CN209974308U - Microwave reduction puffing equipment for continuous preparation of graphene - Google Patents
Microwave reduction puffing equipment for continuous preparation of graphene Download PDFInfo
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- CN209974308U CN209974308U CN201920579841.0U CN201920579841U CN209974308U CN 209974308 U CN209974308 U CN 209974308U CN 201920579841 U CN201920579841 U CN 201920579841U CN 209974308 U CN209974308 U CN 209974308U
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Abstract
The utility model discloses microwave reduction puffing equipment for continuous preparation of graphene, which comprises a feeding system, a puffing furnace and a collecting system which are connected in sequence; the expansion furnace comprises a furnace body, a microwave heating device and at least one furnace tube, wherein the furnace tube is horizontally arranged in the furnace body, the microwave heating device is arranged on the furnace body and used for heating materials in the furnace tube, and the feeding system is communicated with each furnace tube; the collecting system comprises at least two collectors, each collector is communicated with the furnace tube through a collecting tube, and a discharge valve is arranged on each collecting tube. Has the following advantages: 1. microwave heating is adopted, the microwave directly acts on the material, the heating speed is high, and the puffing efficiency is high; 2. at least two parallel collectors are adopted, the collectors are switched by controlling the discharge valve, and the next batch of production is not required to be carried out after the graphene is cooled, so that continuous production operation can be realized; 3. a plurality of furnace tubes are horizontally arranged side by side, so that the efficiency is improved by times.
Description
Technical Field
The utility model relates to a popped production facility technical field of graphite alkene especially relates to a popped equipment of microwave reduction for graphite alkene prepares in succession.
Background
The graphene serving as an ideal two-dimensional crystal material has excellent electrical, mechanical, thermal and optical properties, and has wide application potential in the fields of nano electronic devices, supercomputers, solar cells, photon sensors and the like. The performance of graphene is closely related to the preparation technology of graphene, and optimizing the preparation mode of graphene is the key for obtaining high-quality graphene and promoting the industrialization of graphene. The preparation method of the graphene mainly comprises a physical method and a chemical method, wherein the physical method comprises a mechanical stripping method and an epitaxial growth method, and the chemical method comprises a chemical vapor deposition method and a redox method; in order to realize large-scale industrialization of graphene production, the most widely used preparation process is still an oxidation-thermal reduction method at present, but the traditional electric heating reduction puffing technology has the problems of time consumption for temperature rise and slow temperature reduction rate, and has low heating efficiency and large energy consumption, and the microwave reduction puffing furnace can be started and used immediately, so that the efficiency of heating reduction puffing is greatly improved.
Graphite oxide, as the raw materials of popped preparation graphite alkene, it is common to go up strong acid (concentrated sulfuric acid, concentrated nitric acid) and strong oxidizing agent (potassium permanganate) to carry out the intercalation oxidation treatment to natural graphite, and on the one hand, the graphite of natural output just contains sulphur and other impurity originally, and on the other hand, when oxidation treatment inserted the oxygen-containing group in the lamellar structure of graphite, also inevitable introduced contains sulphur group, consequently, if directly discharge without handling a large amount of tail gas that produces among the popped reduction process, must produce harmful effects to operating personnel health and environment.
The existing puffing reduction furnaces adopt an intermittent batch type production mode, and cannot realize continuous production. After single feeding and puffing, an air inlet is opened for blowing after a puffed product is cooled, and the puffed product is collected at a collector and then fed next time.
The single feeding of the existing large-scale puffing reduction furnace is not more than 10g at most, the production efficiency is low, and the large-scale industrial production of graphene is not facilitated, so that the production efficiency and the productivity are improved, and the problem to be solved by technical personnel in the field is urgently needed.
In the existing continuous graphene puffing reduction furnace, gases are directly introduced into a furnace tube without being preheated, on one hand, the temperature in the furnace tube is rapidly reduced due to low-temperature gases, particularly when the flow of the introduced gases is large, the temperature reduction amplitude in the furnace tube even can reach 20-50 ℃, the process temperature deviating from the graphene reduction puffing process is large, and the continuous and stable production of graphene is not facilitated; on the other hand, after the low-temperature gas is introduced into the furnace tube, the furnace tube is rapidly cooled, so that cracking is easily caused, and the service life of the furnace tube is greatly shortened.
SUMMERY OF THE UTILITY MODEL
To the problem, an object of the utility model is to provide a can realize continuous feed and the ejection of compact, possess the microwave reduction equipment that is used for graphite alkene continuous preparation that production efficiency is high.
The utility model adopts the technical proposal that: a microwave reduction puffing device for continuous preparation of graphene comprises a feeding system, a puffing furnace and a collecting system which are sequentially connected;
the expansion furnace comprises a furnace body, a microwave heating device and at least one furnace tube, wherein the furnace tube is horizontally arranged in the furnace body, the microwave heating device is arranged on the furnace body and used for heating materials in the furnace tube, and the feeding system is communicated with each furnace tube;
the collecting system comprises at least two collectors, each collector is communicated with the furnace tube through a collecting tube, and a discharge valve is arranged on each collecting tube.
Further optimization, the exterior of the furnace tube is coated with a wave-absorbing ceramic auxiliary heating plate.
Further optimizing, the ceramic auxiliary heating plate is a SiC auxiliary heating plate.
Further optimization, a heat insulation material layer is further arranged in the furnace body, and the furnace tube and the ceramic auxiliary heating plate are both embedded in the heat insulation material layer.
Further optimize, each all be equipped with the air inlet with the gas-supply pipe intercommunication on the boiler tube, each all be equipped with the admission valve on the gas-supply pipe.
Further optimizing, still include gaseous preheating device, the gas-supply pipe links to each other with gaseous preheating device.
Further optimize, charge-in system is including the hopper, the feeder that communicate in proper order and the inlet pipe that corresponds with boiler tube quantity, every the boiler tube is through the inlet pipe and the feeder intercommunication that correspond, each all be equipped with feeding control mechanism on the inlet pipe.
Further optimize, feeding control mechanism includes first feed valve and second feed valve, the spaced setting is on the inlet pipe about first feed valve and the second feed valve, enclose synthetic storage between first feed valve, second feed valve and the inlet pipe, be equipped with the intake pipe on the storage chamber, be equipped with the second admission valve in the intake pipe.
Further optimize, still include automatic packaging system, automatic packaging system includes automatic packing machine and conveying pipeline, each the material in the collector is sent into in the automatic packing machine through the conveying pipeline that corresponds.
Further optimizing, still include the tail gas processing system, the tail gas processing system includes tail gas processing apparatus and tail gas pipe, and each collector holds the intracavity and is equipped with in the filter screen of solid-gas separation, the filter screen divides into gas room and solid room in holding the chamber of collector, tail gas processing apparatus passes through tail gas and gas room intercommunication.
Further optimizing, the bottom of each collector all is equipped with the multiunit walking wheel.
Further optimizing, the furnace body is covered with a furnace body shield.
The utility model has the advantages that: the utility model discloses during material in the hopper passes through charge-in system, sends the material to each boiler tube, accomplishes popped operation back in the boiler tube, opens a bleeder valve for the material cools off in getting into a collector, treats a collector and fills with the back, switches and opens another bleeder valve, continues to collect graphite alkene with another collector. The utility model discloses mainly have following advantage:
1. microwave heating is adopted, and the microwave directly penetrates through the furnace body and the tube wall of the furnace tube and then directly acts on the material, so that the heating speed is high, and the puffing efficiency is high;
2. at least two parallel collectors are adopted, the collectors are switched by controlling the discharge valve, when one of the collectors is fully filled with the product and is cooled, the other collector is switched to be cooled and collected, and the next batch of production is not required to be carried out after the graphene is cooled, so that continuous production operation can be realized;
3. a plurality of furnace tubes can be horizontally arranged side by side in the furnace body, and compared with the traditional mode of operating a single furnace tube, the efficiency is improved by times; meanwhile, feeding can be flexible by controlling the feeding control mechanism.
Drawings
The present invention will be further described with reference to the accompanying drawings and embodiments.
Fig. 1 is a schematic front view of the microwave reduction puffing apparatus for continuous graphene preparation according to the present invention;
fig. 2 is a schematic plan view of the microwave reduction puffing equipment for continuous preparation of graphene according to the present invention;
FIG. 3 is a schematic structural view of a plurality of furnace tubes arranged in parallel in a furnace body;
fig. 4 is a schematic structural view of the feed control mechanism.
Detailed Description
The microwave reduction puffing equipment for the continuous preparation of the graphene as shown in fig. 1 and fig. 2 comprises a feeding system, a puffing furnace and a collecting system which are connected in sequence;
the expansion furnace comprises a furnace body 110, a microwave heating device 120 and at least one furnace tube 130, wherein the furnace tube 130 is horizontally arranged in the furnace body 110, the microwave heating device 120 is arranged on the furnace body 110 and used for heating materials in the furnace tube 130, and a feeding system is communicated with each furnace tube 130;
the collecting system comprises at least two collectors 310, each collector 310 is respectively communicated with the furnace tube 130 through a collecting tube 320, and a discharge valve 330 is arranged on each collecting tube 320.
As shown in fig. 3, three furnace tubes 130 are horizontally arranged in parallel in the furnace body 110. Through setting up a plurality of boiler tubes 130, for the structure of single boiler tube 130, the production efficiency of graphite alkene has been improved manyfold.
The microwave emitted from the microwave heating device 120 penetrates through the furnace body 110 and the furnace tube 130 and then directly acts on the material in the furnace tube 130. After the material absorbs the microwaves, the temperature is rapidly raised, so that rapid puffing is realized.
After the graphene is puffed, one of the discharge valves 330 is opened, and the graphene passes through the collector 310 and then enters the collecting pipe 320 to be collected. After the collector 310 is full, another discharge valve 330 is switched to open, and another discharge valve 310 is used for collection, so that the problem that next batch of graphene production can be carried out after the graphene in the collector 310 is cooled down is avoided, continuous production of the graphene is realized, and the production efficiency is improved.
The exterior of the furnace tube 130 is coated with a wave-absorbing ceramic sub-hotplate 410. The ceramic auxiliary hot plate 410 can absorb the microwave emitted by the microwave heating device 120, and the temperature of the ceramic auxiliary hot plate 410 is increased after the microwave is absorbed, so as to heat the furnace tube 130. By arranging the ceramic auxiliary heating plate 410, the ceramic auxiliary heating plate 410 absorbs the microwaves and then heats the furnace tube 130, so that the temperature field in the furnace tube 130 is uniform and stable, and the material is fully expanded.
The ceramic secondary thermal plate 410 is preferably a SiC secondary thermal plate. The SiC auxiliary heating plate can be heated after strongly absorbing microwaves in a microwave field, and the temperature rise speed is high. Meanwhile, the temperature can be kept in a relatively stable temperature range, and the phenomenon of thermal runaway is avoided. Therefore, the furnace tube 130 is kept in a relatively stable heating range, and the condition of large temperature fluctuation is avoided. The temperature range of the SiC auxiliary heating plate can be adjusted by adjusting the content of SiC or the frequency of microwave.
The furnace body 110 is further provided with a heat insulation material layer 420, and the furnace tube 130 and the ceramic auxiliary heating plate 410 are both embedded in the heat insulation material layer 420. By embedding the furnace tube 130 and the SiC auxiliary heat plate in the thermal insulation material layer 400, the dissipation of heat is reduced, the energy loss is reduced, and the temperature in the furnace tube 130 is maintained stable.
Each furnace tube 130 is provided with an air inlet communicated with the air pipe 520, and each air pipe 520 is provided with an air inlet valve 530. Each furnace tube 130 is communicated with the protective atmosphere storage device 510 through a corresponding gas pipe 520, and each gas pipe 520 is provided with an air inlet valve 530. By introducing high purity nitrogen gas, or other protective gases such as inert gases, into the furnace tube 130. And graphene is protected from being oxidized in the production process.
Further, a gas preheating device 540 is also included, and the gas conveying pipe 520 is connected with the gas preheating device 540. The protective atmosphere is preheated to the process temperature by the preheating device 540 before entering the furnace tube 130, and then enters the furnace tube 130.
By preheating the protective atmosphere in advance, the temperature in the furnace tube 130 is prevented from being rapidly reduced after cold gas enters the furnace tube 130, and continuous and stable production of graphene is ensured; meanwhile, cracking of the furnace tube 130 due to rapid temperature drop is avoided, and the service life of the furnace tube 130 is greatly prolonged.
The feeding system comprises a hopper 210, a feeder 220 and feeding pipes 230 with the number corresponding to that of the furnace pipes 130, wherein each furnace pipe 130 is communicated with the feeder 220 through the corresponding feeding pipe 230, and each feeding pipe 230 is provided with a feeding control mechanism 240.
After the material in the hopper 210 passes through the feeder 220 and the feeding tube 230 in sequence, the corresponding feeding control mechanism 240 is opened, and the material is fed into the corresponding furnace tube 130. The corresponding feeding control mechanism 240 is controlled, so that the corresponding furnace tube 130 can be flexibly fed. Correspondingly, a general control mechanism 240 can be provided to feed all the furnace tubes 130 at one time.
As shown in fig. 4, the feeding control mechanism 240 includes a first feeding valve 241 and a second feeding valve 242, the first feeding valve 241 and the second feeding valve 242 are disposed on the feeding pipe 230 at intervals up and down, an accumulator 243 is enclosed among the first feeding valve 241, the second feeding valve 242 and the feeding pipe 230, the accumulator 243 is communicated with the protective atmosphere storage device through a feeding pipe 251, and a second feeding valve 253 is disposed on the feeding pipe 251.
In the feeding process, the first feeding valve 241 and the second feeding valve 242 are not opened at the same time, the first feeding valve 241 is opened first, so that the material enters the storage chamber 243, the second air inlet valve 253 is opened, the protective atmosphere is introduced, the air in the storage chamber 243 is discharged, and then the first feeding valve 241 is closed. Subsequent opening of the second feed valve 242 allows the material to enter the furnace tube 130 under the influence of gravity and blowing air, thereby preventing air from entering the furnace tube 130 along with the feed tube 230. Meanwhile, under the action of blowing, the material in the storage chamber 243 can rapidly enter the furnace tube 130, so as to achieve rapid feeding.
The automatic packaging machine further comprises an automatic packaging system, wherein the automatic packaging system comprises an automatic packaging machine 610 and a conveying pipe 620, and materials in each collector 310 are conveyed into the automatic packaging machine 610 through the corresponding conveying pipe 620.
After the graphene in the collector 310 is cooled, the graphite in the collector 310 is sent to an automatic packing machine 610 through a material conveying pipe 620, and automatic packing is completed. Feed conduit 620 is preferably a screw feeder. Other means of delivery, such as belt delivery, may of course be chosen.
In order to remove waste gases such as sulfuration gas generated in the production process, the tail gas treatment system comprises a tail gas treatment device 710 and a tail gas pipe 720, a filter screen 730 for solid-gas separation is arranged in the cavity of each collector 310, the filter screen 730 divides the cavity of the collector 310 into a gas chamber and a solid chamber, and the tail gas treatment device 710 is communicated with the gas chamber through the tail gas pipe 720.
The separation of graphene and gas is realized by the filter screen 730 arranged in the cavity of the collector 310, the relatively heavy graphene is sunk into the bottom of the collector 310 for cooling, and waste gas such as light sulfurated gas enters the tail gas treatment device 710 through the tail gas pipe 720 and is discharged after treatment, so that air pollution is avoided.
To facilitate the transfer of the collectors 310, a plurality of sets of road wheels 311 are provided at the bottom of each collector 310.
A furnace body cover 111 is provided outside the furnace body 110 to protect the furnace body 110.
Of course, the present invention is not limited to the above-mentioned embodiments, and those skilled in the art can make equivalent modifications or substitutions without departing from the spirit of the present invention, and such equivalent modifications or substitutions are included in the scope defined by the claims of the present application.
Claims (10)
1. A microwave reduction puffing equipment for continuous preparation of graphene is characterized in that: comprises a feeding system, a bulking furnace and a collecting system which are connected in sequence;
the expansion furnace comprises a furnace body (110), a microwave heating device (120) and at least one furnace tube (130), wherein the furnace tube (130) is horizontally arranged in the furnace body (110), the microwave heating device (120) is arranged on the furnace body (110) and used for heating materials in the furnace tube (130), and the feeding system is communicated with each furnace tube (130);
the collecting system comprises at least two collectors (310), each collector (310) is communicated with a furnace tube (130) through a collecting tube (320), and a discharge valve (330) is arranged on each collecting tube (320).
2. The microwave reduction puffing equipment for continuous preparation of graphene according to claim 1, wherein: the exterior of the furnace tube (130) is coated with a wave-absorbing ceramic auxiliary heating plate (410).
3. The microwave reduction puffing equipment for continuous preparation of graphene according to claim 2, wherein: the ceramic auxiliary heating plate (410) is a SiC auxiliary heating plate.
4. The microwave reduction puffing equipment for continuous preparation of graphene according to claim 2 or 3, wherein: the furnace body (110) is also internally provided with a heat insulation material layer (420), and the furnace tube (130) and the ceramic auxiliary heating plate (410) are both embedded in the heat insulation material layer (420).
5. The microwave reduction puffing equipment for continuous preparation of graphene according to any one of claims 1 to 3, wherein: each furnace tube (130) is provided with an air inlet communicated with an air conveying pipe (520), and each air conveying pipe (520) is provided with an air inlet valve (530).
6. The microwave reduction puffing equipment for continuous preparation of graphene according to claim 5, wherein: the gas preheating device (540) is further included, and the gas conveying pipe (520) is connected with the gas preheating device (540).
7. The microwave reduction puffing equipment for continuous preparation of graphene according to any one of claims 1 to 3, wherein: the feeding system comprises a hopper (210), a feeder (220) and feeding pipes (230) corresponding to the number of the furnace pipes (130), wherein the hopper (210), the feeder (220) and the feeding pipes (230) are sequentially communicated, each furnace pipe (130) is communicated with the feeder (220) through the corresponding feeding pipe (230), and each feeding pipe (230) is provided with a feeding control mechanism (240).
8. The microwave reduction puffing equipment for continuous preparation of graphene according to claim 7, wherein: the feeding control mechanism (240) comprises a first feeding valve (241) and a second feeding valve (242), the first feeding valve (241) and the second feeding valve (242) are arranged on the feeding pipe (230) at intervals up and down, a storage chamber (243) is enclosed among the first feeding valve (241), the second feeding valve (242) and the feeding pipe (230), an air inlet pipe (251) is arranged on the storage chamber (243), and a second air inlet valve (253) is arranged on the air inlet pipe (251).
9. The microwave reduction puffing equipment for continuous preparation of graphene according to any one of claims 1 to 3, wherein: still include automatic packaging system, automatic packaging system includes automatic packaging machine (610) and conveying pipeline (620), each material in collector (310) is sent into in automatic packaging machine (610) through corresponding conveying pipeline (620).
10. The microwave reduction puffing equipment for continuous preparation of graphene according to any one of claims 1 to 3, wherein: the tail gas treatment system comprises a tail gas treatment device (710) and a tail gas pipe (720), a filter screen (730) for solid-gas separation is arranged in the cavity of each collector (310), the filter screen (730) divides the cavity of the collector (310) into a gas chamber and a solid chamber, and the tail gas treatment device (710) is communicated with the gas chamber through the tail gas pipe (720).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970051A (en) * | 2019-04-25 | 2019-07-05 | 湖南华冶微波科技有限公司 | A kind of microwave reduction bulking equipment continuously prepared for graphene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970051A (en) * | 2019-04-25 | 2019-07-05 | 湖南华冶微波科技有限公司 | A kind of microwave reduction bulking equipment continuously prepared for graphene |
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