CN219709127U - Device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow - Google Patents
Device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow Download PDFInfo
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- CN219709127U CN219709127U CN202223159919.4U CN202223159919U CN219709127U CN 219709127 U CN219709127 U CN 219709127U CN 202223159919 U CN202223159919 U CN 202223159919U CN 219709127 U CN219709127 U CN 219709127U
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Abstract
The utility model provides a device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow, which comprises an electrolytic tank unit, an electrode unit, an electrolyte slurry flowing unit, an electrolyte slurry caching unit, an electrolyte slurry defoaming unit and an electrolytic tank temperature control unit; the electrolytic tank unit comprises an electrolytic tank body, and an electrolyte inlet pipe and an electrolyte outlet pipe are respectively arranged on the electrolytic tank body; the electrode unit comprises a plurality of cathodes and a plurality of anodes, the cathodes and the anodes are alternately arranged at intervals, and the cathodes and the anodes are arranged between the electrolyte inlet pipe and the electrolyte outlet pipe; an encapsulated electrode diaphragm is paved outside the electrode plate surface of each anode, a gas cavity is formed between the encapsulated electrode diaphragm and the electrode plate of the anode, and an anode exhaust pipe communicated with the gas cavity is arranged at the top of the anode. The device adopts the continuous electrochemical reduction mode of liquid flow to reduce graphene oxide into high-quality reduced graphene, and has high reduction efficiency and good effect.
Description
Technical Field
The utility model relates to the technical field of graphene preparation, in particular to a device for preparing reduced graphene by continuously electrochemically reducing oxidized graphene in a liquid flow mode.
Background
Graphene is formed from a single layer sp 2 Two-dimensional crystal with honeycomb hexagonal plane formed by hybridization of carbon atom array, sp on two-dimensional plane 2 The hybridized carbon atoms are connected with three adjacent carbon atoms through sigma bonds, the rest p electron orbits are perpendicular to the plane of the graphene, and form a large pi bond with surrounding atoms, so that the graphene has good electric conduction, heat conduction and mechanical properties, and the electron mobility is up to 200,000cm 2 /(V.s), conductivity reaches 10 6 S/m, the thermal conductivity can reach 5000W/(m.K), and the strength can reach 130GPa. The excellent characteristics of the graphene lead the graphene to have great potential application prospects in the fields of optoelectronic devices, chemical power sources (such as solar cells and lithium ion batteries), gas sensors, antistatic and heat dissipation materials and the like. The precondition that graphene has the excellent performance is that the graphene has a complete structure and high quality and can be produced in a large scale, however, the current mainstream graphene preparation method has a great challenge to large-scale industrial application.
In the existing graphene preparation technology, the redox method is the mainstream preparation method for industrially producing graphene at present, and is high in yield and easy for large-scale production. However, the method firstly needs to obtain a graphene oxide intermediate product through chemical oxidation, a large number of oxygen-containing groups exist in the graphene oxide structure to form a large number of structural defects, so that the electric conduction and heat conduction properties of graphene are greatly reduced, and a graphene product with higher quality can be obtained through further reduction treatment. The existing reduction method mainly comprises a chemical reduction method and a thermal reduction method, wherein the chemical reduction method involves the use of strong reducing agents (such as hydrazine hydrate, sodium borohydride and potassium borohydride), the thermal reduction method needs to use a high-temperature environment with the temperature of more than 1000 ℃, and the problems of environment unfriendly, high-temperature energy consumption and the like exist, so that the production cost of graphene is high, the large-scale industrial application of the graphene is not facilitated, and meanwhile, the reduction process also brings serious environmental pollution, and the environmental protection and the green production are not facilitated.
In addition, there is also the electrochemical preparation of reduced graphene, but the existing electrochemical preparation method and the device used have the following disadvantages:
1. the electrode in the electrolytic tank is fixed, the electrolyte is in a static state, and graphene oxide in the electrolyte can not fully react with the electrode during electrochemical reaction, so that the defects of insufficient and uneven reaction exist;
2. the traditional disturbance enhancing mode is that the graphene and the electrode can have better contact reaction to a certain extent by stirring the electrolyte, however, the graphene in the electrolyte is easy to contact with the anode in the disturbance process, so that the oxidation reaction of the graphene and oxygen generated by the anode is caused, and the prepared reduced graphene has poor effect and poor quality;
3. when electrolyte is disturbed, oxygen generated by the anode and hydrogen generated by the cathode are easy to mix together, and when mass production is carried out, a large amount of oxygen and hydrogen are easy to mix and explode, so that serious potential safety hazards exist;
4. the graphene in the electrolyte has strong conductivity, and is easy to conduct the anode and the cathode, so that the cathode and the anode are short-circuited, and the electrochemical reduction reaction is influenced.
For the reasons, the graphene obtained by the existing technology for preparing the reduced graphene by the electrochemical reduction method has poor effect, low production efficiency and low yield, and cannot be used for high-efficiency and large-scale industrialized production of high-quality reduced graphene.
Aiming at the defects of the prior art, the utility model provides a device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow, which is used for reducing graphene oxide into high-quality reduced graphene in a liquid flow continuous electrochemical reduction mode, has good reduction efficiency and good effect, and is suitable for mass production of reduced graphene in industry.
Disclosure of Invention
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
the device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow comprises an electrolytic cell unit, an electrode unit and an electrolyte slurry flow unit;
the electrolytic tank unit comprises an electrolytic tank body, and an electrolyte inlet pipe and an electrolyte outlet pipe are respectively arranged on the electrolytic tank body;
the electrode unit comprises a plurality of cathodes and a plurality of anodes, the cathodes and the anodes are alternately arranged at intervals, the cathodes and the anodes are arranged between an electrolyte inlet pipe and an electrolyte outlet pipe, each anode of each cathode is connected with an electrolyte tank power supply bus through an electrode power supply line, the bottoms of each cathode and each anode are tightly connected with a bottom panel of an electrolyte tank body, only one side wall of each cathode is tightly attached to one side wall of the electrolyte tank body, only one side wall of each anode is tightly attached to one side wall of the electrolyte tank body, and only one side wall of each anode is tightly attached to one side wall of the electrolyte tank body; an encapsulated electrode diaphragm is paved outside the electrode plate surface of each anode, a gas cavity is formed between the encapsulated electrode diaphragm and the electrode plate of the anode, and an anode exhaust pipe communicated with the gas cavity is arranged at the top of the anode;
the electrolyte slurry flowing unit comprises a fluid pump, and the discharge end of the fluid pump is communicated with the electrolytic tank body through an electrolyte inlet pipe.
Preferably, the number of cathode arrangements is one more than the number of anode arrangements; all cathodes and all anodes are positioned between an electrolyte inlet pipe and an electrolyte outlet pipe, and the electrolyte inlet pipe is arranged at the upper part of the electrolytic tank body, is close to the top of the electrolytic tank body and is close to one side of the side wall of the electrolytic tank body, which is connected with the cathodes; the electrolyte outlet pipe is arranged at the bottom of the electrolytic tank body and is also close to one side of the side wall of the electrolytic tank body, which is connected with the cathode.
Preferably, the electrode plate of the cathode is in a corrugated shape.
Preferably, the bottom and the side wall of the electrolytic tank body are respectively provided with a fluid circulation spray hole, and all the fluid circulation spray holes are communicated with the discharge end of the fluid pump through pipelines.
Preferably, a sealing cover is arranged at the top of the electrolytic tank body, a cathode exhaust manifold is arranged at the top of the sealing cover, and the cathode exhaust manifold is communicated with the inside of the electrolytic tank body through the sealing cover; the anode exhaust pipes on all anodes extend to the outside of the electrolytic cell body.
Preferably, the fluid pump comprises a feeding pump and a fluid circulating pump, wherein the feeding end of the feeding pump is communicated with the electrolytic tank body through an electrolyte outlet pipe, the discharging end of the feeding pump is communicated with the feeding end of the electrolyte slurry caching unit, the discharging end of the electrolyte slurry caching unit is communicated with the feeding end of the fluid circulating pump, and the discharging end of the fluid circulating pump is communicated with the electrolytic tank body through an electrolyte inlet pipe.
Preferably, the electrolyte slurry buffer unit comprises an electrolyte slurry buffer tank, the electrolyte slurry buffer tank is respectively communicated with the feeding pump and the fluid circulating pump, and a stirrer is further arranged in the electrolyte slurry buffer tank.
Preferably, the electrolyte slurry buffer unit is provided with an electrolyte slurry defoaming unit for defoaming inside the electrolyte slurry buffer unit; the electrolyte slurry defoaming unit comprises a homogenizing pump, an electrolyte defoaming tank, a defoaming negative pressure buffer tank and a negative pressure machine, wherein the liquid inlet end of the homogenizing pump is communicated with the electrolyte slurry buffer unit, the liquid outlet end of the homogenizing pump is communicated with the electrolyte defoaming tank, the electrolyte defoaming tank is also communicated with the electrolyte slurry buffer unit, and the negative pressure machine is communicated with the electrolyte slurry buffer unit through the defoaming negative pressure buffer tank.
Preferably, the electrolyte slurry buffer unit is also connected with an electrolytic tank temperature control unit for regulating the temperature of the electrolyte slurry in the electrolyte slurry buffer unit; the temperature control unit of the electrolytic tank comprises a PLC central controller, a heat exchanger and a first temperature sensor, wherein the PLC central controller is respectively and electrically connected with the heat exchanger and the first temperature sensor, and a heat exchange coil of the heat exchanger and the first temperature sensor are both arranged inside the electrolyte slurry buffer unit.
Preferably, the electrolysis bath temperature control unit further comprises a second temperature sensor and a third temperature sensor, wherein the second temperature sensor and the third temperature sensor are electrically connected with the PLC central controller and are both installed in the electrolysis bath body, the second temperature sensor is close to the part of the electrolysis bath body, where the electrolyte inlet pipe is arranged, and the third temperature sensor is close to the part of the electrolysis bath body, where the electrolyte outlet pipe is arranged.
Preferably, the electrode electron supply line is arranged at the top of the polar plate where the electrode electron supply line is arranged, the electrolytic tank power supply bus is divided into a cathode power supply bus and an anode power supply bus, the cathode power supply bus is arranged on the side wall of the electrolytic tank body, which is connected with the cathode, and is connected with the electrode electron supply line of the cathode, and the anode power supply bus is arranged on the side wall of the electrolytic tank body, which is connected with the anode, and is connected with the electrode electron supply line of the anode.
Compared with the prior art, the utility model has the following beneficial effects:
1. the device is used for continuously electrochemically reducing graphene oxide in liquid flow (liquid mobile phase) to prepare high-quality reduced graphene, the device sends fluid slurry into an electrolytic tank body through a fluid pump, cathodes and anodes in the electrolytic tank body are alternately arranged, S-shaped communication areas are formed in the electrolytic tank body by the fluid pump, the S-shaped communication areas are utilized to continuously disturb the flowing process of the graphene oxide electrolyte slurry along the S-shaped communication areas, and the sufficient contact between the graphene oxide and the cathodes is promoted, so that the graphene oxide is efficiently reduced, and the high-quality reduced graphene is obtained; in addition, when the electrolyte slurry flow unit consists of the feed pump and the circulation circulating pump, the device disclosed by the utility model forms closed circulation of an electrolytic tank, the feed pump, the electrolyte slurry buffer tank, the fluid circulating pump and the electrolytic tank through the electrolytic tank unit, the electrolyte slurry flow unit and the electrolyte slurry buffer unit, and multiple circulation reactions can be carried out according to actual needs in a closed circulation flow mode, so that high-quality reduced graphene meeting the requirements is obtained, and the industrial continuity of mass production of the reduced graphene can be met.
2. The anode is separated by the packaging electrode diaphragm, and oxygen generated by the anode cannot escape and can only be discharged from the arranged anode exhaust pipe, so that oxygen and hydrogen generated by the reaction cannot be mixed together, and the production safety is greatly improved; moreover, the packaging electrode diaphragm only allows ions in the electrolyte to pass through, and graphene in the electrolyte cannot pass through, so that the graphene cannot contact oxygen generated by the anode, and the graphene cannot be oxidized by the oxygen, so that the reduction quality and the reduction efficiency of the graphene are improved; furthermore, as the graphene cannot contact the anode, the situation that the anode and the cathode are conducted and short-circuited does not exist, and the electrochemical reaction can be continuously carried out; therefore, by the arrangement of the anode structure, the electrochemical reduction reaction can be fully and safely carried out.
3. Compared with the existing electrochemical reduction reaction, the method for preparing graphene by continuous electrochemical reduction of liquid flow can enhance the reduction effect of graphene oxide, can obviously improve the reduction productivity, does not need to use harsh production conditions such as high temperature, high vacuum and the like, and has low production requirement, environmental protection, energy conservation and low cost.
Drawings
FIG. 1 is a schematic illustration of the structural use of the present utility model; the seal cap is not shown in the figures;
FIG. 2 is a schematic view of the structure of the cell body.
Description of the main reference signs
In the figure: the electrolytic cell comprises a cell body, a 1-1 electrolyte liquid inlet pipe, a 1-2 electrolyte liquid outlet pipe, a 1-3 electrolytic cell power supply bus, a 1-3-1 power supply bus insulating cushion, a 1-3-2 bus bearing fixed support, a 2 feeding pump, a 3 electrolyte slurry buffer tank, a 3-1 stirrer, a 4 fluid circulating pump, a 5 electrode unit, a 5-1 cathode, a 5-2 anode, a 5-2-1 packaged electrode diaphragm, a 5-2-2 electrode power supply wire, a 6 electrolyte slurry defoaming unit, a 6-1 homogenizing pump, a 6-2 electrolyte defoaming tank, a 6-3 defoaming negative pressure buffer tank, a 6-4 negative pressure machine, a 7 electrolytic cell temperature control unit, a 7-1 central controller, a 7-2 heat exchanger, a 7-3 first temperature sensor, a 7-4 second temperature sensor, a 7-5 third temperature sensor and an 8 pipeline stop valve.
The utility model will be further described in the following detailed description in conjunction with the above-described figures.
Detailed Description
Referring to fig. 1-2, in a preferred embodiment of the present utility model, an apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide in a liquid stream includes an electrolytic cell unit, an electrode unit 5, and an electrolyte slurry flow unit.
The electrolytic tank unit comprises an electrolytic tank body 1, and an electrolyte inlet pipe 1-1 and an electrolyte outlet pipe 1-2 are respectively arranged on the electrolytic tank body 1.
The electrode unit 5 comprises a plurality of cathodes 5-1 and a plurality of anodes 5-2, wherein the cathodes 5-1 and the anodes 5-2 are alternately arranged at intervals, the cathodes 5-1 and the anodes 5-2 are arranged between an electrolyte inlet pipe 1-1 and an electrolyte outlet pipe 1-2, each cathode 5-1 and each anode 5-2 are connected with an electrolyte tank power supply bus 1-3 through an electrode power supply wire 5-2, the bottoms of each cathode 5-1 and each anode 5-2 are tightly connected with an electrolyte tank bottom panel, only one side wall of each cathode 5-1 is tightly attached to one side wall of the electrolyte tank body 1, only one side wall of each anode 5-2 is tightly attached to one side wall of the electrolyte tank body 1, and the side wall of the electrolyte tank body 1 to which the anodes 5-2 are attached is opposite to the side wall of the electrolyte tank body 1 to which the cathodes 5-1 are attached; the outer side of the electrode plate surface of each anode 5-2 is paved with a packaging electrode diaphragm 5-2-1, a gas cavity is formed between the packaging electrode diaphragm 5-2-1 and the electrode plate of the anode 5-2, and the top of the anode 5-2 is provided with an anode exhaust pipe communicated with the gas cavity.
The electrolyte slurry flow unit comprises a fluid pump, and the discharge end of the fluid pump is communicated with the electrolytic tank body 1 through an electrolyte inlet pipe 1-1.
According to the utility model, the slurry to be reacted is sent into the electrolytic tank body 1 through the fluid pump, in the electrolytic tank body 1, as the cathodes 5-1 and the anodes 5-2 of the electrode units 5 are alternately arranged in a staggered way, and the cathodes 5-1 and the anodes 5-2 are respectively attached to one side tank wall of the electrolytic tank body 1 and are spaced from one side tank wall, the fluid circulation channel in the electrolytic tank body 1 is S-shaped, the electrolyte slurry flows along the S-shaped communication area, the graphene oxide in the electrolyte slurry is intermittently contacted with the cathodes 5-1 in the flowing process, and is reduced into reduced graphene after the contact reaction, and as the electrolyte slurry is disturbed in the S-shaped flowing process, the graphene oxide in the electrolyte slurry can be fully contacted with the cathodes 5-1, so that the reduction efficiency is improved.
In the utility model, hydrogen generated by a cathode 5-1 in the process of reducing graphene oxide by electrolyte slurry in an electrolytic tank body 1 is directly discharged, and in order to facilitate centralized collection of hydrogen and avoid overflow of hydrogen, a sealing cover is arranged at the top of the electrolytic tank body 1 in the embodiment, a cathode exhaust main pipe is arranged at the top of the sealing cover, and the cathode exhaust main pipe is communicated with the inside of the electrolytic tank body 1 through the sealing cover; the anode exhaust pipes on all anodes 5-2 extend outside the electrolytic cell body 1. In this way, the hydrogen generated by the reaction of the cathode 5-1 can be uniformly discharged out of the electrolytic tank body 1 through the cathode exhaust manifold at the top of the sealing cover and collected and treated in a concentrated way, preferably, a plurality of cathode exhaust pipes are arranged on the sealing cover, each cathode exhaust pipe is communicated with the cathode exhaust manifold, and the cathode exhaust pipes are arranged right above each cathode 5-1, so that the hydrogen generated on each cathode 5-1 can be discharged out of the electrolytic tank body 1 better. In addition, oxygen generated by the anode 5-2 in the electrolytic tank body 1 flows in a gas cavity formed between the anode 5-2 and the packaging electrode diaphragm 5-2-1 and is discharged out of the gas cavity and the electrolytic tank body 1 through an anode exhaust pipe, preferably, anode exhaust pipes on all the anode 5-2 are communicated with the outside of the electrolytic tank body through an anode exhaust main pipe, namely, oxygen generated by the anode 5-2 is discharged out of the electrolytic tank body 1 through the anode exhaust main pipe after being discharged out of the gas cavity through the anode exhaust pipe, and due to the arrangement of the packaging electrode diaphragm 5-2-1, oxygen generated in the electrochemical reaction process is not discharged out of the gas cavity through the anode exhaust pipe directly, so that the oxygen is not reacted with reduced graphene obtained after reduction in the electrolyte, and the reduction efficiency and the effectiveness of the reduced graphene are improved. In this embodiment, the encapsulated electrode membrane 5-2-1 is one of a filter cloth, a homogeneous ion exchange membrane, an asbestos membrane, a ceramic membrane, a polytetrafluoroethylene membrane, a polyacrylic acid membrane and a polyvinylidene fluoride membrane, and the encapsulated motor membrane has a certain pore structure and is corrosion-resistant.
Preferably, in the present embodiment, for better reduction of graphene oxide, the number of the cathodes 5-1 is one more than the number of the anodes 5-2, that is, the electrode units 5 in the electrolytic cell body 1 form a "cathode-anode-cathode" alternating structure so that graphene oxide sufficiently contacts the cathodes 5-1; all cathodes 5-1 and all anodes 5-2 are positioned between an electrolyte inlet pipe 1-1 and an electrolyte outlet pipe 1-2, wherein the electrolyte inlet pipe 1-1 is arranged at the upper part of an electrolytic tank body 1 and is close to the top of the electrolytic tank body 1, and is close to one side of the side wall of the electrolytic tank body 1, which is connected with the cathode 5-1; the electrolyte outlet pipe 1-2 is arranged at the bottom of the electrolytic tank body 1 and is also close to one side of the cathode 5-1 connected with the side wall of the electrolytic tank body 1; further, the electrolyte liquid inlet pipe 1-1 and the electrolyte liquid outlet pipe 1-2 are respectively arranged on two opposite side walls of the electrolyte tank body, the plate surfaces of the cathode 5-1 and the anode 5-2 are opposite to each other and are opposite to the electrolyte liquid inlet pipe 1-1 and the electrolyte liquid outlet pipe 1-2, and are arranged at intervals with the side walls where the pipes are arranged; through the arrangement, the flowing degree of electrolyte slurry can be improved, so that the disturbance is larger, and the reduction effect is better. The electrode plate surface of the cathode 5-1 is in a corrugated shape so as to increase the electrode surface area and the disturbance degree of electrolyte slurry on the electrode plate surface; it should be noted that the area of the electrode plate surfaces of the cathode 5-1 and the anode 5-2 of the present utility model may be adjusted according to actual needs, the area ratio of the two may be 1:1, or may be other, for example, the area may vary within the range of 1:1-1:100, and the inter-electrode distance between the adjacent cathode 5-1 and anode 5-2 may be adjusted according to actual needs, which may be 0.5-50cm, and the electrode plate of the cathode 5-1 is made of a conductive metal or a non-metal material, such as one or more of lead-antimony alloy, lead-tin alloy, lead plate, nickel, nichrome, copper alloy, aluminum alloy, stainless steel, titanium alloy, and graphite, and the electrode plate of the anode 5-2 is made of a conductive metal or a non-metal and an electrochemical corrosion resistant material, which is a boron doped diamond anode, a ruthenium titanium anode, an iridium titanium anode, a platinum titanium anode, a graphite electrode, and a glassy carbon electrode.
Further, fluid circulation spray holes are formed in the bottom and the side wall of the electrolytic tank body 1, all the fluid circulation spray holes are communicated with the discharge end of the fluid pump through pipelines, so that part of electrolyte slurry is sprayed into the electrolytic tank body 1 from the fluid circulation spray holes through the fluid pump, sediment at the bottom and electrolyte slurry in the middle of the electrolytic tank body 1 are impacted and stirred, graphene oxide in the electrolyte slurry is uniformly dispersed, and meanwhile, the electrolyte slurry in the electrolytic tank body 1 is disturbed.
In the present utility model, each electrode of the electrode unit 5 is supplied with power through an electrolytic cell power supply bus bar 1-3, in this embodiment, the electrode power supply bus bar 5-2-2 is disposed on top of a plate where it is located, the electrolytic cell power supply bus bar 1-3 is divided into a cathode power supply bus bar and an anode power supply bus bar, the cathode power supply bus bar is disposed on a side wall of the electrolytic cell body 1 connected to the cathode 5-1, which is connected to the electrode power supply bus bar 5-2-2 of the cathode 5-1, and the anode power supply bus bar is disposed on a side wall of the electrolytic cell body 1 connected to the anode 5-2, which is connected to the electrode power supply bus bar 5-2-2 of the anode 5-2.
The above-mentioned setting is the open-loop design, and electrode arrangement in cell body 1 is suitable for the S-shaped route satisfies the reaction requirement, can make electrolyte thick liquids fully react, and the quality of the reduction graphene oxide of preparation can satisfy the production demand.
In addition, the device of the utility model can also realize closed-loop design, and the device is concretely as follows:
the fluid pump comprises a feeding pump 2 and a fluid circulating pump 4, wherein the feeding end of the feeding pump 2 is communicated with the electrolytic tank body 1 through an electrolyte outlet pipe 1-2, the discharging end of the feeding pump 2 is communicated with the feeding end of an electrolyte slurry buffer unit, the discharging end of the electrolyte slurry buffer unit is communicated with the feeding end of the fluid circulating pump 4, and the discharging end of the fluid circulating pump 4 is communicated with the electrolytic tank body 1 through the electrolyte inlet pipe 1-1.
Through the arrangement of the feeding pump 2, the fluid circulating pump 4 and the electrolyte buffer unit, the utility model can form a closed cycle of 'the electrolytic tank-feeding pump 2-the electrolyte slurry buffer tank 3-the fluid circulating pump 4-the electrolytic tank' through the electrolytic tank unit, the electrolyte slurry flowing unit and the electrolyte slurry buffer unit, so as to perform liquid flow continuous electrochemical reduction operation on graphene oxide, wherein the feeding pump 2 pumps the electrolyte slurry in the electrolytic tank body 1 into the electrolyte slurry buffer unit, the electrolyte slurry in the electrolyte slurry buffer unit is pumped into the electrolytic tank body 1 by the fluid circulating pump 4 after being processed, the electrolyte slurry in the electrolytic tank body 1 forms a flowing state under the action of the feeding pump 2 and the fluid circulating pump 4, and the electrolyte slurry flows from an electrolyte feeding pipe to an electrolyte discharging pipe, so that the reaction effect is better, and the continuous production of industrialization and mass production can be satisfied.
Preferably, in this embodiment, the electrolyte slurry buffering unit includes an electrolyte slurry buffering tank 3, the electrolyte slurry buffering tank 3 is respectively communicated with the feed pump 2 and the fluid circulation pump 4, a stirrer 3-1 is further disposed in the electrolyte slurry buffering tank 3, so that the electrolyte slurry in the electrolyte slurry buffering tank 3 is stirred by the stirrer 3-1, and the stirrer 3-1 is preferably a high-speed stirrer 3-1, and the rotation speed of the stirrer is 0-20000 rpm.
Further, for better reaction, the electrolyte slurry buffer unit is provided with an electrolyte slurry defoaming unit 6 for defoaming inside the electrolyte slurry buffer unit, so that the electrolyte slurry in the electrolytic tank body 1 is pumped from the feed pump 2 into the electrolyte slurry buffer unit, and defoaming treatment is performed on the electrolyte slurry in the electrolyte slurry buffer unit by using the electrolyte slurry defoaming unit 6, so that the electrolyte slurry is convenient to perform circulating operation. The electrolyte slurry defoaming unit 6 is a vacuum defoaming component, specifically, the electrolyte slurry defoaming unit 6 comprises a homogenizing pump 6-1, an electrolyte defoaming tank 6-2, a defoaming negative pressure cache tank 6-3 and a negative pressure machine 6-4, the liquid inlet end of the homogenizing pump 6-1 is communicated with the electrolyte slurry cache unit, specifically, the electrolyte slurry cache tank 3 is communicated, the liquid outlet end of the homogenizing pump 6-1 is communicated with the electrolyte defoaming tank 6-2, the electrolyte defoaming tank 6-2 is also communicated with the electrolyte slurry cache unit, specifically, the electrolyte slurry cache tank 3 is communicated, and the negative pressure machine 6-4 is communicated with the electrolyte defoaming tank 6-2 through the defoaming negative pressure cache tank 6-3.
In order to make the electrolyte slurry fully react in the electrolytic tank body 1, the electrolyte slurry needs to be controlled within a certain temperature range, in this embodiment, the electrolyte slurry buffer unit is further connected with an electrolytic tank temperature control unit 7 for adjusting the temperature of the electrolyte slurry in the electrolyte slurry buffer unit, so as to control the temperature of the electrolyte slurry through the electrolytic tank temperature control unit 7, specifically, the electrolytic tank temperature control unit 7 includes a PLC central controller 7-1, a heat exchanger 7-2 and a first temperature sensor 7-3, the PLC central controller 7-1 is electrically connected with the heat exchanger 7-2 and the first temperature sensor 7-3 respectively, the heat exchange coil of the heat exchanger 7-2 and the first temperature sensor 7-3 are both installed in the electrolyte slurry buffer unit, specifically, in the electrolyte slurry buffer tank 3, the heat exchanger 7-2 is used for heating the electrolyte slurry in the electrolyte slurry buffer tank 3, the first temperature sensor 7-3 is used for sensing the electrolyte slurry in the electrolyte slurry buffer tank 3, and the temperature sensor 7-3 is controlled within the temperature range of the first temperature sensor 7-3, such as the electrolyte slurry in the first temperature sensor 7-3 is controlled within the temperature range of the electrolyte slurry buffer tank 7-3, thereby realizing that the temperature control of the electrolyte slurry in the first temperature buffer tank 7-3 is controlled within the temperature range of the PLC central controller 7-3, such as the temperature sensor 7-20. Further, for better controlling the temperature of the electrolyte slurry in the electrolytic tank body 1, the electrolytic tank temperature control unit 7 comprises a second temperature sensor 7-4 and a third temperature sensor 7-5, wherein the second temperature sensor 7-4 and the third temperature sensor 7-5 are electrically connected with the PLC central controller 7-1 and are both installed in the electrolytic tank body 1, the second temperature sensor 7-4 is close to one side wall of the electrolytic tank body 1, the electrolyte inlet pipe 1-1 is arranged close to the electrolytic tank body 1, and the third temperature sensor 7-5 is close to one side wall of the electrolytic tank body 1, the electrolyte outlet pipe 1-2 is arranged close to the electrolytic tank body 1. Further, the electrolyte liquid inlet pipe 1-1 is further communicated with the total discharging pipe 9, the total discharging pipe 9 is provided with a pipeline stop valve 8, the electrolyte liquid outlet pipe 1-2 is further communicated with the total feeding pipe 10, and the total feeding pipe 10 is also provided with the pipeline stop valve 8, so that the slurry to be reacted can enter the electrolytic tank body 1 through the total feeding pipe 10, and the slurry after the reaction is discharged out of the device through the total discharging pipe 9, thereby realizing continuous production of the reduced graphene. Of course, according to the actual production requirement, the utility model can also be used for introducing a new batch of raw materials through the total feeding pipe 10 after all the slurry is discharged through the total discharging pipe 9, namely, the utility model can also be used for intermittent production besides continuous production.
The utility model reduces electrolyte slurry according to the following principle:
fully mixing graphene oxide, electrolyte, solvent, additives and the like to prepare electrolyte slurry, conveying the electrolyte slurry into an electrolyte slurry cache tank 3, starting an electrolytic tank temperature control unit 7 to perform temperature control treatment on the electrolyte slurry in the electrolyte slurry cache tank 3, and conveying the electrolyte slurry into an electrolytic tank body 1 through a Liu Tie circulating pump after the temperature of the material is stable. The power supply bus 1-3 of the electrolytic tank is communicated with a direct current power supply, voltage is applied to each electrode through the electrode electron supply line 5-2-2 for electrochemical reduction, electrolyte slurry flows through the surface of the cathode 5-1, S-shaped flow is shown in the electrolytic tank body 1, the electrolyte slurry flows through the last cathode 5-1 and then enters the electrolyte slurry buffer tank through the feed pump 2, and the electrolyte slurry enters the electrolytic tank body 1 through the fluid circulating pump 4 after temperature control and flows circularly. Meanwhile, the temperature of the materials in the electrolytic tank body 1 is monitored through the PLC central controller 7-1, and the heat exchanger is controlled to perform constant temperature treatment on the materials. And (3) carrying out solid-liquid separation on the material obtained after the reduction is finished, and cleaning, separating and drying the solid material to finally obtain the electrochemically reduced graphene oxide.
Finally, the shape of the electrolytic tank body 1 of the present utility model may be selected according to actual needs, and may be square or rectangular, and the electrolytic tank body 1 may be made of an insulating material or a metal material with an insulating material covered on the surface. A pipeline stop valve 8 is arranged on the pipeline through which the fluid flows so as to control the passage of the pipeline. The power supply bus 1-3 of the electrolytic cell is arranged on a bus bearing fixed support 1-3-2 through a power supply bus insulating cushion layer 1-3-1, and the bus bearing fixed support 1-3-2 is fixed on the side wall of the electrolytic cell body 1.
The foregoing description is directed to the preferred embodiments of the present utility model, but the embodiments are not intended to limit the scope of the utility model, and all equivalent changes or modifications made under the technical spirit of the present utility model should be construed to fall within the scope of the present utility model.
Claims (10)
1. The device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow is characterized in that: comprises an electrolytic tank unit, an electrode unit and an electrolyte slurry flow unit;
the electrolytic tank unit comprises an electrolytic tank body, and an electrolyte inlet pipe and an electrolyte outlet pipe are respectively arranged on the electrolytic tank body;
the electrode unit comprises a plurality of cathodes and a plurality of anodes, the cathodes and the anodes are alternately arranged at intervals, the cathodes and the anodes are arranged between an electrolyte inlet pipe and an electrolyte outlet pipe, each cathode and each anode are connected with an electrolyte tank power supply bus through an electrode power supply line, the bottoms of each cathode and each anode are tightly connected with a bottom panel of an electrolyte tank body, only one side wall of each cathode is tightly attached to one side wall of the electrolyte tank body, only one side wall of each anode is tightly attached to one side wall of the electrolyte tank body, and only one side wall of each anode is tightly attached to one side wall of the electrolyte tank body; an encapsulated electrode diaphragm is paved outside the electrode plate surface of each anode, a gas cavity is formed between the encapsulated electrode diaphragm and the electrode plate of the anode, and an anode exhaust pipe communicated with the gas cavity is arranged at the top of the anode;
the electrolyte slurry flowing unit comprises a fluid pump, and the discharge end of the fluid pump is communicated with the electrolytic tank body through an electrolyte inlet pipe.
2. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 1, wherein: the number of the cathode is one more than the number of the anode; all cathodes and all anodes are positioned between an electrolyte inlet pipe and an electrolyte outlet pipe, and the electrolyte inlet pipe is arranged at the upper part of the electrolytic tank body, is close to the top of the electrolytic tank body and is close to one side of the side wall of the electrolytic tank body, which is connected with the cathodes; the electrolyte outlet pipe is arranged at the bottom of the electrolytic tank body and is also close to one side of the side wall of the electrolytic tank body, which is connected with the cathode.
3. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 1, wherein: the electrode plate of the cathode is in a fold shape.
4. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 1, wherein: the bottom and the side wall of the electrolytic tank body are respectively provided with a fluid circulation spray hole, and all the fluid circulation spray holes are communicated with the discharge end of the fluid pump through pipelines.
5. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 1, wherein: the top of the electrolytic tank body is provided with a sealing cover, the top of the sealing cover is provided with a cathode exhaust manifold, and the cathode exhaust manifold is communicated with the inside of the electrolytic tank body through the sealing cover; the anode exhaust pipes on all anodes extend to the outside of the electrolytic cell body.
6. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 1, wherein: the fluid pump comprises a feeding pump and a fluid circulating pump, wherein the feeding end of the feeding pump is communicated with the electrolytic tank body through an electrolyte outlet pipe, the discharging end of the feeding pump is communicated with the feeding end of the electrolyte slurry caching unit, the discharging end of the electrolyte slurry caching unit is communicated with the feeding end of the fluid circulating pump, and the discharging end of the fluid circulating pump is communicated with the electrolytic tank body through an electrolyte inlet pipe.
7. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with a liquid stream according to claim 6, wherein: the electrolyte slurry caching unit comprises an electrolyte slurry caching tank which is respectively communicated with the feeding pump and the fluid circulating pump, and a stirrer is further arranged in the electrolyte slurry caching tank.
8. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with a liquid stream according to claim 6, wherein: the electrolyte slurry buffer unit is provided with an electrolyte slurry defoaming unit for defoaming the inside of the electrolyte slurry buffer unit; the electrolyte slurry defoaming unit comprises a homogenizing pump, an electrolyte defoaming tank, a defoaming negative pressure buffer tank and a negative pressure machine, wherein the liquid inlet end of the homogenizing pump is communicated with the electrolyte slurry buffer unit, the liquid outlet end of the homogenizing pump is communicated with the electrolyte defoaming tank, the electrolyte defoaming tank is also communicated with the electrolyte slurry buffer unit, and the negative pressure machine is communicated with the electrolyte slurry buffer unit through the defoaming negative pressure buffer tank.
9. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with a liquid stream according to claim 6, wherein: the electrolyte slurry buffer unit is also connected with an electrolytic tank temperature control unit for regulating the temperature of the electrolyte slurry in the electrolyte slurry buffer unit; the temperature control unit of the electrolytic tank comprises a PLC central controller, a heat exchanger and a first temperature sensor, wherein the PLC central controller is respectively and electrically connected with the heat exchanger and the first temperature sensor, and a heat exchange coil of the heat exchanger and the first temperature sensor are both arranged inside the electrolyte slurry buffer unit.
10. The apparatus for preparing reduced graphene by continuously electrochemically reducing graphene oxide with liquid flow according to claim 9, wherein: the electrolysis bath temperature control unit further comprises a second temperature sensor and a third temperature sensor, wherein the second temperature sensor and the third temperature sensor are electrically connected with the PLC central controller and are both installed in the electrolysis bath body, the second temperature sensor is close to the part of the electrolysis bath body, which is provided with the electrolyte inlet pipe, and the third temperature sensor is close to the part of the electrolysis bath body, which is provided with the electrolyte outlet pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223159919.4U CN219709127U (en) | 2022-11-28 | 2022-11-28 | Device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202223159919.4U CN219709127U (en) | 2022-11-28 | 2022-11-28 | Device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow |
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| CN219709127U true CN219709127U (en) | 2023-09-19 |
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| CN202223159919.4U Active CN219709127U (en) | 2022-11-28 | 2022-11-28 | Device for preparing reduced graphene by continuously electrochemically reducing graphene oxide through liquid flow |
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| CN (1) | CN219709127U (en) |
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