CN113603082A - Electrode structure for preparing graphene by graphite powder electrochemical method - Google Patents
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- CN113603082A CN113603082A CN202110916045.3A CN202110916045A CN113603082A CN 113603082 A CN113603082 A CN 113603082A CN 202110916045 A CN202110916045 A CN 202110916045A CN 113603082 A CN113603082 A CN 113603082A
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- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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Abstract
The invention discloses an electrode structure for preparing graphene by a graphite powder electrochemical method, which comprises two cathode plate groups, an anode plate and a U-shaped frame; the U-shaped frame is an insulating part with an upward notch and a through inner groove at the left and right sides, the two cathode plate groups are vertically arranged in the U-shaped frame along the front and back direction and are distributed in the U-shaped frame at intervals along the left and right direction, and the two cathode plate groups and the U-shaped frame jointly enclose to form a groove chamber with an upward notch; the side, close to each other, of each of the two cathode plate groups is provided with an insulating grid plate, each grid plate is provided with a plurality of grid holes, and the opening sides of the grid holes in the two grid plates are close to each other; a cathode plate is also arranged in the two cathode plate groups; the negative plate group is provided with a left and right through flow dispersing channel, the positive plate is vertically clamped between the two negative plate groups along the front and back direction, and the opening sides of the grid holes on the two grid plates are plugged; the anode plate is uniformly provided with left and right through flow dredging holes, so that the graphene preparation cost is low, and the preparation efficiency is high.
Description
Technical Field
The invention belongs to the field of graphene preparation devices, and particularly relates to an electrode structure for preparing graphene by a graphite powder electrochemical method.
Background
The existing methods for preparing graphene include mechanical stripping methods, redox methods, chemical vapor deposition methods, epitaxial growth methods, electrochemical methods and the like. The graphene prepared by the oxidation-reduction method has very low efficiency, the reduced graphene oxide prepared by the oxidation-reduction method has very large defects, and the graphene prepared by the electrochemical method has the characteristics of almost complete structure, large specific surface area and low oxidation defect, which are different from the former two methods.
Disclosure of Invention
In order to solve the technical problems pointed out in the background art, the invention aims to provide an electrode structure which is high in preparation efficiency and low in cost and can be used for preparing graphene by a graphite powder electrochemical method on a large scale.
The technical scheme of the invention is as follows: an electrode structure for preparing graphene by a graphite powder electrochemical method comprises two cathode plate groups, an anode plate and a U-shaped frame;
the U-shaped frame is an insulating part with an upward notch and a through inner groove at the left and right sides, the two cathode plate groups are vertically arranged in the U-shaped frame along the front and back direction and are distributed in the U-shaped frame at intervals along the left and right direction, and the two cathode plate groups and the U-shaped frame jointly enclose to form a groove chamber with an upward notch;
one side, close to each other, of each of the two cathode plate groups is provided with an insulating grid plate, each grid plate is provided with a plurality of grid holes, and the opening sides of the grid holes in the two grid plates are close to each other;
a cathode plate is also arranged in the two cathode plate groups;
the cathode plate groups are uniformly provided with left and right through flow channels, the anode plate is vertically clamped between the two cathode plate groups along the front and back direction and plugs the opening sides of the grid holes on the two grid plates;
flow dredging holes which penetrate left and right are uniformly distributed on the anode plate;
every the downthehole graphite powder batching that is used for containing of grid in the middle part of grid plate, the rest the grid hole is used for supplying graphite powder inflation is filled, the anode plate is used for being connected with the anodal electricity of power, two the cathode plate all is used for being connected with power negative pole electricity.
Preferably, a plurality of convex columns extending into the grid holes on the same side are convexly arranged on two sides of the anode plate, at least one convex column extends into each grid hole, and a drainage hole penetrating the convex column from left to right is arranged at a position corresponding to each convex column.
Preferably, the anode plate and the cathode plate are titanium plates, and the surfaces of the anode plate and the cathode plate are coated with ruthenium oxide coatings.
Preferably, the cathode plate group further comprises a clamping plate and a diaphragm, wherein the clamping plate is an insulating plate;
the negative plate is arranged on one side of the clamping plate, and the grid plate is convexly arranged in the middle of one side of the negative plate, which is far away from the clamping plate;
the clamping plate and the cathode plate are respectively provided with a plurality of through holes, the through holes in the clamping plate are communicated with the through holes in the cathode plate to form the flow distribution channel, and each grid hole is communicated with at least one through hole in the cathode plate;
the diaphragm is attached to any one side or two sides of the clamping plate and used for preventing the graphite powder ingredient from leaking through the flow dredging channel;
specifically, the U-shaped frame and the two clamping plates jointly enclose to form the slot chamber.
Specifically, the clamping plate is a PP plate.
Specifically, the diaphragm is a PE non-woven velvet fabric layer.
Preferably, the two cathode plate groups are a first cathode plate group and a second cathode plate group respectively;
the clamping plate of the first cathode plate group is fixedly connected with the left side of the U-shaped frame or integrally formed;
the second cathode plate group is arranged in the U-shaped frame and limited in the U-shaped frame or limited in the U-shaped frame by a limiting part arranged on the right side of the U-shaped frame.
Further preferably, the limiting member comprises a plurality of bolts;
a plurality of screw holes penetrating through the U-shaped frame in the front and back direction are formed in the right sides of the groove walls on the two sides of the U-shaped frame at intervals up and down, the screw holes are located in the same vertical plane, one bolt is installed at each screw hole in a threaded mode, and the threaded end of each bolt faces the inside of the U-shaped frame;
the second cathode plate group is arranged in the U-shaped frame and positioned on the left side of the plurality of bolts, the bolts are screwed until the threaded ends of the bolts all extend into the U-shaped frame and are blocked on the right side of the second cathode plate group to limit, or the bolts are unscrewed to release the limit and take the second cathode plate group out of the U-shaped frame.
The invention has the beneficial effects that: the graphene is prepared by taking graphite powder as a raw material, and the cost of the raw material is far lower than that of a graphite rod or flexible graphite paper; the convex columns are arranged on the two sides of the anode plate, and the flow-dredging holes are formed in the positions of the convex columns, so that on one hand, the contact area of the anode plate and graphite powder can be increased, on the other hand, the flow-dredging holes and the flow-dredging channels are matched to improve the circulation of electrolyte, free and rapid penetration of electrolyte ions can be realized, and the current density at each position is uniform, the catalytic potential is high, so that the preparation efficiency of graphene is higher; ruthenium oxide coatings are coated on the cathode plate and the anode plate, so that the electrocatalytic activity and the corrosion resistance of the cathode plate and the anode plate can be improved; the graphite powder support device has the advantages that the grid plates are arranged to serve as supports of the graphite powder, so that the graphite powder support effect is good; in addition, the reserved grid holes are used for graphite powder to expand and fill on each grid plate, so that the graphite powder floats upwards or sinks downwards along the upper cavity and the lower cavity after expansion and stripping, the change of the distance between the cathode plate group and the anode plate caused by expansion is reduced, and the potential between the cathode plate and the anode plate is prevented from being reduced in the electrolysis process.
Drawings
FIG. 1 is a top view of an electrode structure according to the present invention;
FIG. 2 is a right side view of the electrode structure of the present invention;
FIG. 3 is a schematic view of a cathode plate set and an anode plate set according to the present invention;
FIG. 4 is an exploded view of a cathode plate set and an anode plate set according to the present invention;
figure 5 is a schematic view of the construction of the anode plate of the present invention;
fig. 6 is a schematic view of the construction of the grid plate according to the 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, an embodiment of the present invention provides an electrode structure for preparing graphene by a graphite powder electrochemical method, including two cathode plate groups 100, an anode plate 200, and a U-shaped frame 300;
the U-shaped frame 300 is an insulating member with an upward notch and a through inner groove in the U-shaped frame, the two cathode plate groups 100 are vertically arranged in the U-shaped frame 300 along the front-back direction and are distributed in the U-shaped frame 300 at intervals along the left-right direction, and the two cathode plate groups 100 and the U-shaped frame 300 jointly enclose to form a groove chamber with an upward notch;
an insulating grid plate 110 is arranged on one side of each of the two cathode plate groups 100 close to each other, each of the two grid plates 110 has a plurality of grid holes 111, and the opening sides of the grid holes 111 on the two grid plates 110 are close to each other;
a cathode plate 120 is further arranged in the two cathode plate groups 100;
left and right through flow channels (which are beneficial for electrolyte to pass through the cathode plate groups) are uniformly distributed on the cathode plate groups 100, and the anode plate 200 is vertically clamped between the two cathode plate groups 100 along the front-back direction and plugs the opening sides of the grid holes 111 on the two grid plates 110;
flow-dredging holes 210 which penetrate left and right are uniformly distributed on the anode plate 200 (which is beneficial for the electrolyte to pass through the anode plate);
each grid hole 111 in the middle of each grid plate is used for containing graphite powder ingredients, the rest grid holes are used for filling the graphite powder in an expansion mode, the anode plate 200 is used for being electrically connected with a positive electrode of a power supply, and the two cathode plates 120 are both used for being electrically connected with a negative electrode of the power supply.
Preferably, a plurality of convex columns 220 extending into the grid holes 111 on the same side are convexly arranged on both sides of the anode plate 200, at least one convex column 220 extends into each grid hole 111, and a drainage hole 210 penetrating the convex column 220 from left to right is arranged at a position corresponding to each convex column 220.
Preferably, the anode plate 200 and the cathode plate 120 are both titanium plates, and the surfaces thereof are coated with ruthenium oxide coatings.
Preferably, the cathode plate group 100 further includes a clamping plate 130 and a diaphragm 140, wherein the clamping plate 130 is an insulating plate;
the cathode plate 120 is arranged on one side of the clamping plate 130, and the grid plate 110 is convexly arranged in the middle of one side of the cathode plate 120, which is far away from the clamping plate 130;
the clamping plate 130 and the cathode plate 120 are respectively provided with a plurality of through holes, the through holes on the clamping plate 130 are communicated with the through holes on the cathode plate 120 to form the flow distribution channel, and each grid hole 111 is communicated with at least one through hole on the cathode plate 120;
the diaphragm 140 is attached to any one side or two sides of the clamping plate 130, and the diaphragm 140 is used for preventing the graphite powder ingredient from leaking through the flow dredging channel;
the U-shaped frame 300 and the two clamping plates 130 together enclose the slot chamber.
Wherein, the through-hole on splint and the negative plate is all comparatively intensive, and the through-hole on splint and the negative plate can have local through-going or partial through-hole to link up in order to form to dredge the flow passage when splint and negative plate laminating are fixed like this, and when being equipped with the diaphragm between the two, the through-hole on splint and the negative plate or link up in order to form to dredge the flow passage through the diaphragm.
Preferably, the size and shape of the clamping plate, the diaphragm and the cathode plate are consistent and are sequentially attached and fixed, preferably, the lower end of the grid plate is aligned with the lower ends and two sides of the cathode plates at two sides, but the height of the grid plate is lower than that of the cathode plates, the lower end of the anode plate is flush with the lower end of the grid plate, but the upper end of the anode plate is higher than that of the grid plate, so that graphite powder can be added into grid holes above the grid plate, the grid holes at the lower part of the grid plate can be used as a lower expansion area of the graphite powder, the area at the upper part of the grid plate can be used as an upper expansion area of the graphite powder, and the graphite powder expands upwards and downwards respectively when expanding.
Specifically, the clamping plate 130 is a PP plate (preferably, a PP mesh plate, meshes of which form the through holes, and similarly, the cathode plate is also a titanium mesh plate, meshes of which form the through holes), and preferably, both the U-shaped frame and the grid plate are made of PP.
Specifically, the diaphragm 140 is a PE nonwoven velour layer.
Preferably, the two cathode plate groups 100 are a first cathode plate group and a second cathode plate group respectively;
the clamping plate 130 of the first cathode plate group is fixedly connected with the left side of the U-shaped frame 300 or integrally formed;
the second cathode plate group is placed in the U-shaped frame 300, and is limited in the U-shaped frame 300 or released from the limitation by a limiting member disposed on the right side of the U-shaped frame 300.
Further preferably, the limiting member includes a plurality of bolts 310;
a plurality of screw holes penetrating through the U-shaped frame 300 from front to back are formed in the right sides of the groove walls on the two sides of the U-shaped frame at intervals up and down, the screw holes are located in the same vertical plane, one bolt 310 is installed at each screw hole in a threaded mode, and the threaded end of each bolt 310 faces the inside of the U-shaped frame 300;
the second cathode plate set is arranged in the U-shaped frame 300 and positioned at the left side of the plurality of bolts 310, the plurality of bolts 310 are screwed until the threaded ends of the plurality of bolts 310 all extend into the U-shaped frame 300 and stop at the right side of the second cathode plate set for limiting, or the plurality of bolts 310 are unscrewed to release the limitation and take the second cathode plate set out of the U-shaped frame 300. Preferably, when the anode plate is clamped in the U-shaped frame by the two cathode plate groups, a gap of about 0.5cm can be reserved between the bolts and the second cathode plate group, when the bolts are tightened, the second cathode plate group is pressed to move rightwards to abut against the bolts when graphite powder ingredients expand, and a gap is reserved between the anode plate and the two cathode plate groups for graphite powder to diffuse to the periphery of the grid plate.
Wherein, the distance between the cathode plate and the anode plate 200 is preferably 20-25mm, the electrolyte can adopt acid electrolyte, alkaline or salt electrolyte, the graphite powder ingredient comprises graphite powder (200 mesh graphite powder with carbon content not less than 99%), sodium nitrate and a small amount of acid anion dispersing powder, the electrode structure can firstly process under the condition of acid electrolyte with low-voltage high-frequency alternating current (100V, 200Hz) to realize intercalation, oxidation, expansion and stripping of the graphite powder, then reduce by a constant-voltage (20V) direct electrochemical cathode in another electrolytic tank of alkaline electrolyte containing sodium borohydride reducing agent, and disperse by low-frequency ultrasound, thereby being beneficial to improving the space-time-yield to prepare graphene by the electrochemical method of graphite powder, and having most economic cost and considerable benefit, the method is suitable for large-scale industrial production, and during electrolysis, the electrode structure provided by the embodiment is immersed in the electrolyte.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (8)
1. An electrode structure for preparing graphene by a graphite powder electrochemical method is characterized by comprising two cathode plate groups (100), an anode plate (200) and a U-shaped frame (300);
the U-shaped frame (300) is an insulating part with an upward notch and a through inner groove at the left and right sides, the two cathode plate groups (100) are vertically arranged in the U-shaped frame (300) along the front and back direction and are distributed in the U-shaped frame (300) at intervals along the left and right direction, and the two cathode plate groups (100) and the U-shaped frame (300) jointly enclose to form a groove chamber with an upward notch;
one side, close to each other, of each of the two cathode plate groups (100) is provided with an insulating grid plate (110), each of the two grid plates (110) is provided with a plurality of grid holes (111), and the opening sides of the grid holes (111) in the two grid plates (110) are close to each other;
cathode plates (120) are also arranged in the two cathode plate groups (100);
left and right through flow channels are uniformly distributed on the cathode plate groups (100), the anode plate (200) is vertically clamped between the two cathode plate groups (100) along the front-back direction, and the opening sides of the grid holes (111) in the two grid plates (110) are plugged;
flow dredging holes (210) which penetrate through the anode plate (200) from left to right are uniformly distributed on the anode plate;
the graphite powder is contained in the grid holes (111) in the middle of each grid plate, the rest grid holes are used for filling the graphite powder in an expansion mode, the anode plate (200) is electrically connected with the positive pole of a power supply, and the two cathode plates (120) are electrically connected with the negative pole of the power supply.
2. The electrode structure for preparing graphene by using the graphite powder electrochemical method according to claim 1, wherein a plurality of convex columns (220) extending into the grid holes (111) on the same side are convexly arranged on both sides of the anode plate (200), at least one convex column (220) extends into each grid hole (111), and a drainage hole (210) penetrating the convex column (220) from left to right is arranged at a position corresponding to each convex column (220).
3. The electrode structure for preparing graphene by the graphite powder electrochemical method according to claim 1, wherein the anode plate (200) and the cathode plate (120) are titanium plates, and the surfaces of the anode plate and the cathode plate are coated with ruthenium oxide coatings.
4. The electrode structure for graphene electrochemical preparation by graphite powder according to any one of claims 1 to 3, wherein the cathode plate group (100) further comprises a clamping plate (130) and a diaphragm (140), the clamping plate (130) is an insulating plate;
the cathode plate (120) is arranged on one side of the clamping plate (130), and the grid plate (110) is convexly arranged in the middle of one side, away from the clamping plate (130), of the cathode plate (120);
the clamping plate (130) and the cathode plate (120) are respectively provided with a plurality of through holes, the through holes in the clamping plate (130) are communicated with the through holes in the cathode plate (120) to form the flow distribution channel, and each grid hole (111) is communicated with at least one through hole in the cathode plate (120);
the diaphragm (140) is attached to any one side or two sides of the clamping plate (130), and the diaphragm (140) is used for preventing the graphite powder ingredient from leaking through the flow dredging channel;
the U-shaped frame (300) and the two clamping plates (130) jointly enclose the slot chamber.
5. The electrode structure for preparing graphene by graphite powder electrochemical method according to claim 4, wherein the clamping plate (130) is a PP plate.
6. The electrode structure for preparing graphene by graphite powder electrochemical method according to claim 4, wherein the separator (140) is a PE non-woven velvet fabric layer.
7. The electrode structure for graphene electrochemical preparation by graphite powder according to claim 4, wherein the two cathode plate groups (100) are a first cathode plate group and a second cathode plate group respectively;
the clamping plate (130) of the first cathode plate group is fixedly connected with the left side of the U-shaped frame (300) or integrally formed;
the second cathode plate group is placed in the U-shaped frame (300) and limited in the U-shaped frame (300) or limited in a releasing mode by a limiting piece arranged on the right side of the U-shaped frame (300).
8. The electrode structure for graphene electrochemical preparation by graphite powder according to claim 7, wherein the stopper comprises a plurality of bolts (310);
a plurality of screw holes penetrating through the U-shaped frame (300) from front to back are formed in the right side of the groove wall on the two sides of the U-shaped frame at intervals up and down, the screw holes are located in the same vertical plane, one bolt (310) is installed at each screw hole in a threaded mode, and the threaded end of each bolt (310) faces the inside of the U-shaped frame (300);
the second cathode plate group is arranged in the U-shaped frame (300) and positioned on the left side of the plurality of bolts (310), the bolts (310) are screwed down until the threaded ends of the bolts all extend into the U-shaped frame (300) and stop on the right side of the second cathode plate group to be limited, or the bolts (310) are unscrewed to release the limitation and take the second cathode plate group out of the U-shaped frame (300).
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| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
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2021
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| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
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