CN212559475U

CN212559475U - Device for preparing graphene

Info

Publication number: CN212559475U
Application number: CN202021241587.2U
Authority: CN
Inventors: 曹浩; 陈杰; 裴晓东; 骆艳华; 杨修光; 张玲; 汤凤林; 朱叶峰
Original assignee: Sinosteel Nanjing New Material Research Institute Co Ltd; Sinosteel New Materials Co Ltd
Current assignee: Sinosteel Nanjing New Material Research Institute Co Ltd
Priority date: 2020-06-30
Filing date: 2020-06-30
Publication date: 2021-02-19
Anticipated expiration: 2030-06-30

Abstract

The utility model discloses a device for preparing graphene, which relates to the technical field of inorganic material preparation, and aims to solve the problems that the device for preparing graphene by an electrolytic method needs a high-price electrode and the stability of the electrode and graphite paper is influenced after a stirring device is additionally arranged; the utility model comprises an electrolytic cell, a bracket is arranged at the lower end of the electrolytic cell, a discharge port is arranged in the middle of the lower end of the electrolytic cell, a group of electrode clamps capable of clamping graphite paper are arranged above the electrolytic cell near the two sides, the electrode clamps are fixedly connected with the electrolytic cell, electrodes capable of contacting with the graphite paper are fixedly arranged at the inner sides of the electrode clamps, a group of driving rollers for conveying the graphite paper are arranged below each group of electrode clamps, a supporting table is fixedly arranged at the position near the two groups of driving rollers in the electrolytic cell, and a stirring sheet is arranged between each supporting table and the bottom end in the electrolytic cell; the utility model discloses can prevent effectively that graphite paper from breaking off under the complete condition of not electrolyzing because of reasons such as gravity or flow and coming off, and can use the copper electrode, practice thrift the cost.

Description

Device for preparing graphene

Technical Field

The utility model relates to an inorganic material preparation technical field specifically is a device of preparation graphite alkene.

Background

The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future; the low-cost large-scale preparation of the high-quality graphene is a key technical problem which needs to be solved by exerting excellent electric conduction and heat conduction characteristics of the graphene and promoting the graphene to be applied to the fields of electric heating, sensing, energy storage and the like. The most important technical route for preparing high-quality graphene is to take cheap graphite as a raw material and perform intercalation and stripping between graphite layers. For the technical route, high quality is the premise of realizing various applications of the preparation method, and the environmental protection and safety of a preparation system and a preparation process are considered; the preparation of graphene by an electrolytic method is widely concerned due to the characteristics of rapidness, relative environmental friendliness and the like.

At present, an electrolytic electrode is usually required to be immersed in an electrolyte solution by a commercial electrolytic graphene preparation device, but since the electrolyte solution for electrolyzing graphene is an acidic ammonium sulfate-ammonia water solution, a general electrolytic electrode can be decomposed, for example, a copper electrode, only titanium, platinum or platinum-plated titanium with higher price can be used as the electrode, so that the production cost is increased; in addition, the flowing electrolyte can accelerate the electrolysis speed, but the graphene preparation device by the electrolytic method on the market only stays at the position of the additionally-arranged stirring device, and the electrode stability in the electrolyte can be influenced during stirring, and the unsupported graphite paper is easy to break, so that incomplete stripping is caused, raw materials are wasted, and the production cost is indirectly increased.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide a device of preparation graphite alkene to the device of solving electrolysis preparation graphite alkene needs the higher electrode of price, and can influence the stable problem of electrode and graphite paper after installing agitating unit additional.

In order to achieve the above object, the utility model provides a following technical scheme: the utility model provides a device of preparation graphite alkene, including the electrolysis trough, its lower extreme is provided with the support, the middle part of electrolysis trough lower extreme is provided with the discharge gate, the electrolysis trough is close to the top of both sides department and all is provided with a set of electrode holder that can carry graphite paper, its and electrolysis trough fixed connection, the inboard of electrode holder sets firmly can with the electrode of graphite paper contact, the below of every electrode holder of group is provided with a set of driving roller that is used for carrying graphite paper, nearly two sets of driving roller department fixed mounting respectively has a brace table in the electrolysis trough, be provided with a stirring piece between each brace table and the inside bottom of electrolysis trough.

Preferably, the electrode clamp comprises a first vertical clamping plate, a second vertical clamping plate and an electrode, wherein the second clamping plate and the electrode are parallel to the first clamping plate, the electrode is located between the first clamping plate and the second clamping plate and fixedly connected with the second clamping plate, four corners of the first clamping plate and the second clamping plate are provided with connecting holes for penetrating through bolts, and the two clamping plates are fixedly connected with the bolts at the four corners.

Preferably, the electrodes of the two groups of electrode clamps are respectively connected with the positive electrode and the negative electrode of the same power supply.

Preferably, a horizontal first fixing rod is arranged above the middle part of the electrolytic cell, a plurality of second fixing rods are fixedly arranged at the lower end of the first fixing rod, the lower ends of the second fixing rods are fixedly connected with the upper end of the wall of the electrolytic cell, and the two groups of electrode fixtures are fixedly arranged at two ends of the first fixing rod respectively.

Preferably, the driving roller at least comprises a driving roller, a driven roller I and a driven roller II, wherein the driving roller is positioned at one side close to the middle part of the electrolytic cell under the electrode clamp; the first driven roller is positioned on one side, far away from the middle part of the electrolytic bath, below the driving roller, the connecting line of the first driven roller and the center of the driving roller forms an included angle of 45 degrees with the horizontal plane, and the distance between the first driven roller and the driving roller is equal to the thickness of the graphite paper; the second driven roller is positioned on one side of the support platform far away from the middle part of the electrolytic bath, and the upper end of the second driven roller and the upper end of the support platform are positioned in the same horizontal plane.

Preferably, the lower end of the electrolytic cell is provided with two motors which are respectively in transmission connection with the two stirring sheets.

Preferably, the electrode is a copper electrode.

Preferably, the support platform is made of an insulating material, and a plurality of vent holes are formed in the support platform and penetrate through the support platform in the vertical or horizontal direction.

Preferably, a plurality of air pipes are arranged outside the electrolytic cell, the air outlet ends of the air pipes are communicated with the electrolytic cell and arranged below the supporting table, and the air inlet ends of the air pipes are provided with air pumps and air valves for supplying air.

Compared with the prior art, the beneficial effects of the utility model are that:

1. this device of preparation graphite alkene adopts the stirring and ventilates and makes electrolyte flow, is provided with the brace table simultaneously, can prevent effectively that graphite paper from breaking off under the complete condition of not electrolyzing because of reasons such as gravity or flow and droing, therefore can not cause the waste of raw materials, practices thrift manufacturing cost and improved the productivity.

2. According to the device for preparing the graphene, the electrode does not need to be immersed in the acidic electrolyte, so that a common copper material electrode can be used, the device is easy to purchase and low in price compared with a commonly used platinum or titanium material electrode, the production cost is saved, and meanwhile, when the stirring device is used for stirring the electrolyte, the electrode cannot shake.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

In the figure: 1. an electrolytic cell; 11. a support; 12. a discharge port; 2. an electrode holder; 21. a first clamping plate; 22. a second clamping plate; 23. an electrode; 24. fixing a rod I; 25. a second fixing rod; 3. graphite paper; 4. a drive roll; 41. a driven roller I; 42. a driven roller II; 5. a support table; 6. a stirring sheet; 61. a motor; 7. the trachea.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

As shown in figure 1, a device for preparing graphene comprises an electrolytic tank 1, a bracket 11 is arranged at the lower end of the electrolytic tank 1, a discharge port 12 is arranged in the middle of the lower end of the electrolytic tank 1, the discharge port 12 can be opened for blanking after electrolysis, a group of electrode clamps 2 capable of clamping graphite paper 3 are arranged above the electrolytic tank 1 close to two sides, the electrode clamps 2 can be of a structure comprising a first vertical clamping plate 21, a second clamping plate 22 and an electrode 23, the electrode 23 is not in the electrolytic tank 1, and can realize electrolysis without being in electrolyte due to good conductivity of graphite, so that a copper electrode can be used, the device is easy to purchase and cheap, the first clamping plate 22 and the electrode 23 are parallel to the first clamping plate 21, the electrode 23 is positioned between the first clamping plate 21 and the second clamping plate 22 and fixedly connected with the second clamping plate 22, and connecting holes for passing through bolts are arranged at four corners of the first clamping plate 21 and the second clamping plate 22, the electrode clamps 2 can also be other equivalent replacement structures, the function of the electrode clamps is to enable the electrodes 23 to be in close contact with the graphite paper 3 when the graphite paper 3 is clamped, and the electrodes 23 of the two groups of electrode clamps 2 are respectively connected with the positive pole and the negative pole of the same power supply to form a loop; the two groups of electrode clamps 2 are fixedly connected with the electrolytic cell 1 in a manner that a horizontal fixing rod I24 is arranged above the middle part of the electrolytic cell 1, a plurality of fixing rods II 25 are fixedly arranged at the lower end of the horizontal fixing rod I, the lower ends of the fixing rods II 25 are fixedly connected with the upper end of the cell wall of the electrolytic cell 1, the two groups of electrode clamps 2 are respectively and fixedly arranged at two ends of the fixing rod I24, and the two groups of electrode clamps can also be in other structures with the same effect as long as the positions of the electrode clamps 2 can be fixed; a supporting table 5 is fixedly arranged in the electrolytic cell 1 close to the two groups of driving rollers respectively, the mounting mode can be as shown in the figure, a block-shaped connecting piece is arranged in the middle of the lower end of the supporting table and is connected by adopting a buckle or a bolt, a stirring sheet 6 is arranged between each supporting table 5 and the bottom end in the electrolytic cell 1, two motors 61 can be arranged at the lower end of the electrolytic cell 1 and are in transmission connection with the two stirring sheets 6 respectively, the motors 61 are preferably servo motors capable of regulating speed and rotating forward and backward, if the electrolytic cell 1 is larger, a three-phase asynchronous motor provided with a speed reducing mechanism and a forward and backward rotation relay can be used, and only one motor 61 can be used for driving the two stirring sheets 6 through a belt wheel or other; a plurality of air pipes 7 can be arranged outside the electrolytic cell 1, the air outlet ends of the air pipes 7 are communicated with the electrolytic cell 1 and are arranged below the support table 5, the air inlet ends of the air pipes 7 are provided with air pumps and air valves for supplying air, the electrolyte flows by utilizing air and stirring, the stripping speed of the graphene can be accelerated, the support table 5 can ensure that the graphite paper 3 is not easy to be broken due to the influence of gravity, stirring and the like, the support table 5 is made of insulating materials such as polytetrafluoroethylene, alumina and the like, a plurality of air holes are arranged on the support table 5, and the air holes penetrate through the support table 5 in the vertical or horizontal direction, so that the air supplied by the air pipes 7 can pass through the air pipes, the; the below of every group electrode holder 2 is provided with a set of driving roller that is used for carrying graphite paper 3, and the driving roller can be as follows structure: the electrolytic cell at least comprises a driving roller 4, a driven roller I41 and a driven roller II 42, wherein the driving roller 4 is positioned on one side close to the middle part of the electrolytic cell 1 under the electrode clamp 2; the first driven roller 41 is positioned on one side, far away from the middle part of the electrolytic bath 1, below the driving roller 4, the included angle between the connecting line of the first driven roller 41 and the center of the driving roller 4 and the horizontal plane is 45 degrees, and the distance between the first driven roller 41 and the driving roller is equal to the thickness of the graphite paper 3; the second driven roller 42 is positioned on one side of the support table 5 far away from the middle part of the electrolytic cell 1, the upper end of the second driven roller 42 and the upper end of the support table 5 are positioned in the same horizontal plane, and the driving roller can also adopt other structures as long as the graphite paper 3 vertically downward at the electrode clamp 2 can be conveyed to the lower part of the electrode clamp and is changed into a horizontal direction towards the middle part of the electrolytic cell 1.

The working principle is as follows:

the bolts of the two groups of electrode clamps 2 are all loosened, the two rolls of graphite rolls are installed on the unreeling machine, the graphite paper 3 of the two rolls of graphite rolls is respectively conveyed to the two support tables 5 in the electrolytic bath 1 through the two groups of electrode clamps 2 and the driving rollers, the bolts of the electrode clamps 2 are all screwed down, so that the two electrodes 23 are completely contacted with the graphite paper 3, the power supply is turned on to start electrolysis, meanwhile, the stirring sheet 6 is rotated and stirred, and the air pipe 7 is ventilated; after the electrolysis is finished, the product slowly settles at the discharge port 12, and at the moment, the discharge port 12 is opened to discharge the slurry.

Example (b):

firstly, adding a proper amount of electrolyte into an electrolytic cell 1, wherein the electrolyte amount is higher than that of the electrolytic cell by about 1cm just after the support table 5 is completely soaked, feeding the graphite paper 3 into the electrolytic cell 1 through a driving roller, and increasing or decreasing the electrolyte according to the situation, so that only the horizontal part of the graphite paper 3 on the support table 5 is soaked in the electrolyte as far as possible to prevent the graphite roll from being broken; all the bolts of the electrode clamp 2 are screwed down to make the graphite paper 3 tightly contact with the electrode 23; controlling the gas outlet rate of the gas pipe 7 to be about 500sccm, initially controlling the electrolytic voltage to be about 3V to 3.5V, controlling the rotating speed of the stirring sheet to be about 100rpm to 200rpm, increasing the voltage to be about 6V to 6.5V after 1h to 2h, controlling the rotating speed of the stirring sheet to be about 500pm to 1000rpm, keeping the graphite paper 3 on the support table 5 to completely fall off, completing electrolysis, standing for 1h, opening the discharge port 12, and discharging a product.

The above is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention should be covered by the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.

The parts of the present invention not described in detail are the known techniques of those skilled in the art.

Claims

1. The utility model provides a device of preparation graphite alkene, includes electrolysis trough (1), and its lower extreme is provided with support (11), and the middle part of electrolysis trough (1) lower extreme is provided with discharge gate (12), its characterized in that: the utility model discloses a graphite paper, including electrolysis trough (1), the top that is close to both sides department all is provided with a set of electrode holder utensil (2) that can clip graphite paper (3), it and electrolysis trough (1) fixed connection, the inboard of electrode holder utensil (2) has set firmly electrode (23) that can contact with graphite paper (3), the below of every electrode holder utensil of group (2) is provided with a set of driving roller that is used for carrying graphite paper (3), close two sets of driving roller departments of electrolysis trough (1) interior fixed mounting respectively has one to prop up supporting bench (5), be provided with one stirring piece (6) between each supporting bench (5) and the inside bottom of electrolysis trough (1).

2. The apparatus for preparing graphene according to claim 1, wherein: electrode holder (2) include vertical splint one (21), splint two (22) and electrode (23), wherein splint two (22) and electrode (23) all are parallel with splint one (21), electrode (23) are located between splint one (21) and splint two (22) and with splint two (22) fixed connection, the four corners of splint one (21) and splint two (22) all are provided with the connecting hole that is used for passing the bolt, the two bolt fixed connection through the four corners.

3. The apparatus for preparing graphene according to claim 1, wherein: the electrodes (23) of the two groups of electrode clamps (2) are respectively connected with the positive and negative electrodes of the same power supply.

4. The apparatus for preparing graphene according to claim 1, wherein: a horizontal first fixing rod (24) is arranged above the middle of the electrolytic cell (1), a plurality of second fixing rods (25) are fixedly arranged at the lower end of the first fixing rod, the lower ends of the second fixing rods (25) are fixedly connected with the upper end of the cell wall of the electrolytic cell (1), and the two groups of electrode fixtures (2) are fixedly arranged at two ends of the first fixing rods (24) respectively.

5. The apparatus for preparing graphene according to claim 1, wherein: the driving rollers at least comprise a driving roller (4), a driven roller I (41) and a driven roller II (42), wherein the driving roller (4) is positioned on one side, close to the middle part of the electrolytic cell (1), under the electrode clamp (2); the driven roller I (41) is positioned on one side, far away from the middle part of the electrolytic bath (1), below the driving roller (4), the connecting line of the driven roller I (41) and the center of the driving roller (4) forms an included angle of 45 degrees with the horizontal plane, and the distance between the driven roller I and the driving roller I is equal to the thickness of the graphite paper (3); the driven roller II (42) is positioned on one side of the support platform (5) far away from the middle part of the electrolytic tank (1), and the upper end of the driven roller II (42) and the upper end of the support platform (5) are positioned in the same horizontal plane.

6. The apparatus for preparing graphene according to claim 1, wherein: the lower end of the electrolytic cell (1) is provided with two motors (61) which are respectively in transmission connection with the two stirring sheets (6).

7. The apparatus for preparing graphene according to claim 1, wherein: the electrode (23) is a copper electrode.

8. The apparatus for preparing graphene according to claim 1, wherein: the supporting platform (5) is made of insulating materials, a plurality of vent holes are formed in the supporting platform, and the vent holes penetrate through the supporting platform (5) in the vertical or horizontal direction.

9. The apparatus for preparing graphene according to any one of claims 1 to 8, wherein: a plurality of air pipes (7) are arranged outside the electrolytic cell (1), the air outlet ends of the air pipes (7) are communicated with the electrolytic cell (1) and are arranged below the supporting table (5), and air pumps and air valves for supplying air are arranged at the air inlet ends of the air pipes (7).