CN212269468U - Realize annular stripping off device of graphite powder electrochemical method production graphite alkene - Google Patents
Realize annular stripping off device of graphite powder electrochemical method production graphite alkene Download PDFInfo
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Abstract
The utility model discloses a realize annular stripping off device of graphite powder electrochemistry method production graphite alkene, including the electrolysis trough, be equipped with electrolyte in the electrolysis trough, be equipped with annular counter electrode and the support of taking the mesh in the electrolysis trough, annular counter electrode centers on the support, and the filter bag membrane is adorned in the support, is equipped with graphite powder and current collector in the filter bag membrane, and graphite electrode is constituteed to graphite powder and current collector, and wherein graphite electrode and annular counter electrode are concentric, is equipped with the interval between annular counter electrode and the graphite electrode, and the graphite powder upper end in the filter bag membrane is equipped with the heavy object, annular counter electrode and current collector external power supply. The device can realize large-scale, stable, efficient and low-cost electrochemical stripping of graphite powder to produce graphene, improves the graphene yield and stabilizes the stripping current.
Description
Technical Field
The utility model relates to a preparation graphite alkene field specifically is an annular stripping off device who realizes graphite powder electrochemistry method production graphite alkene.
Background
The production of graphene by electrochemical stripping of graphite is a new graphene production technology, and compared with the existing technologies such as a mechanical stripping method, a CVD method, a redox method and the like, the technology has the advantages of low cost, rapidness, high efficiency, environmental friendliness and the like, and is widely concerned and favored by the academic and industrial fields in recent years. However, the yield of graphene obtained by the existing technology for preparing graphene by stripping graphite powder as a raw material is generally low, one important reason is that graphite particles are dispersedly distributed in an electrolyte in the electrical stripping process, and the contact point between the graphite particles and adjacent particles is limited or even zero, so that the graphite particles on the surface of an expanded pellet subjected to electrochemical treatment can rapidly loose contact with the pellet after contacting with the electrolyte, so that the expansion of the pellet stops at a relatively early stage of the process, and the graphite particles can not obtain electrons any more, namely the graphene can not be further generated by an electrochemical stripping method, so that the yield of graphene prepared by electrochemical stripping of graphite powder is greatly reduced, if the graphite particles falling off from an electrode matrix can stay (are limited) on the surface of the graphite electrode matrix, and the conduction of the electron current of a graphite electrode current collector is maintained, therefore, the graphite particles falling off from the electrode substrate can be subjected to electrochemical stripping continuously, so that graphene is continuously generated, and the yield of graphene prepared by electrochemical stripping of graphite is improved finally.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to the not enough of existence among the prior art, provide an annular stripping off device who realizes graphite powder electrochemistry method production graphite alkene. The device can realize large-scale, stable, efficient and low-cost electrochemical stripping of graphite powder to produce graphene, improves the graphene yield and stabilizes the stripping current.
Realize the technical scheme of the utility model is that:
the utility model provides an annular stripping off device of graphite powder electrochemistry method production graphite alkene, which comprises an electrolytic bath, be equipped with electrolyte in the electrolytic bath, be equipped with annular counter electrode in the electrolytic bath and take the support of mesh, annular counter electrode centers on the support, the filter bag membrane is adorned in the support, be equipped with graphite powder and current collector in the filter bag membrane, graphite electrode is constituteed to graphite powder and current collector, wherein graphite electrode and annular counter electrode are concentric, be equipped with the interval between annular counter electrode and the graphite electrode, the graphite powder upper end in the filter bag membrane is equipped with the heavy object, annular counter electrode and current collector external power supply, the pressure that the heavy object applyed for the graphite powder can be regulated and control.
The annular counter electrode is made of corrosion-resistant metal conductive material.
A gap is arranged between the bottom surface of the annular counter electrode and the inner bottom surface of the electrolytic bath.
The filter bag membrane is provided with a pore structure, the material is acid-resistant, alkali-resistant and corrosion-resistant, the pore diameter in the pore structure of the filter bag membrane is smaller than the particle diameter of graphite powder, the filter bag membrane allows electrolyte ions to freely pass through, and graphite powder stripping products are limited to flow, so that the yield of graphene preparation through graphite powder electrochemical stripping is improved.
The current collector is a columnar high-hardness corrosion-resistant conductive material.
The bracket is made of acid-resistant, alkali-resistant and corrosion-resistant materials.
The distance between the annular counter electrode and the graphite electrode is 1-7 cm.
The power supply is one of a direct current stabilized power supply, an alternating current stabilized power supply or a pulse power supply.
The method for producing the graphene by using the annular stripping device for electrochemically producing the graphene by using the graphite powder comprises the following steps:
1) selecting graphite powder materials and particle sizes: selecting one of artificial graphite, natural graphite or recovered waste graphite powder, wherein the particle size of the graphite powder is 50-800 meshes;
2) selecting an electrolyte: selecting one of water system electrolyte, organic electrolyte and ionic liquid;
3) selecting the material and the pore size of the filter bag membrane: selecting the material and mesh number of the filter bag membrane according to the type and property of the electrolyte and the aperture size of the graphite powder raw material;
4) assembling an electric stripping device: filling the electrolyte selected in the step 2) into an electrolytic cell, putting a filter bag membrane filled with graphite powder and a current collector into a support, forming a graphite electrode by the graphite powder and the current collector in the filter bag membrane as an anode or any one of cathodes, taking an annular counter electrode as a counter electrode, vertically immersing the two electrodes into the electrolytic cell filled with the electrolyte, wherein the annular counter electrode is arranged around the periphery of the support, the annular counter electrode and the graphite electrode keep concentric circles, a gap is arranged between the two electrodes, a gap is arranged between the bottom surface of the annular counter electrode and the inner bottom surface of the electrolytic cell, and the two electrodes are connected with the anode and the cathode of a power supply;
5) selecting the weight of a heavy object: determining the weight of an applied weight according to the particle size of the graphite particles and the bulk density of the graphite particles;
6) electrochemical stripping: setting the stripping voltage to be 1-60V and the stripping time to be 1-10h according to the mass and the volume of the graphite powder;
7) and (4) finishing stripping: stripping the graphite powder in the filter bag membrane into graphene slurry, and taking out the graphene slurry in the filter bag membrane for storage.
Compared with the prior art, the technical scheme is as follows:
1. the stable current transmission in the stripping process is maintained by applying external pressure to the graphite powder and using a filter bag film, and the bulk density of the graphite powder can be adjusted;
2. the continuity of stripping current is ensured by utilizing the confinement effect of the filter bag membrane, so that the stripped and fallen part of graphite particles or graphite sheet layers are stripped for the second time, and the yield of graphene is improved;
3. short circuit of the graphene and the graphite particles to the cathode and the anode is avoided, and stripping current is stabilized.
According to the device, graphite particles falling off from the graphite electrode substrate are limited on the surface of the graphite substrate to the greatest extent, and the graphite substrate keeps conduction of electronic current, and the graphite particles falling off can be continuously electrochemically stripped to continuously produce graphene, so that the yield of graphene prepared by graphite powder electrochemistry can be greatly improved, and meanwhile, products are effectively collected.
The device can realize large-scale, stable, efficient and low-cost electrochemical stripping of graphite powder to produce graphene, improves the graphene yield and stabilizes the stripping current.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment;
FIG. 2 is a schematic structural view of a stent in an embodiment;
fig. 3 is an XRD pattern of the exfoliated graphene and graphene standard card of example 1;
fig. 4 is an SEM image of exfoliated graphene in example 1;
fig. 5 is a TEM image of exfoliated graphene in example 2.
In the figure, 1, an electrolytic cell 2, an annular counter electrode 3, a support 4, a current collector 5, graphite powder 6, a filter bag membrane 7, a heavy object 8, a power supply 9 and electrolyte.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific embodiments, but the present invention is not limited thereto.
Example (b):
example 1:
referring to fig. 1 and 2, an annular stripping device for graphene production by a graphite powder electrochemical method comprises an electrolytic cell 1, electrolyte 9 is arranged in the electrolytic cell 1, an annular counter electrode 2 and a support 3 with meshes are arranged in the electrolytic cell 1, the annular counter electrode 2 surrounds the support 3, a filter bag film 6 is sleeved in the support 3, graphite powder 5 and a current collector 4 are arranged in the filter bag film 6, the graphite powder 5 and the current collector 4 form a graphite electrode, the graphite electrode and the annular counter electrode 2 are concentric, a gap is arranged between the annular counter electrode 2 and the graphite electrode, a heavy object 7 is arranged at the upper end of the graphite powder 5 in the filter bag film 6, the annular counter electrode 2 and the current collector 4 are externally connected with a power supply 8, and the heavy object 7 can regulate and control the pressure applied to the graphite powder 5.
The annular counter electrode 2 is made of corrosion-resistant metal conductive material.
A gap is arranged between the bottom surface of the annular counter electrode 2 and the inner bottom surface of the electrolytic bath 1.
The filter bag membrane 6 is provided with a pore structure, the material is acid-resistant, alkali-resistant and corrosion-resistant, the pore diameter in the pore structure of the filter bag membrane 6 is smaller than the particle diameter of the graphite powder 5, the filter bag membrane 6 allows electrolyte ions to freely pass through, and a graphite powder stripping product is limited to flow, so that the yield of graphene preparation through graphite powder electrochemical stripping is improved.
The current collector 4 is a columnar high-hardness corrosion-resistant conductive material.
The bracket 3 is made of acid-resistant, alkali-resistant and corrosion-resistant materials.
The distance between the annular counter electrode 2 and the graphite electrode is 1-7cm, and 3cm is selected in the embodiment.
The power supply 8 is one of a direct current stabilized power supply, an alternating current stabilized power supply or a pulse power supply, and the direct current stabilized power supply is selected in the embodiment.
The method for producing the graphene by using the annular stripping device for producing the graphene by the graphite powder electrochemical method comprises the following steps:
1) selecting a graphite powder 5 material and a particle size: selecting one of artificial graphite, natural graphite or recovered waste graphite powder, wherein the particle size of the graphite powder 5 is 50-800 meshes, and the artificial graphite powder of 80-100 meshes is selected in the embodiment;
2) selecting an electrolyte 9: one of an aqueous electrolyte, an organic electrolyte and an ionic liquid is selected, in this example, 0.1M Na is selected2SO4The aqueous electrolyte of (1);
3) selecting the material and the pore size of the filter bag membrane 6: selecting the material and the mesh number of the filter bag membrane 6 according to the type and the property of the electrolyte 9 and the pore size of the raw material of the graphite powder 5, wherein gauze with the pore size of 200 meshes is selected as the filter bag membrane in the embodiment;
4) assembling an electric stripping device: filling the electrolyte 9 selected in the step 2) into the electrolytic cell 1, putting the filter bag membrane 6 filled with the graphite powder 5 and the current collector 4 into the bracket 3, forming a graphite electrode by the graphite powder 5 and the current collector 4 in the filter bag membrane 6 as any one of an anode or a cathode, taking the annular counter electrode 2 as a counter electrode, vertically immersing the two electrodes into the electrolytic cell 1 filled with the electrolyte 9, wherein the annular counter electrode 2 is arranged around the periphery of the bracket 3, the annular counter electrode 2 and the graphite electrode keep concentric, a gap is arranged between the two electrodes, a gap is arranged between the bottom surface of the annular counter electrode 2 and the inner bottom surface of the electrolytic cell 1, and the two electrodes are connected with the anode and the cathode of the power supply 8;
5) selecting the weight of a heavy object: determining the weight of the weight 7 according to the particle size of the graphite particles and the bulk density of the graphite particles, wherein the weight of the weight 7 is 1.5kg;
6) electrochemical stripping: setting the stripping voltage to be 1-60V and the stripping time to be 1-10h according to the mass and the volume of the graphite powder 5, wherein the stripping voltage is 10V and the stripping time is 3 h;
7) and (4) finishing stripping: stripping the graphite powder in the filter bag membrane 6 into graphene slurry, and taking out the graphene slurry in the filter bag membrane 6 for storage.
The XRD patterns and SEM patterns of the graphene and graphene standard cards exfoliated by the apparatus and method of the present embodiment are shown in fig. 3 and 4, respectively.
Example 2:
the artificial graphite powder with 100-120 meshes is selected in the embodiment.
In this example, 0.1M (NH) was selected4)2SO4The aqueous electrolyte of (1).
The peeling voltage in this example was 10V and the peeling time was 3 hours.
The rest is the same as example 1.
A TEM image of the graphene exfoliated using the apparatus and method of this example is shown in fig. 5.
Example 3:
in this example, 120-140 mesh artificial graphite powder was selected.
In this example, nylon with a pore size of 200 mesh was selected as the filter bag membrane.
The rest is the same as example 1.
Compared with the graphene slurry stripped in the prior art, the graphene slurry stripped in the embodiments 1, 2 and 3 has obviously improved yield.
Claims (7)
1. The utility model provides a realize annular stripping off device of graphite powder electrochemistry method production graphite alkene, including the electrolysis trough, be equipped with electrolyte in the electrolysis trough, its characterized in that, be equipped with annular counter electrode and the support of taking the mesh in the electrolysis trough, annular counter electrode centers on the support, the filter bag membrane of suit in the support, be equipped with graphite powder and current collector in the filter bag membrane, graphite electrode is constituteed to graphite powder and current collector, wherein graphite electrode and annular counter electrode are concentric, be equipped with the interval between annular counter electrode and the graphite electrode, the graphite powder upper end in the filter bag membrane is equipped with the heavy object, annular counter electrode and current collector external power supply.
2. The annular stripping device for producing graphene by the graphite powder electrochemical method according to claim 1, wherein the annular counter electrode is made of a corrosion-resistant metal conductive material.
3. The annular stripping device for realizing graphene production by the graphite powder electrochemical method according to claim 1, wherein a gap is formed between the bottom surface of the annular counter electrode and the inner bottom surface of the electrolytic cell.
4. The annular stripping device for realizing graphene production by graphite powder electrochemical process as claimed in claim 1, wherein the filter bag membrane is provided with a pore structure, the material is acid-resistant, alkali-resistant and corrosion-resistant, and the pore diameter in the pore structure of the filter bag membrane is smaller than the particle size of graphite powder.
5. The annular stripping device for realizing graphene production by a graphite powder electrochemical method according to claim 1, wherein the current collector is a columnar high-hardness corrosion-resistant conductive material.
6. The annular stripping device for realizing the electrochemical production of graphene by graphite powder according to claim 1, wherein the distance between the annular counter electrode and the graphite electrode is 1-7 cm.
7. The annular stripping device for realizing graphene production by using the graphite powder electrochemical method as claimed in claim 1, wherein the power supply is one of a regulated direct current power supply, a regulated alternating current power supply or a pulse power supply.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943181A (en) * | 2020-09-23 | 2020-11-17 | 广西师范大学 | Annular stripping device and stripping method for producing graphene by graphite powder electrochemical method |
| CN113603082A (en) * | 2021-08-11 | 2021-11-05 | 上海浙道新材料技术有限公司 | Electrode structure for preparing graphene by graphite powder electrochemical method |
| CN114804085A (en) * | 2021-01-27 | 2022-07-29 | 河南烯力新材料科技有限公司 | Graphene generation device |
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2020
- 2020-09-23 CN CN202022106266.8U patent/CN212269468U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943181A (en) * | 2020-09-23 | 2020-11-17 | 广西师范大学 | Annular stripping device and stripping method for producing graphene by graphite powder electrochemical method |
| CN114804085A (en) * | 2021-01-27 | 2022-07-29 | 河南烯力新材料科技有限公司 | Graphene generation device |
| CN113603082A (en) * | 2021-08-11 | 2021-11-05 | 上海浙道新材料技术有限公司 | Electrode structure for preparing graphene by graphite powder electrochemical method |
| CN113603082B (en) * | 2021-08-11 | 2022-10-21 | 上海浙道新材料技术有限公司 | Electrode structure for preparing graphene by graphite powder electrochemical method |
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