitator 8 in body of heater 1, agitator 8 is spiral Agitator, passes through motor and ball-screw and coordinates so that agitator 8 done in body of heater 1 above and below linear motion, so as to drive stove Airflow reflux in body 1.
Wherein, processor uses microprocessor, and the first controller uses air inlet valve-driving circuit, and second controller, which is used, to be added Expect valve-driving circuit, the 3rd controller uses heat driven circuit.
Twice ultrasonic device includes prestripping device 102 and ultrasonic stripping off device 103, and prestripping device 102 includes first Batch mixing pond 96 and the first circulation system of multiple first ultrasonic reaction kettles composition, the first ultrasonic reaction kettle include the He of Vltrasonic device 12 Reactor 11, the first batch mixing pond 96 is provided with the dog-house 91 being connected with graphite expansion 101, and upper end passes through the first reflux line 10 It is connected with the first ultrasonic reaction kettle, lower end connects the first ultrasonic reaction kettle, first by the first ultrasonic reaction kettle pipeline 13 respectively Connecting pipe 14 is connected with the first discharge port 20, and the first ultrasonic reaction kettle pipeline 13 is provided with centrifugal pump 22 and flowmeter 21, many Individual first ultrasonic reaction kettle arranges connection, wherein the first minimum ultrasonic reaction kettle of horizontal level and the first connecting tube in difference in height Connected between road 14 by the first drainage conduit 15;
Ultrasonic stripping off device 103 includes the second circulation system that the second batch mixing pond 23 and multiple second ultrasonic reaction kettles are constituted, the Two ultrasonic reaction kettles include Vltrasonic device 27 and reactor 26, and the upper end in the second batch mixing pond passes through the second reflux line 25 and second Ultrasonic reaction kettle is connected, and lower end is connected with the second connecting tube 28;Second connecting tube 28 is provided with what is be connected with the first discharge port 20 Charging aperture 94, centrifugal pump 91, flowmeter 92 and the second discharge port 29 being connected with filter 104, the second ultrasonic reaction kettle water Prosposition, which is put, to be sequentially connected, and provided with air bleeding valve, and be connected by the second drainage conduit 30 with the second connecting tube 28;
Filter 104 is plate and frame type filter-press.
The present embodiment operation principle is as follows:
S1. the graphite after intercalation is entered in body of heater 1 as raw material by feed arrangement 2, it is complete in the presence of air-flow shower nozzle 4 Into expanded, and cooling device 7 is blown out to, obtains expanded graphite, then collected by reserves storehouse 31, then transport prestripping dress Put;Expanded time and temperature can be controlled by control panel, specifically processor, which passes through, controls the first controller and second Controller controls air velocity and charging rate, so as to control the intercalated graphite expanded reaction time, and the 3rd controller can be with The temperature of heater 11 is controlled, the intelligentized control method technological parameter of graphite expansion control is realized;
S2. expanded graphite and stripper are added in the first batch mixing pond 96, stirred by motor, then opened ball valve 19, open Centrifugal pump 22 is opened, multiple circular response is carried out, after having reacted, centrifugal pump 22 is closed, ball valve 16, ball valve 18 and ball is opened successively Valve 17, the expanded graphite for completing prestripping enters ultrasonic stripping off device by the first discharge port 20;
S3. the expanded graphite that prestripping is completed in step S2 enters the second connecting tube 28 by charging aperture 94, now opens ball valve 94th, ball valve 36, close ball valve 37, open centrifugal pump 91, carry out multiple circulating ultrasonic glass reaction, graphite is obtained after having reacted Alkene slurry, closes centrifugal pump 91, and ball valve 30, ball valve 37 are opened successively, and now graphene slurry is entered by the second discharge port 29 Plate and frame type filter-press;
S4. the graphene slurry that plate and frame type filter-press is completed to reaction is filtered, and collection obtains product.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, and difference is, agitator 8 is done using centrifugal stirrer in body of heater Rotary motion, as shown in fig. 7, centrifugal stirrer includes puddler 81 and mixing part 82, mixing part 82 is circular or ellipse, many Individual mixing part 82 is that axle center is located on puddler 81 with puddler 81, and the upper and lower ends of puddler 81 are connected by bearing with body of heater, Motor is coordinated to drive.
The agitator 5 of the present embodiment drives air-flow so that intercalated graphite does centrifugal motion by centrifugal motion, it is to avoid Inboard wall of furnace body it is with center section temperature different so as to cause heated uneven the problem of, reaction efficiency is greatly improved.
Obviously, above-described embodiment is only intended to clearly illustrate technical scheme example, and is not Restriction to embodiments of the present invention.For those of ordinary skill in the field, on the basis of the above description also It can make other changes in different forms.Any modification for being made within the spirit and principles of the invention, etc. With replacement and improvement etc., it should be included within the protection of the claims in the present invention.

Claims (10)

1. a kind of graphene production system, it is characterised in that including conserving graphite expanding furnace, twice ultrasonic device and filter, institute State conserving graphite expanding furnace to be connected with twice ultrasonic device, the twice ultrasonic device is connected with filter;
The conserving graphite expanding furnace includes body of heater, feeding device and drawing mechanism, and then raw material is passed through by feeding device to body of heater Drawing mechanism is collected, and the drawing mechanism is located above body of heater, and the feeding device is located at below body of heater;It is provided with the body of heater Heater;The body of heater inner bottom part is additionally provided with above air-flow shower nozzle, the air-flow shower nozzle and is provided with feeding device;
The twice ultrasonic device includes prestripping device and ultrasonic stripping off device, and the prestripping device includes the first batch mixing pond The first circulation system constituted with multiple first ultrasonic reaction kettles, the first cycle system is provided with dog-house and the first discharging Mouthful;The ultrasonic stripping off device includes the second circulation system that the second batch mixing pond and multiple second ultrasonic reaction kettles are constituted, described Second circulation system is provided with charging aperture and the second discharge port.
2. graphene production system according to claim 1, it is characterised in that the first circulation system also includes first time Flow tube road and the first connecting pipe, first reflux line connect the first ultrasonic reaction kettle and the first batch mixing pond, described first Connecting tube connects batch mixing pond and the first discharge port.
3. graphene production system according to claim 2, it is characterised in that multiple first ultrasonic reaction kettles and first The first drainage conduit is additionally provided between connecting pipe.
4. graphene production system according to claim 1, it is characterised in that the second circulation system also includes second time Be sequentially connected in flow tube road and the second connecting tube, second connecting tube charging aperture, the second batch mixing pond, the second ultrasonic reaction kettle, Second return duct and the second discharge port, second reflux line connect the second batch mixing pond and the second ultrasonic reaction kettle.
5. graphene production system according to claim 4, it is characterised in that the second ultrasonic reaction kettle is connected with second The second drainage conduit is additionally provided between pipeline.
6. the graphene production system according to Claims 1 to 5 any one, it is characterised in that first ultrasonic reaction Kettle or/and the second ultrasonic reaction kettle are provided with air bleeding valve.
7. the graphene production system according to Claims 1 to 5 any one, it is characterised in that first ultrasonic reaction The difference in height of horizontal direction is provided between kettle or/and the second ultrasonic reaction kettle.
8. graphene production system according to claim 1, it is characterised in that the filter is plate and frame type filter-press.
9. graphene production system according to claim 1, it is characterised in that the furnace interior is additionally provided with agitator, institute State agitator be move up and down spiral agitator or be rotary motion centrifugal stirrer.
10. graphene production system according to claim 1, it is characterised in that control device, institute are additionally provided with the body of heater Control device is stated including processor and controller, the processor is connected with controller, the controller respectively with air-flow shower nozzle, Feeding device and heater connection.
CN201710605688.XA 2017-07-24 2017-07-24 A kind of graphene production system Pending CN107253717A (en)

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