CN114307912B - Graphene oxide reduction equipment - Google Patents

Graphene oxide reduction equipment Download PDF

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Publication number
CN114307912B
CN114307912B CN202111634507.9A CN202111634507A CN114307912B CN 114307912 B CN114307912 B CN 114307912B CN 202111634507 A CN202111634507 A CN 202111634507A CN 114307912 B CN114307912 B CN 114307912B
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reaction tank
bushing
communicated
powder feeding
air outlet
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CN114307912A (en
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郑少波
杨胤
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention discloses graphene oxide reduction equipment, which belongs to the field of graphene preparation equipment and comprises a reaction tank, a microwave emitter and two electrode plates, wherein the lower end of the reaction tank is in a horn line closing-in shape, the closing-in opening at the lower end of the reaction tank forms a discharge opening of the reaction tank, a valve is arranged at the discharge opening of the reaction tank, a tubular cylindrical bushing is vertically arranged in the reaction tank, the upper end of the bushing is connected with the inner top wall of the reaction tank, an annular gap with an open lower end is arranged between the bushing and the inner wall of the reaction tank, an air outlet communicated with the annular gap is arranged at the upper end of the side wall of the reaction tank, a feed inlet communicated with the inside of the bushing is arranged at the upper end of the reaction tank, the microwave emitter is arranged on the side wall of the reaction tank, the emitting end of the microwave emitter hermetically extends into the bushing, and the two electrode plates are both installed on the inner wall of the bushing in an insulating manner.

Description

Graphene oxide reduction equipment
Technical Field
The invention belongs to the field of graphene preparation equipment, and particularly relates to graphene oxide reduction equipment.
Background
In recent years, many researchers have been dedicated to exploring the large-scale preparation method of graphene so that the physicochemical properties and other possible applications of the novel carbon material can be systematically studied. The preparation method of graphene is divided into a physical method and a chemical method, and mainly comprises a mechanical stripping method, an epitaxial growth method, a chemical vapor deposition method, a carbon nanotube cutting method and a graphite reduction oxidation method. The preparation methods have advantages and disadvantages, and the biggest problem is how to obtain the graphene with uniform structure (including the number of layers and size) and controllable oxygen-containing functional groups.
The graphene oxide reduction method is considered to be the most likely method for industrially producing graphene, the chemical reduction method is mainly adopted for reducing the graphene oxide, and commonly used reagents are reducing agents such as hydrazines and strongly basic substances (most of the reducing agents have certain toxicity, and the environment is polluted due to improper waste liquid treatment), but the production cost is high, and the method is not friendly to the environment.
Disclosure of Invention
The present invention aims to solve the above technical problems, and provides a graphene oxide reduction apparatus capable of reducing graphene oxide.
The technical scheme of the invention is as follows: the utility model provides a graphite oxide reduction equipment, includes retort, microwave emitter, connects hopper, air current to send whitewashed mechanism, dust recovery mechanism and two plate electrodes, the lower extreme of retort is the horn wire binding off, just the binding off department of retort lower extreme constitutes the discharge gate of retort, the discharge gate department of retort is equipped with the valve, and with connect the material mouthful connection of hopper, still vertically be equipped with the bush of a tub cylindricality in the retort, the upper end of bush with the interior roof of retort is connected, the bush with the open annular gap of lower extreme has between the retort inner wall, the upper end of retort lateral wall be equipped with the gas outlet of intercommunication in the annular gap, the upper end of retort be equipped with the feed inlet of intercommunication in the bush, microwave emitter installs on the lateral wall of retort, and its transmitting terminal is sealed stretch into in the bush, two the plate electrode is all insulation installation on the inner wall of bush, and relative distribution on the inner wall of bush, two the positive negative pole electricity that is used for being connected with DC power supply, the discharge gate of air current send whitewashed mechanism with the feed inlet intercommunication of retort, the feed inlet with the dust recovery mechanism with the feed inlet of retort communicates with the dust recovery mechanism.
The microwave emitters are arranged in plurality and uniformly distributed on the side wall of the reaction tank.
The top wall of the reaction tank is also provided with a manhole and an observation hole which are communicated with the inside of the lining, and the manhole is provided with a cover plate.
The gas flow powder feeding mechanism comprises a gas supply device and an even adjustable powder feeding device, the even adjustable powder feeding device is provided with a gas inlet, a discharge port and a powder inlet, a gas outlet of the gas supply device is communicated with the gas inlet of the even adjustable powder feeding device, the discharge port of the even adjustable powder feeding device is communicated with a feed port of the reaction tank, a valve is arranged at the powder inlet, and the gas supply device supplies mixed gas of hydrogen and argon to the even adjustable powder feeding device.
The dust recovery mechanism comprises a bag-type dust collector, the bag-type dust collector is provided with an air inlet, a dust outlet and an air outlet, and the air inlet of the bag-type dust collector is communicated with the air outlet of the reaction tank.
The dust recovery mechanism further comprises a dust collecting hopper, and a feed inlet of the dust collecting hopper is detachably connected with a dust removing opening of the bag-type dust remover.
The dust recovery mechanism further comprises an electrostatic dust collector, the electrostatic dust collector is provided with an air inlet and an air outlet, the air inlet of the electrostatic dust collector is communicated with the air outlet of the bag-type dust collector, the air outlet of the electrostatic dust collector is communicated with the air inlet of the uniform and adjustable powder feeding device, and the air outlet of the electrostatic dust collector is provided with a check valve used for avoiding gas backflow.
The invention has the beneficial effects that: the graphene oxide powder is subjected to reduction treatment in the environment of hydrogen and argon mixed gas by combining an electric field and microwaves, the graphene oxide powder is environment-friendly, reducing agents such as hydrazine and alkali are not needed, and in addition, dust and tail gas in gas discharged from a gas outlet of a reaction tank can be respectively recovered, so that the production cost is reduced and the production efficiency is improved.
Drawings
Fig. 1 is a structural diagram of a graphene oxide reduction apparatus according to the present invention;
fig. 2 is a schematic diagram of graphene oxide reduction equipment according to the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
As shown in fig. 1 and 2, the present invention provides a graphene oxide reduction apparatus, which includes a reaction tank 1, a microwave emitter 2, a receiving hopper 3, an airflow powder feeding mechanism 4, a dust recovery mechanism 5, and two electrode plates 6, wherein a lower end of the reaction tank 1 is a horn line closing in, a closing in at a lower end of the reaction tank 1 forms a discharge port of the reaction tank 1, a discharge port of the reaction tank 1 is provided with a first valve 101 and is connected with the receiving port of the receiving hopper 3, the reaction tank 1 is further internally and vertically provided with a tubular column-shaped bushing 102, an upper end of the bushing 102 is connected with an inner top wall of the reaction tank 1, an annular gap with an open lower end is formed between the bushing 102 and an inner wall of the reaction tank 1, an upper end of a side wall of the reaction tank 1 is provided with an air outlet communicated with the annular gap, an upper end of the side wall of the reaction tank 1 is provided with a feed inlet communicated with the bushing 102, the microwave emitter 2 is installed on the side wall of the reaction tank 1, an emission end of the bushing 102 is hermetically extended into the bushing 102, the two electrode plates 6 are installed on the inner wall of the bushing 102 in an insulating manner, the inner wall of the bushing is electrically connected with the feed inlet of the reaction tank 1, the two electrode plates, the inlet of the airflow powder feeding mechanism is electrically connected with the discharge port of the reaction tank 1, and the dust recovery mechanism, and the exhaust port of the reaction tank 1, and the dust recovery mechanism, and the anode and the exhaust port of the reaction tank 1 are electrically connected with the exhaust port of the reaction tank 1.
Wherein, the microwave emitter 2 is provided with a plurality of (can be 5-10), and a plurality of microwave emitters 2 are evenly distributed on the lateral wall of the reaction tank 1.
Wherein, the top wall of retort 1 still be equipped with manhole 103 and observation hole 104 of the interior intercommunication of bush 102 (observation hole department seal installation has glass), just manhole 103 department seal installation has the apron.
Wherein, the airflow powder feeding mechanism 4 comprises an air supply device 401 and an even adjustable powder feeding device 402, the even adjustable powder feeding device 402 is provided with an air inlet, a discharge port and a powder inlet, the air outlet of the air supply device 401 is communicated with the air inlet of the even adjustable powder feeding device 402, the discharge port of the even adjustable powder feeding device 402 is communicated with the feed inlet of the reaction tank 1, the powder inlet of the even adjustable powder feeding device 402 is provided with a valve II 403, the air supply device 401 supplies mixed gas of hydrogen and argon into the even adjustable powder feeding device 402, the air supply device comprises two gas storage bottles, one of the two gas storage bottles contains argon, the other gas storage bottle contains hydrogen, the air outlets of the two gas storage bottles are communicated with the air inlet of the even adjustable powder feeding device, wherein, argon gas and hydrogen gas are mixed and enter the uniform and adjustable powder feeding device to blow graphene oxide powder in the uniform and adjustable powder feeding device into the reaction tank, argon gas serves as protective gas in the reaction tank, hydrogen serves as reducing gas in the reaction tank, the graphene oxide powder is subjected to reduction reaction with the hydrogen in the reaction tank under the action of an electric field and microwaves to produce graphene, the graphene powder is discharged into the receiving hopper, the first valve is closed after the graphene in the receiving hopper is filled, the receiving hopper is disassembled, the receiving hopper is installed at the discharge port of the reaction tank again after the graphene in the receiving hopper is discharged, the first valve is opened, and residual gas in the reaction tank enters the dust recovery mechanism, wherein the structure of the uniform and adjustable powder feeding device 402 is similar to that of equipment disclosed in CN102114972B, a uniform and adjustable powder feeding device. The graphene oxide and hydrogen react to produce graphene and water, and the water is mixed in the graphene in a moisture mode and is discharged along with the graphene.
The dust recovery mechanism 5 comprises a bag-type dust collector 501, the bag-type dust collector 501 is provided with an air inlet, a dust outlet and an air outlet, and the air inlet of the bag-type dust collector 501 is communicated with the air outlet of the reaction tank 1.
The dust recycling mechanism 5 further comprises a dust collecting hopper 502, and a feed inlet of the dust collecting hopper 502 is detachably connected with a dust removing opening of the bag-type dust remover 501.
The dust recovery mechanism 5 further comprises an electrostatic dust collector 503, the electrostatic dust collector 503 is provided with an air inlet and an air outlet, the air inlet of the electrostatic dust collector 503 is communicated with the air outlet of the bag-type dust collector 501, the air outlet of the electrostatic dust collector 501 is communicated with the air inlet of the uniform and adjustable powder feeding device 402, and the air outlet of the electrostatic dust collector 501 is provided with a check valve 504 for avoiding gas backflow.
An air pump 404 may be additionally disposed at an air inlet of the uniformly adjustable powder feeding device 402, an air outlet of the air pump is communicated with the air inlet of the uniformly adjustable powder feeding device 402, air outlets of the two air storage bottles are communicated with the air inlet of the air pump, and an air outlet of the electrostatic precipitator 501 is communicated with the air inlet of the air pump 404 (i.e., is communicated with the air inlet of the uniformly adjustable powder feeding device 402 through the air inlet pump).
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, particular embodiments, but rather to those skilled in the art, and it is to be understood that the invention is capable of numerous modifications and that various changes may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.

Claims (3)

1. The graphene oxide reduction equipment is characterized by comprising a reaction tank, a microwave emitter, a receiving hopper, an airflow powder feeding mechanism, a dust recovery mechanism and two electrode plates, wherein the lower end of the reaction tank is in a horn line closing-up shape, a closing-up opening at the lower end of the reaction tank forms a discharge opening of the reaction tank, a valve is arranged at the discharge opening of the reaction tank and is connected with a receiving opening of the receiving hopper, a tubular column-shaped bushing is vertically arranged in the reaction tank, the upper end of the bushing is connected with the inner top wall of the reaction tank, an annular gap with an open lower end is arranged between the bushing and the inner wall of the reaction tank, an air outlet communicated with the annular gap is arranged at the upper end of the side wall of the reaction tank, a feed inlet communicated with the inside of the bushing is arranged at the upper end of the reaction tank, the microwave emitter is arranged on the side wall of the reaction tank, an emitting end of the microwave emitter is hermetically extended into the bushing, the two electrode plates are both insulated and arranged on the inner wall of the bushing and are oppositely distributed on the inner wall of the bushing, the two electrode plates are used for being electrically connected with a positive electrode and a negative electrode of a direct current power supply, a discharge opening of the airflow powder feeding mechanism is communicated with the air outlet of the reaction tank; the gas flow powder feeding mechanism comprises a gas supply device and an even and adjustable powder feeding device, the even and adjustable powder feeding device is provided with a gas inlet, a discharge hole and a powder inlet, a gas outlet of the gas supply device is communicated with the gas inlet of the even and adjustable powder feeding device, the discharge hole of the even and adjustable powder feeding device is communicated with a feed hole of the reaction tank, a valve is arranged at the powder inlet, and the gas supply device supplies mixed gas of hydrogen and argon into the even and adjustable powder feeding device; the dust recovery mechanism comprises a bag-type dust remover, the bag-type dust remover is provided with an air inlet, a dust outlet and an air outlet, and the air inlet of the bag-type dust remover is communicated with the air outlet of the reaction tank; the dust recovery mechanism also comprises a dust receiving hopper, and a feed inlet of the dust receiving hopper is detachably connected with a dust removing port of the bag-type dust remover; the dust recycling mechanism further comprises an electrostatic dust collector, the electrostatic dust collector is provided with an air inlet and an air outlet, the air inlet of the electrostatic dust collector is communicated with the air outlet of the bag-type dust collector, the air outlet of the electrostatic dust collector is communicated with the air inlet of the uniform and adjustable powder feeding device, and a check valve used for avoiding gas backflow is arranged at the air outlet of the electrostatic dust collector.
2. The graphene oxide reduction apparatus according to claim 1, wherein the microwave emitters are provided in plurality, and the plurality of microwave emitters are uniformly distributed on a side wall of the reaction tank.
3. The graphene oxide reduction apparatus according to claim 1 or 2, wherein the top wall of the reaction tank is further provided with a manhole and an observation hole which are communicated with the inside of the lining, and a cover plate is installed at the manhole.
CN202111634507.9A 2021-12-29 2021-12-29 Graphene oxide reduction equipment Active CN114307912B (en)

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Application Number Priority Date Filing Date Title
CN202111634507.9A CN114307912B (en) 2021-12-29 2021-12-29 Graphene oxide reduction equipment

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Application Number Priority Date Filing Date Title
CN202111634507.9A CN114307912B (en) 2021-12-29 2021-12-29 Graphene oxide reduction equipment

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CN114307912B true CN114307912B (en) 2022-11-08

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Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291322B (en) * 2014-11-20 2016-04-20 青岛金墨自动化科技有限公司 A kind of Graphene atmosphere protection continuous reduction furnace
PT109387B (en) * 2016-05-13 2021-12-14 Inst Superior Tecnico PROCESS AND SYSTEM FOR THE SELECTIVE PRODUCTION OF AUTONOMOUS TWO-DIMENSIONAL NANOSTRUCTURES USING PLASMA TECHNOLOGY
CN206705681U (en) * 2017-04-18 2017-12-05 青岛华高墨烯科技股份有限公司 A kind of continous way graphene microwave reduction stove
CN107686108B (en) * 2017-09-20 2020-05-29 天津大学 Method for preparing reduced graphene oxide by dielectric barrier discharge plasma
CN110342496A (en) * 2019-07-01 2019-10-18 上海欣材科技有限公司 A kind of reduction furnace for realizing graphene continuous production

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