CN212269467U - Counter electrode device for preparing graphene through electrochemical stripping - Google Patents
Counter electrode device for preparing graphene through electrochemical stripping Download PDFInfo
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- CN212269467U CN212269467U CN202022095210.7U CN202022095210U CN212269467U CN 212269467 U CN212269467 U CN 212269467U CN 202022095210 U CN202022095210 U CN 202022095210U CN 212269467 U CN212269467 U CN 212269467U
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Abstract
The utility model discloses a preparation graphite alkene is peeled off to electrode assembly to electrochemistry, including the metal counter electrode board, the plate electrode is arranged in insulating ion exchange membrane braced frame, the part that the plate electrode stretches out from the ion exchange membrane support frame forms banding conductive tab, conductive tab is pressed from both sides the dress by the insulation board, the shape that insulation board and conductive tab are the mirror symmetry part is unanimous for insulating tab with the shape of conductive tab this symmetry part, conductive tab and insulating tab tip outwards are equipped with the radius that the direction is unanimous and the semicircle orifice that the line footpath is the same of conductive bus, the insulation board is stretched out to the semicircle orifice portion of conductive tab, ion exchange membrane braced frame all is equipped with a set of branch spacer with the parallel two sides of plate electrode working face, all be equipped with the ion exchange membrane with branch spacer sealing connection in every branch spacer, ion exchange membrane braced frame is equipped with a. The device has the advantages of low cost, safety, high efficiency, simple operation and continuous production.
Description
Technical Field
The utility model relates to a technique of electrochemistry rule modularization production graphite alkene specifically is an electrochemistry peels off counter electrode device of preparation graphite alkene.
Background
Graphene is a two-dimensional crystalline material consisting of a layer of atoms of carbon, the main source of preparation being graphite. The single-layer crystal graphene successfully prepared from the raw graphite by professor gooves and professor norwoshohol, university of manchester, uk, proves that the graphene can exist in the natural environment. The graphene has excellent mechanical, electrical, thermal and optical properties.
Compared with other methods, the method for preparing graphene by electrochemically stripping graphite has the advantages of low cost, greenness, safety, high efficiency and the like, and is a new method for industrially producing graphene. In the process of electrical stripping of a water system, oxygen generated by an anode props up sheets of graphite, so that graphene is generated, hydrogen is generated by the cathode simultaneously due to electrochemical stripping in an aqueous solution, a large amount of gas is generated in large-scale production, if measures are not taken to separate the gas generated by the anode and the cathode in the electrical stripping process, the oxygen generated by the anode and the hydrogen generated by the cathode can be directly contacted, explosion can be generated under the condition of existence of tiny sparks, and great potential safety hazards exist in the large-scale production process. Therefore, the key to avoid explosion of the electric stripping process is to avoid the contact between oxygen generated by the anode and hydrogen generated by the cathode during the electric stripping process.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a counter electrode device of preparation graphite alkene is peeled off to prior art must not be enough to the electrochemistry. The device has the advantages of low cost, safety, high efficiency, simple operation and continuous production.
Realize the utility model discloses the technical scheme of purpose is:
a counter electrode device for preparing graphene by electrochemical stripping comprises a metal counter electrode plate, wherein the electrode plate is arranged in an insulated ion exchange membrane supporting frame, the part of the electrode plate extending out of the ion exchange membrane supporting frame forms a strip-shaped conductive tab, the conductive tab is clamped by an insulating plate, the shape of the mirror symmetry part of the insulating plate and the conductive tab is consistent with the shape of the symmetry part of the conductive tab and is an insulated tab, the outward end parts of the conductive tab and the insulated tab are provided with semicircular holes with consistent directions and the radius of which is the same as the diameter of a conductive bus, the semicircular hole parts of the conductive tab extend out of the insulating plate, two surfaces of the ion exchange membrane supporting frame, which are parallel to the working surface of the counter electrode plate, are respectively provided with a group of separation frames, each separation frame is internally provided with an ion exchange membrane hermetically connected with the separation frame, and the upward end, the lower part of the ion exchange membrane supporting frame extending into the electrode groove is provided with a group of liquid guide holes, and the counter electrode device is fixed on the bus in a suspension mode.
The insulating plate and the ion exchange membrane supporting frame are made of acrylic plates, polypropylene plastic plates or wood plates, the function of the insulating plate and the ion exchange membrane supporting frame is an insulating effect, and when the acrylic plates are adopted, the adhesive adopted by the acrylic plates is dichloromethane.
The ion exchange membrane is a material which can enable electrolyte ions to freely pass through and can also isolate the contact between a cathode and an anode gas product, oxygen generated by the anode and hydrogen generated by the cathode can not contact with each other through the ion exchange membrane, so that the danger of explosion is avoided, the ion exchange membrane allows the ions to pass through and isolates the gas from passing through, and the rapid passing of the ions and the migration of the ions to the graphite electrode are subjected to intercalation reaction.
The quantity of air guide hole and drain hole is 2 at least, and the produced gas of counter electrode passes through the air guide hole and discharges and can be collected and recycle, and the setting up of drain hole can make the electrolyte in the electrolysis trough can get into ion exchange membrane braced frame, and the electrolyte in the inslot of being convenient for like this exchanges with the electrolyte in the ion exchange membrane braced frame to slow down concentration polarization.
The counter electrode device is a cathode when working in an aqueous electric stripping environment, and is an anode when working in an organic electric stripping environment.
The ion exchange membrane is in a swelling state when being soaked in the electrolyte, and the ion exchange membrane is fixed by the ion exchange membrane support frame, so that stable production is realized.
The working process of the device is as follows: the two buses are placed on a cell body of an electrolytic cell in parallel, then N graphite electrode devices and N +1 counter electrode devices are arranged on a conductive bus at intervals, the graphite electrode devices and the counter electrode devices are in opposite parallel positions, adjacent electrode devices have polar distances, electrolyte is injected into the electrolytic cell, the buses in the electrolytic cell are connected with a direct-current power supply through a lead, the power supply output is set to be 1V-60V, liquid exchange is carried out on the counter electrode devices through two liquid guide pipes at the lower part of the counter electrode devices, the concentration polarization of the electrolyte is favorably slowed down, after electrification, under the action of an electric field, cations in the electrolyte migrate to cathodes, and anions migrate to the anodes to intercalate graphite; gas is generated by gas evolution reaction of an anode and a cathode, a large amount of gas is generated at the side of the cathode, a large amount of bubbles upwards emerge along an electrode plate, the gas is limited at one side of a counter electrode device and cannot diffuse to the side of a graphite electrode in the presence of an ion exchange membrane and is discharged through two gas guide pipes at the upper part of the electrode device, so that the gas of the cathode and the anode is isolated, the electric stripping time is 1-8h, the anode graphite electrode is completely stripped into a large amount of graphene, the gas generated in the counter electrode device is only discharged from a gas guide hole and collected all the time, the graphite electrode is stripped into graphene slurry, the counter electrode device can be recycled, the counter electrode device is ultrasonically cleaned for 10min after stripping is finished, and the graphene slurry is soaked in deionized water for the next use.
According to the technical scheme, a layer of ion exchange membrane is adopted between a cathode and an anode, so that oxygen generated by the anode cannot contact hydrogen generated by the cathode, and the explosion danger is avoided; the counter electrode plate is suspended at one end of two ends of the bus to be conductive, and the other end of the counter electrode plate is connected with the electrode by adopting an insulating material, so that one end of the electrode is insulated to avoid the danger of short circuit; when the graphene is prepared, if the diaphragm is arranged on one side of the graphite working electrode, the complexity of the graphite working electrode device is increased, meanwhile, the product of the graphite electrode is attached to an ion exchange membrane, the ion exchange membrane is polluted and difficult to clean, and the ion exchange membrane is arranged on one side of the counter electrode device, so that the structural complexity of the graphite electrode device can be simplified; when the service life of the ion exchange membrane reaches the service life and needs to be replaced, the ion exchange membrane is convenient to replace.
The device has the advantages of low cost, safety, high efficiency, simple operation and continuous production.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment;
FIG. 2 is an SEM photograph of a stripped product of the example;
FIG. 3 is a TEM image of the product stripped off in the example.
In the figure, 1, an electrode plate 2, an ion exchange membrane supporting frame 3, a conductive tab 4, an insulating plate 5, an insulating tab 6, a separation frame 7, an ion exchange membrane 8, an air vent 9 and a liquid vent.
Detailed Description
The contents of the present invention will be further described with reference to the accompanying drawings and examples, but the present invention is not limited thereto.
Example (b):
referring to fig. 1, a counter electrode device for preparing graphene by electrochemical stripping comprises a metal counter electrode plate 1, wherein the electrode plate 1 is arranged in an insulating ion exchange membrane support frame 2, a strip-shaped conductive tab 3 is formed by a part of the electrode plate 1 extending out of the ion exchange membrane support frame 2, the conductive tab 3 is clamped by an insulating plate 4, the insulating plate 4 and the conductive tab 3 are in mirror symmetry, the shape of the symmetrical part of the conductive tab 3 is consistent with that of the insulating tab 5, semicircular holes with the same direction and the same radius as the diameter of a conductive bus line are arranged at the outward end parts of the conductive tab 3 and the insulating tab 5, the semicircular hole part of the conductive tab 3 extends out of the insulating plate 4, a group of separation frames 6 are arranged on two parallel surfaces of the working surface of the ion exchange membrane support frame 2 and the counter electrode plate 1, and an ion exchange membrane 7 hermetically connected with the separation frames 6 is, the tip up when ion exchange membrane braced frame 2 stretches into the electrode tank is equipped with a set of air guide 8, and the lower part that ion exchange membrane braced frame 2 stretched into the electrode tank is equipped with a set of drain hole 9, adopts the mode of hanging to fix on the generating line to electrode assembly.
The insulating plate 4 and the ion exchange membrane supporting frame 2 are made of acrylic plates, polypropylene plastic plates or wood plates, and the function of the insulating plate and the ion exchange membrane supporting frame is insulating, wherein the acrylic plates are adopted in the embodiment, and dichloromethane is adopted as an adhesive for the acrylic plates.
The ion exchange membrane 7 is a material which can enable electrolyte ions to freely pass through and can also isolate the contact between a cathode and an anode gas product, the ion exchange membrane 7 enables oxygen generated by the anode and hydrogen generated by the cathode not to contact, the explosion danger is avoided, the ion exchange membrane 7 allows the ions to pass through but isolates the gas from passing through, the ions rapidly pass through and migrate to a graphite electrode to carry out intercalation reaction, and the ion exchange membrane 7 is a perfluorinated sulfonic acid ion exchange membrane.
The quantity of air guide hole 8 and drain hole 9 is 2 at least, and the produced gas of counter electrode 1 passes through air guide hole 8 and discharges and can be collected and recycle, and the setting up of drain hole 9 can make the electrolyte in the electrolysis trough can get into ion exchange membrane braced frame 2, and the electrolyte of the inslot of being convenient for like this exchanges with the electrolyte in the ion exchange membrane braced frame 2 to slow down concentration polarization.
The counter electrode device is a cathode when working in an aqueous electric stripping environment, and is an anode when working in an organic electric stripping environment.
The working process of the device is as follows: the working process of the device is as follows: the two buses are placed on a cell body of an electrolytic cell in parallel, then N graphite electrode devices and N +1 counter electrode devices are arranged on a conductive bus at intervals, the graphite electrode devices and the counter electrode devices are in opposite parallel positions, adjacent electrode devices have polar distances, electrolyte is injected into the electrolytic cell, the buses in the electrolytic cell are connected with a direct-current power supply through a lead, the power supply output is set to be 1V-60V, liquid exchange is carried out on the counter electrode devices through two liquid guide pipes at the lower part of the counter electrode devices, the concentration polarization of the electrolyte is favorably slowed down, after electrification, under the action of an electric field, cations in the electrolyte migrate to cathodes, and anions migrate to the anodes to intercalate graphite; gas is generated by gas evolution reaction of an anode and a cathode, a large amount of gas is generated at the side of the cathode, a large amount of bubbles are upwards emitted along an electrode plate, the gas is limited at one side of a counter electrode device and cannot be diffused to the side of a graphite electrode in the presence of an ion exchange membrane and is discharged through two gas guide pipes at the upper part of the electrode device, so that the gas of the cathode and the anode is isolated, the electric stripping time is 1-8h, the anode graphite electrode is completely stripped into a large amount of graphene, the gas generated in the counter electrode device is only discharged from a gas guide hole 7 and collected all the time, the graphite electrode is stripped into graphene slurry, the counter electrode device can be recycled, the counter electrode device is ultrasonically cleaned for 10min after stripping is finished and is soaked in deionized water for next use, and the device is used for electrochemically stripping an SEM image of a product for preparing the graphene, The TEM images are shown in fig. 2 and 3, respectively.
Claims (5)
1. A counter electrode device for preparing graphene by electrochemical stripping is characterized by comprising a metal counter electrode plate, wherein the electrode plate is arranged in an insulated ion exchange membrane supporting frame, the part of the electrode plate, which extends out of an ion exchange membrane supporting frame, forms a strip-shaped conductive tab, the conductive tab is clamped by an insulating plate, the shape of the mirror symmetry part of the insulating plate and the conductive tab is consistent with the shape of the symmetry part of the conductive tab and is an insulated tab, the outward end parts of the conductive tab and the insulated tab are provided with semicircular holes with consistent directions and the same radius as the line diameter of a conductive bus, the semicircular holes of the conductive tab extend out of the insulating plate, two surfaces of the ion exchange membrane supporting frame, which are parallel to the working surface of the counter electrode plate, are respectively provided with a group of separation frames, each separation frame is internally provided with an ion exchange membrane which is hermetically connected with the separation frame, and the upward end, the lower part of the ion exchange membrane supporting frame extending into the electrode groove is provided with a group of liquid guide holes, and the counter electrode device is fixed on the bus in a suspension mode.
2. The counter electrode device for preparing graphene through electrochemical stripping according to claim 1, wherein the insulating plate and the ion exchange membrane support frame are made of acrylic plates, polypropylene plastic plates or wood plates.
3. The counter electrode device for preparing graphene through electrochemical stripping according to claim 1, wherein the ion exchange membrane is made of a material capable of enabling electrolyte ions to freely pass through and isolating contact between cathode and anode gas products.
4. The counter electrode device for preparing graphene by electrochemical stripping as claimed in claim 1, wherein the number of the gas-conducting holes and the liquid-conducting holes is at least 2.
5. The counter electrode device for preparing graphene through electrochemical stripping according to any one of claims 1 to 4, wherein the counter electrode device is a cathode when operated in an aqueous electrostripping environment and is an anode when operated in an organic electrostripping environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022095210.7U CN212269467U (en) | 2020-09-23 | 2020-09-23 | Counter electrode device for preparing graphene through electrochemical stripping |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202022095210.7U CN212269467U (en) | 2020-09-23 | 2020-09-23 | Counter electrode device for preparing graphene through electrochemical stripping |
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| CN212269467U true CN212269467U (en) | 2021-01-01 |
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