CN111908459A - Free combination square device for producing graphene by electrically stripping graphite powder and stripping method - Google Patents
Free combination square device for producing graphene by electrically stripping graphite powder and stripping method Download PDFInfo
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- CN111908459A CN111908459A CN202011009991.1A CN202011009991A CN111908459A CN 111908459 A CN111908459 A CN 111908459A CN 202011009991 A CN202011009991 A CN 202011009991A CN 111908459 A CN111908459 A CN 111908459A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 197
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 30
- 239000003792 electrolyte Substances 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 239000011148 porous material Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 69
- 239000010439 graphite Substances 0.000 claims description 69
- 230000007797 corrosion Effects 0.000 claims description 11
- 238000005260 corrosion Methods 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 9
- 238000005868 electrolysis reaction Methods 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002608 ionic liquid Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910021382 natural graphite Inorganic materials 0.000 claims description 3
- 239000005486 organic electrolyte Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- -1 graphite alkene Chemical class 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 2
- 239000011159 matrix material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
The invention discloses a method for producing graphene by electrically stripping graphite powder, which comprises the following steps: 1) selecting a graphite powder material and particle size; 2) selecting an electrolyte; 3) selecting the material and the pore size of the filter bag membrane; 4) selecting the size and number of electrodes; 5) assembling an electric stripping device; 6) selecting the weight of a heavy object; 7) electrochemical stripping; 8) and (5) finishing stripping. The method can realize the large-scale, stable, efficient and low-cost production of graphene by electrochemically stripping graphite powder, improves the yield of the graphene and stabilizes the stripping current. The invention also discloses a free combination square device for producing graphene by electrically stripping graphite powder.
Description
Technical Field
The invention relates to the field of graphene preparation, in particular to a free combination square device and a stripping method for producing graphene by electrically stripping graphite powder.
Background
Graphene is a two-dimensional carbon nanomaterial consisting of carbon atoms in sp hybridized orbitals in a hexagonal honeycomb lattice. Has an ultra-large specific surface area, excellent thermal conductivity, electrical conductivity, mechanical properties and chemical stability, and has recently received extensive attention from academia. The current preparation methods mainly comprise: the method mainly comprises the following steps of taking graphite powder as a raw material to prepare the graphene by stripping, wherein the graphite powder is generally low in yield, because the continuous and sufficient stripping cannot be kept in the electrochemical stripping process, the distribution of graphite particles is discrete, and the contact points of adjacent particles are limited or even zero, so that the expanded graphite particles fall off after the electrochemical stripping process occurs, and the expansion stops at an early stage to cause the incomplete and insufficient stripping. Therefore, the yield of graphene prepared by electrochemically stripping graphite powder is greatly reduced, and if part of the graphite particles falling off from the electrode substrate can be retained (limited) on the surface of the graphite electrode substrate and kept in conduction with the electron current of the graphite electrode current collector, the part of the graphite particles falling off from the electrode substrate can be continuously electrochemically stripped, so that graphene is continuously generated, and finally the yield of graphene prepared by electrochemically stripping graphite is improved. The stripping yield of a single electrolytic cell is low, square electrodes can be freely combined, only one square counter electrode needs to be placed between adjacent combined monomers, the cost is saved during mass production of graphene, meanwhile, the continuity of stripping current is guaranteed by utilizing the limiting effect of a filter bag membrane, and the stripped and fallen part of graphite particles or graphite sheets is subjected to secondary stripping, so that the graphene yield is improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a free combination square device and a stripping method for producing graphene by electrically stripping graphite powder. The method can realize the large-scale, stable, efficient and low-cost production of graphene by electrochemically stripping graphite powder, improves the yield of the graphene and stabilizes the stripping current.
The technical scheme for realizing the invention is as follows:
the utility model provides a square device of independent assortment of graphite powder production graphite alkene is peeled off to electricity, including the electrolysis trough, be equipped with electrolyte in the electrolysis trough, be equipped with square counter electrode in the electrolysis trough and take the support of mesh, be equipped with the filter bag membrane 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, be equipped with the interval between graphite electrode and the square counter electrode, square counter electrode encircles graphite electrode and places, be equipped with the clearance between the bottom surface in square counter electrode and the electrolysis trough, graphite electrode top is equipped with the heavy object and exerts pressure, square counter electrode and current collector external power supply.
The graphite electrode monomer is square, and a plurality of single graphite electrodes and a plurality of square counter electrodes can be combined respectively.
The square counter electrode is made of corrosion-resistant metal conductive material.
The current collector is made of a high-hardness corrosion-resistant conductive material.
The bracket is made of acid-resistant, alkali-resistant and corrosion-resistant materials.
The filter bag membrane is provided with a pore structure, is made of acid-resistant, alkali-resistant and corrosion-resistant materials, has a pore diameter smaller than the particle diameter of graphite powder, allows electrolyte ions to freely pass through the filter bag membrane, enables stripping products to flow in a limited region, and improves the yield of graphene preparation through graphite powder electrochemical stripping.
The weight can adjust the bulk density of the graphite powder, keep the conduction of the electronic current of the graphite electrode current collector, and improve the yield of graphene prepared by electrochemical stripping of the graphite powder.
The distance between the square 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.
A method for producing graphene by electrically stripping graphite powder comprises the freely combined square device for producing graphene by electrically stripping graphite powder, and 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 the pore size of the filter bag membrane according to the type and the property of the electrolyte and the pore size of the graphite powder raw material;
4) selecting the size and number of electrodes: selecting the size, combination mode and number of the electrodes according to the required yield;
5) assembling an electric stripping device: filling the electrolyte selected in the step 2) into an electrolytic cell, filling graphite powder and a current collector into a filter bag membrane, wherein the graphite powder is distributed on two side edges of the current collector, the graphite powder and the current collector in the filter bag membrane form a graphite electrode as any one of an anode or a cathode, immersing a selected number of square counter electrodes into the electrolytic cell filled with the electrolyte, wherein the square counter electrodes are arranged around the periphery of a support, a gap is arranged between the graphite electrode and the square counter electrodes, a gap is arranged between the square counter electrodes and the inner bottom surface of the electrolytic cell, and the graphite electrodes and the square counter electrodes are connected with the anode and the cathode of a power supply;
6) selecting the weight of a heavy object: determining the weight of the applied weight according to the particle size of the graphite particles and the bulk density of the graphite particles;
7) 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;
8) 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.
The power supply in the step 5) is one of a direct current stabilized power supply, an alternating current stabilized power supply or a pulse power supply.
The distance between the graphite electrode and the square counter electrode in the step 5) is 1-7 cm.
Compared with the prior art, the technical scheme is as follows:
1. the continuity of stripping current is ensured by utilizing the limiting effect of the filter bag film and the support, so that the stripped and fallen part of graphite particles or graphite sheets are stripped for the second time, and the yield of graphene is improved;
2. short circuit of the graphene and graphite particles to the positive electrode and the negative electrode is avoided, and stripping current is stabilized;
3. the production scale can be freely combined according to the yield requirement, and the amplification mode has the characteristics of high efficiency and convenience.
According to the method, the graphite particles falling off from the graphite electrode matrix are limited on the surface of the graphite matrix to the greatest extent, and the conduction of the electronic current is kept between the graphite electrode matrix and the graphite matrix, and the graphite particles falling off can be subjected to electrochemical stripping continuously to produce graphene continuously, so that the yield of graphene prepared by graphite powder electrochemistry can be greatly improved, and the product can be effectively collected.
The method can realize the large-scale, stable, efficient and low-cost production of graphene by electrochemically stripping graphite powder, improves the yield of the graphene and stabilizes the stripping current.
Drawings
FIG. 1 is a schematic structural view of example 1;
FIG. 2 is a schematic view of a graphite electrode cross-assembly in example 1;
FIG. 3 is a schematic view showing an array arrangement of a plurality of graphite electrodes and square counter electrodes in example 1 after being combined;
fig. 4 is an XRD pattern of the exfoliated graphene and graphene standard card of example 1;
fig. 5 is an SEM image of exfoliated graphene in example 1;
fig. 6 is a TEM image of exfoliated graphene in example 1.
In the figure, 1, an electrolytic cell 2, a square counter electrode 3, a support 4, a filter bag membrane 5, graphite powder 6, a current collector 7, a power supply 8 and electrolyte.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples, but the invention is not limited thereto.
Example (b):
example 1:
referring to fig. 1, a freely combined square device for producing graphene by electrically stripping graphite powder comprises an electrolytic cell 1, an electrolyte 8 is arranged in the electrolytic cell 1, a square counter electrode 2 and a support 3 with meshes are arranged in the electrolytic cell 1, a filter bag membrane 4 is arranged in the support 3, graphite powder 5 and a current collector 6 are arranged in the filter bag membrane 4, a graphite electrode is composed of the graphite powder 5 and the current collector 6, a weight is arranged at the top of the graphite electrode to apply pressure, as shown in fig. 2 and 3, the square counter electrode 2 can be arranged at two sides or around the graphite electrode, the graphite electrode can be in a single or cross combination form, the square counter electrode 2 and the graphite electrode arranged around the graphite electrode can be used as a single body to perform contact type array arrangement, when the square counter electrode 2 and the graphite electrode arranged around the graphite electrode are used as a single body to perform contact type array arrangement, the contact part between the adjacent monomers only needs to be provided with one square counter electrode 2, so that the cost is saved during the batch production of the graphene.
The graphite electrode monomer is square, and a plurality of the graphite electrode monomers and the square counter electrode 2 can be combined respectively.
The square counter electrode 2 is made of corrosion-resistant metal conductive material.
The current collector 6 is made of a high-hardness corrosion-resistant conductive material.
The bracket 3 is made of acid-resistant, alkali-resistant and corrosion-resistant materials.
The filter bag membrane 4 is provided with a pore structure, is made of acid-resistant, alkali-resistant and corrosion-resistant materials, has a pore diameter smaller than the particle diameter of the graphite powder 5 in the pore structure of the filter bag membrane, allows electrolyte ions to freely pass through the filter bag membrane 4, enables the stripping product to flow in a limited area, and improves the yield of graphene preparation through electrochemical stripping of the graphite powder.
The weight can adjust the bulk density of the graphite powder 5, keep conduction with the electronic current of a current collector in the graphite electrode, and improve the yield of graphene prepared by electrochemical stripping of the graphite powder.
The distance between the square counter electrode 2 and the graphite electrode is 1-7 cm.
The power supply 7 is one of a direct current stabilized power supply, an alternating current stabilized power supply or a pulse power supply.
A method for producing graphene by electrically stripping graphite powder comprises the freely combined square device for producing graphene by electrically stripping graphite powder, and 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 with the particle size of 160-200 meshes is adopted in the embodiment;
2) selecting an electrolyte solution 8: selecting one of water-based electrolyte, organic electrolyte and ionic liquid, in this example, selecting 0.1M Na2SO4 water-based electrolyte;
3) selecting the material and the pore size of the filter bag membrane 4: selecting the material and pore size of the filter bag membrane 4 according to the type and property of the electrolyte 8 and the pore size of the raw material of the graphite powder 5, and selecting 300-mesh gauze as the filter bag membrane in the embodiment;
4) selecting the size and number of electrodes: selecting the size, combination mode and number of electrodes according to the required yield, and carrying out contact array arrangement and combination by taking the square counter electrodes on the periphery of the graphite electrodes and the graphite electrodes as a monomer, wherein the embodiment selects a combination of two rows and three columns of six monomers in total;
5) assembling an electric stripping device: filling the electrolyte 8 selected in the step 2) into an electrolytic tank 1, filling graphite powder 5 and a current collector 6 into a filter bag membrane 4, wherein the graphite powder 5 is distributed on two side edges of the current collector 6, the graphite electrode consisting of the graphite powder 5 and the current collector 6 in the filter bag membrane 4 is used as any one of an anode and a cathode, immersing a selected number of square counter electrodes 2 into the electrolytic tank 1 filled with the electrolyte 8, wherein the square counter electrodes 2 are placed around the periphery of a support 3, a gap is arranged between each graphite electrode and the corresponding square counter electrode 2, a gap is arranged between each square counter electrode 2 and the inner bottom surface of the electrolytic tank 1, and the graphite electrodes and the square counter electrodes 2 are connected with the anode and the cathode of a power supply 7;
6) selecting the weight of a heavy object: determining the weight of the applied weight according to the particle size of the graphite particles and the bulk density of the graphite particles, wherein 2kg of the applied weight is selected for each graphite electrode monomer;
7) electrochemical stripping: according to the mass and the volume of the graphite powder 5, the stripping voltage is set to be 1-60V, the stripping time is 1-10h, the stripping voltage is set to be 10V, and the stripping time is 4 h;
8) and (4) finishing stripping: stripping the graphite powder in the filter bag membrane 4 into graphene slurry, and taking out the graphene slurry in the filter bag membrane for storage.
The power supply 7 in the step 5) 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 distance between the graphite electrode and the square counter electrode 2 in the step 5) is 1-7cm, and 2cm is selected in the embodiment.
The XRD, SEM and TEM images of the graphene and graphene standard card exfoliated by the apparatus and method of the present example are shown in fig. 4, 5 and 6, respectively.
Example 2:
the artificial graphite powder with 160-200 meshes is selected in the embodiment.
This example selects 0.1M K2SO4The aqueous electrolyte of (1).
In this example, 300 mesh nylon cloth was selected as the filter bag membrane.
The rest is the same as example 1.
Example 3:
in this example, the stripping voltage was 8V and the stripping time was 6 h.
The rest is the same as example 1.
Claims (8)
1. The utility model provides a square device of independent assortment of graphite powder production graphite alkene is peeled off to electricity, including the electrolysis trough, be equipped with electrolyte in the electrolysis trough, a serial communication port, be equipped with square counter electrode in the electrolysis trough and take the support of mesh, be equipped with the filter bag membrane 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, be equipped with the interval between graphite electrode and the square counter electrode, square counter electrode encircles graphite electrode and places, be equipped with the clearance between the bottom surface in square counter electrode and the electrolysis trough, graphite electrode top is equipped with the heavy object and exerts pressure, square counter electrode and current collector external power supply.
2. The freely combined square device for realizing the production of graphene by electrically stripping graphite powder as claimed in claim 1, wherein the graphite electrode monomer is square, and a plurality of single graphite electrodes and a plurality of square counter electrodes can be combined respectively.
3. The freely-combined square device for realizing the production of graphene by electrically stripping graphite powder as claimed in claim 1, wherein the square counter electrode is made of corrosion-resistant metal conductive material.
4. The square device of claim 1, wherein the filter bag membrane has a pore structure, the material of the filter bag membrane is acid, alkali and corrosion resistant, and the pore diameter of the filter bag membrane pore structure is smaller than the particle size of the graphite powder.
5. The free-combination square device for realizing the production of graphene by electrically stripping graphite powder as claimed in claim 1, wherein the current collector is a high-hardness and corrosion-resistant conductive material.
6. The freely-combined square device for realizing the production of graphene by electrically stripping graphite powder according to claim 1, wherein the distance between the square counter electrode and the graphite electrode is 1-7 cm.
7. A method for producing graphene by electrically stripping graphite powder, which is characterized by comprising a free-combination square device for realizing the production of graphene by electrically stripping graphite powder according to any one of claims 1 to 6, wherein the method 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 the pore size of the filter bag membrane according to the type and the property of the electrolyte and the pore size of the graphite powder raw material;
4) selecting the size and number of electrodes: selecting the size, combination mode and number of the electrodes according to the required yield;
5) assembling an electric stripping device: filling the electrolyte selected in the step 2) into an electrolytic cell, filling graphite powder and a current collector into a filter bag membrane, wherein the graphite powder is distributed on two side edges of the current collector, the graphite powder and the current collector in the filter bag membrane form a graphite electrode as any one of an anode or a cathode, immersing a selected number of square counter electrodes into the electrolytic cell filled with the electrolyte, wherein the square counter electrodes are arranged around the periphery of a support, a gap is arranged between the graphite electrode and the square counter electrodes, a gap is arranged between the square counter electrodes and the inner bottom surface of the electrolytic cell, and the graphite electrodes and the square counter electrodes are connected with the anode and the cathode of a power supply;
6) selecting the weight of a heavy object: determining the weight of the applied weight according to the particle size of the graphite particles and the bulk density of the graphite particles;
7) 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;
8) 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.
8. The method for producing graphene by electrically stripping graphite powder as claimed in claim 7, wherein the power supply in step 5) is one of a regulated dc power supply, a regulated ac power supply or a pulse power supply.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113481520A (en) * | 2021-07-28 | 2021-10-08 | 上海大学 | Anode structure for preparing graphene by electrolytic oxidation method |
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| CN108862254A (en) * | 2018-07-12 | 2018-11-23 | 西安交通大学 | A kind of method that the bipolar electrode removing of electrochemistry yin-yang prepares graphene |
| WO2020105646A1 (en) * | 2018-11-21 | 2020-05-28 | 学校法人工学院大学 | Method for producing graphene, and graphene production equipment |
| CN212403474U (en) * | 2020-09-23 | 2021-01-26 | 广西师范大学 | Free combination square device for producing graphene by electrically stripping graphite powder |
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2020
- 2020-09-23 CN CN202011009991.1A patent/CN111908459A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104768871A (en) * | 2012-10-24 | 2015-07-08 | 独立行政法人物质·材料研究机构 | Ultrathin graphene piece, manufacturing device for ultrathin graphene piece, manufacturing method for ultrathin graphene piece, capacitor, and manufacturing method for capacitor |
| CN108862254A (en) * | 2018-07-12 | 2018-11-23 | 西安交通大学 | A kind of method that the bipolar electrode removing of electrochemistry yin-yang prepares graphene |
| WO2020105646A1 (en) * | 2018-11-21 | 2020-05-28 | 学校法人工学院大学 | Method for producing graphene, and graphene production equipment |
| CN212403474U (en) * | 2020-09-23 | 2021-01-26 | 广西师范大学 | Free combination square device for producing graphene by electrically stripping graphite powder |
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| CN113481520A (en) * | 2021-07-28 | 2021-10-08 | 上海大学 | Anode structure for preparing graphene by electrolytic oxidation method |
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