CN113249740B - Method for preparing graphene by electrochemical continuous and synchronous stripping and reduction - Google Patents
Method for preparing graphene by electrochemical continuous and synchronous stripping and reduction Download PDFInfo
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Abstract
The invention discloses a method for preparing graphene by electrochemical continuous and synchronous stripping and reduction, which comprises the following steps: 1) Preparing materials; 2) Assembling an electric stripping device; 3) Carrying out electrochemical reaction; 4) The reaction is finished; 5) And (4) continuously reacting. The method can realize simultaneous reduction when the graphene is prepared by electrochemical stripping, the process is a sustainable reaction, the stripping and reduction effectiveness is ensured, the graphene can be prepared by electrochemical continuous stripping and reduction in a large-scale, stable, efficient and low-cost manner, the quality and the energy utilization rate of the obtained graphene are improved, and the method is green, environment-friendly and easy to operate. The invention also discloses a device for realizing electrochemical continuous stripping and reducing preparation of graphene.
Description
Technical Field
The invention relates to a technology for electrochemically reducing graphite oxide and graphene oxide and a technology for continuously and synchronously producing graphene, in particular to a method for preparing graphene by electrochemically continuously and synchronously stripping and reducing.
Background
The preparation of graphene by electrochemical stripping 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 preparation method has the advantages of low cost, rapidness, high efficiency, environmental friendliness and the like, so that the preparation method is favored by the academic and industrial fields in recent years. The stripping in the electrochemical stripping method can generate oxidation reaction while stripping, so that the obtained graphene is mostly high in oxygen content, various functional groups such as carbonyl, carboxyl, hydroxyl and epoxy can be introduced in the oxidation process of the graphite, and the method is especially suitable for mass productionIn the process. There are some reduction methods, which mostly use hydrazine hydrate, high-concentration KOH, naOH, naBH 4 And amines and other chemical strong reducing agents have good reducing effect, but have great harm to the environment and higher requirement on operation. Reduction treatment is generally carried out on the basis of the obtained oxidation product, so that the time period is longer and the cost is higher; is not favorable for mass production and use. If the obtained graphene with high oxygen content can be directly reduced in the stripping process, a large batch of high-quality graphene can be obtained, the time period can be controlled, and the utilization rate of energy is finally improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for preparing the graphene by electrochemical continuous and synchronous stripping and reduction, the method can realize simultaneous reduction when the graphene is prepared by electrochemical stripping, the process is a sustainable reaction, the effectiveness of stripping and reduction is ensured, the graphene can be prepared by electrochemical continuous stripping and reduction in a large scale, stably, efficiently and low cost, the quality and the energy utilization rate of the obtained graphene are improved, and the method is environment-friendly and easy to operate.
The utility model provides a realize that electrochemistry is continuous and synchronous peels off and reduces device of preparation graphite alkene, includes the electrolysis trough, is equipped with electrolyte in the electrolysis trough, is equipped with the graphite oxide or the graphite oxide electrode of spaced filter bag membrane encapsulation, the graphite counter electrode of filter bag membrane encapsulation in the electrolysis trough, and graphite oxide or graphite oxide electrode of filter bag membrane encapsulation are as the negative pole, the graphite counter electrode of filter bag membrane encapsulation is as the positive pole, and wherein the counter electrode comprises graphite and current collector.
The spacing distance between the graphite electrode and the counter electrode is 1-7cm.
The current collector is made of one of an acid-resistant alkali-resistant oxidation corrosion-resistant metal material or graphite.
The filter bag film is made of acid-resistant, alkali-resistant and corrosion-resistant materials.
The single cathode and anode can be used as a monomer, and the monomers can be arrayed
A method for preparing graphene by electrochemical continuous and synchronous stripping and reduction comprises the device for preparing graphene by electrochemical continuous and synchronous stripping and reduction, and comprises the following steps:
1) Preparing materials: preparing a graphite oxide or graphene oxide electrode packaged by a filter bag film, a graphite electrode packaged by the filter bag film, electrolyte, a power supply and an electrolytic cell for later use;
2) Assembling an electric stripping device: graphite oxide or graphene oxide packaged by a filter bag film is used as a cathode, graphite packaged by the filter bag film is used as an anode, the two electrodes are vertically and parallelly immersed in electrolyte, and a gap is arranged between the two electrodes;
3) Electrochemical reaction: switching on a power supply, and setting the voltage to be 1-30V; the electrochemical reaction time is 1-10h;
4) And (3) finishing the reaction: reducing graphite oxide or graphene oxide in the cathode filter bag membrane into reduced graphite or reduced graphene, and performing intercalation stripping on graphite in the anode filter bag membrane to obtain graphite oxide or graphene oxide;
5) And (3) continuous reaction: taking the cathode out to obtain a reduced graphite or reduced graphene product, taking the anode electrode after the reaction in the step 4) as a cathode electrode of the next experiment, simultaneously adding a new anode, namely graphite packaged by the filter bag membrane, repeating the electrochemical reaction in the step 3), obtaining the reduced graphite or reduced graphene at the cathode after the reaction is finished, obtaining graphite oxide or graphene oxide at the anode, and then accumulating and collecting the reduced product obtained by the filter bag membrane for subsequent treatment.
The graphite oxide or the graphene oxide packaged by the filter bag film in the step 1) is one of a graphene stripping substance prepared by an electrochemical stripping method with high oxygen content, graphene oxide, graphite oxide, a mixture of graphite oxide and graphene oxide.
The shape of the graphite packaged by the filter bag film in the step 1) is one of a rod shape, a block shape, a sheet shape and a powder shape, and the graphite material is one of graphite foil, highly oriented pyrolytic graphite, natural crystalline flake graphite and graphite powder.
The filter bag membrane in the step 1) is provided with a pore structure, and is acid-resistant, alkali-resistant and corrosion-resistant.
The power supply in the step 1) is a direct current stabilized power supply.
The interval in the step 2) is 1-7cm.
The shape and the volume of the filter bag membrane are set according to the scale of the raw materials.
Compared with the existing method for reducing graphite oxide (graphene), the method has the following advantages:
1. the neutral aqueous electrolyte is used, and a strong reducing agent which can damage the environment is not used, so that the environment is protected;
2. the stripping and reduction degree of the product can be realized by regulating and controlling voltage and time, and the method is effective and easy to operate;
3. the filter bag membrane limits graphite oxide (graphene) in the filter bag membrane by utilizing a self pore structure, so that collection, transfer and cleaning of products are facilitated, and the electrolyte can be recycled.
4. And the proper electrolyte is selected for carrying out electrochemical stripping on the anode and reducing the product at the same time, so that the yield and the product quality of graphene prepared by an electrochemical stripping method are further improved, and the utilization rate of energy is further improved.
The method can realize simultaneous reduction when the graphene is prepared by electrochemical stripping, the process is a sustainable reaction, the stripping and reduction effectiveness is ensured, the graphene can be prepared by electrochemical continuous stripping and reduction in a large-scale, stable, efficient and low-cost manner, the quality and the energy utilization rate of the obtained graphene are improved, and the method is green, environment-friendly and easy to operate.
Drawings
FIG. 1 is a structural view of an apparatus in an embodiment;
fig. 2 is the graphene product obtained after the example reduction.
Detailed Description
The invention will be described in further detail with reference to the following figures and specific examples, which are not intended to limit the invention.
The embodiment is as follows:
a method for preparing graphene by electrochemical continuous and synchronous stripping and reduction comprises the following steps:
1) Preparing materials: preparing a graphite oxide or graphene oxide electrode packaged by a filter bag film, a graphite electrode packaged by the filter bag film, electrolyte, a power supply and an electrolytic cell for later use;
2) Assembling an electric stripping device: graphite oxide or graphene oxide packaged by a filter bag film is used as a cathode, graphite packaged by the filter bag film is used as an anode, the two electrodes are vertically and parallelly immersed into electrolyte, and a gap is formed between the two electrodes;
3) Electrochemical reaction: the two electrodes are respectively connected with the positive electrode and the negative electrode of a power supply, and the set voltage is 1-30V; the electrochemical reaction time is 1-10h;
4) And (3) finishing the reaction: graphite oxide or graphene oxide in the cathode filter bag membrane is reduced, and graphite in the anode filter bag membrane is stripped;
5) And (3) continuous reaction: taking out the cathode, taking the anode after the reaction in the step 4) as the cathode of the next experiment, simultaneously adding a new anode, namely the graphite electrode packaged by the filter bag membrane, repeating the electrochemical reaction in the step 3), accumulating and collecting the reduced product obtained by the filter bag membrane, and then carrying out subsequent treatment.
The graphite oxide or graphene oxide packaged by the filter bag film in the step 1) is one of an exfoliation substance prepared from graphene, graphene oxide, graphite oxide, a mixture of graphite oxide and graphene oxide by an electrochemical exfoliation method with high oxygen content.
The shape of the graphite packaged by the filter bag film in the step 1) is one of a rod shape, a block shape, a sheet shape and a powder shape, and the graphite material is one of graphite foil, highly oriented pyrolytic graphite, natural crystalline flake graphite and graphite powder.
The filter bag membrane in the step 1) is provided with a pore structure, and is acid-resistant, alkali-resistant and corrosion-resistant.
The power supply in the step 1) is a direct current stabilized power supply.
The interval in the step 2) is 1-7cm.
The shape and volume of the filter bag membrane are set according to the scale of the raw materials.
Specifically, the method comprises the following steps:
example 1:
1) Preparing materials: selecting an exfoliation product of graphene prepared by electrochemical exfoliation of flake graphite as a cathode of a first reaction, and packaging the exfoliation product with a filter bag film for later use; selecting sodium sulfate as an electrolytic solute, and preparing 250 ml of sodium sulfate solution with the concentration of 0.1M as electrolyte; selecting gauze of 500 meshes as a filter bag film; adopting a graphite foil packaged by a filter bag film and a collective flow platinum sheet as a counter electrode, a power supply and an electrolytic tank for standby;
2) Assembling an electric stripping device: 0.1M sodium sulfate electrolyte is put into the electrolytic cell, two electrodes which encapsulate the filter bag membrane are vertically and parallelly immersed into the electrolyte, and a 2cm interval is arranged between the two electrodes; the method comprises the following steps that a stripping product of graphene prepared by electrochemical stripping of flake graphite is used as a cathode and connected with a negative electrode of a power supply, and a graphite foil is used as an anode and connected with a positive electrode of the power supply;
3) Electrochemical reduction: switching on a direct current stabilized power supply, and setting the voltage to be 10V; the reaction time is 6h;
4) And (3) finishing the reaction: the stripping product of the graphene oxide in the cathode filter bag membrane is reduced, and the graphite foil in the anode filter bag membrane is stripped;
5) And (3) continuous reaction: taking out the cathode, taking the anode after the reaction in the step 4) as the cathode of the next experiment, simultaneously adding a new anode, namely the graphite foil and the collective flow which are packaged by the filter bag membrane, repeating the electrochemical reduction reaction in the step 3), accumulating and collecting the reduced products obtained by the filter bag membrane, and then carrying out subsequent treatment.
The oxygen content of the product reduced by the process of this example is shown in Table 1.
TABLE 1
| Oxygen content | |
| Preparation of graphene product by electrochemical stripping of graphite flake | 31.13% |
| After electrochemical reduction | 7.56% |
Example 2:
1) Preparing materials: selecting an exfoliation product of graphene prepared by electrochemical exfoliation of flake graphite as a cathode of a first reaction, and packaging the exfoliation product with a filter bag film for later use; selecting sodium sulfate as an electrolytic solute, and preparing 250 ml of sodium sulfate solution with the concentration of 0.1M as electrolyte; selecting gauze of 500 meshes as a filter bag film; graphite powder packaged by a filter bag membrane and a platinum sheet serving as a collective flow are used as a counter electrode, a power supply and an electrolytic cell are prepared for standby;
2) Assembling an electric stripping device: 0.1M sodium sulfate electrolyte is put into the electrolytic bath, two electrodes which encapsulate the filter bag membrane are vertically and parallelly immersed into the electrolyte, and a 2cm interval is arranged between the two electrodes; the method comprises the following steps that (1) an exfoliation product of graphene prepared by electrochemical exfoliation of flake graphite is used as a cathode and connected with a negative electrode of a power supply, and graphite powder is used as an anode and connected with a positive electrode of the power supply;
3) Electrochemical reduction: switching on a direct current stabilized power supply, and setting the voltage to be 10V; the reaction time is 6h;
4) And (3) finishing the reaction: the stripping product of the graphene oxide in the cathode filter bag membrane is reduced, and the graphite powder in the anode filter bag membrane is stripped;
5) And (3) continuous reaction: taking out the cathode, taking the anode after the reaction in the step 4) as the cathode of the next experiment, simultaneously adding a new anode, namely the graphite powder and the collective flow packaged by the filter bag membrane, repeating the electrochemical reduction reaction in the step 3), accumulating and collecting the reduced products obtained by the filter bag membrane, and then carrying out subsequent treatment.
Claims (10)
1. The utility model provides a realize that electrochemistry is continuous and synchronous peels off and reduces device of preparation graphite alkene, includes the electrolysis trough, is equipped with electrolyte in the electrolysis trough, its characterized in that is equipped with the graphite oxide or the graphite oxide electrode of filter bag membrane encapsulation of interval, filter bag membrane encapsulation in the electrolysis trough, and graphite counter electrode of filter bag membrane encapsulation is as negative pole, filter bag membrane encapsulation graphite counter electrode is as the positive pole, and wherein graphite counter electrode comprises graphite and current collector.
2. The device for realizing electrochemical continuous and synchronous stripping and reduction graphene preparation according to claim 1, wherein the distance between the graphite oxide or graphene oxide electrode and the graphite counter electrode is 1-7cm.
3. The apparatus for electrochemical continuous and synchronous exfoliation and reduction preparation of graphene according to claim 1, wherein the current collector is made of one of metal material or graphite with acid, alkali, oxidation and corrosion resistance.
4. The device for electrochemical continuous and synchronous stripping and reduction for graphene preparation according to claim 1, wherein the material of the filter bag membrane is acid, alkali and corrosion resistant.
5. The apparatus for electrochemical continuous and synchronous exfoliation and reduction to produce graphene according to claim 1, wherein a single anode and cathode is used as a single body, and the single bodies are arranged in an array.
6. A method for preparing graphene by electrochemical continuous and synchronous stripping and reduction, which comprises the device for preparing graphene by electrochemical continuous and synchronous stripping and reduction according to any one of claims 1 to 5, and is characterized by comprising the following steps:
1) Preparing materials: preparing a graphite oxide or graphene oxide electrode packaged by a filter bag film, a graphite electrode packaged by the filter bag film, electrolyte, a power supply and an electrolytic cell for later use;
2) Assembling an electric stripping device: graphite oxide or graphene oxide packaged by a filter bag film is used as a cathode, graphite packaged by the filter bag film is used as an anode, the two electrodes are vertically and parallelly immersed into electrolyte, and a gap is formed between the two electrodes;
3) Electrochemical reaction: switching on a power supply, and setting the voltage to be 1-30V; the electrochemical reaction time is 1-10h;
4) And (3) finishing the reaction: reducing the graphite oxide or graphene oxide in the cathode filter bag membrane into reduced graphite or reduced graphene, and carrying out intercalation stripping on the graphite in the anode filter bag membrane to obtain graphite oxide or graphene oxide;
5) And (3) continuous reaction: taking the cathode out to obtain a reduced graphite or reduced graphene product, taking the anode electrode after the reaction in the step 4) as a cathode electrode of the next experiment, simultaneously adding a new anode, namely graphite packaged by the filter bag membrane, repeating the electrochemical reaction in the step 3), obtaining the reduced graphite or reduced graphene at the cathode after the reaction is finished, obtaining graphite oxide or graphene oxide at the anode, and then accumulating and collecting the reduced product obtained by the filter bag membrane for subsequent treatment.
7. The method for preparing graphene through electrochemical continuous and synchronous stripping and reduction according to claim 6, wherein the graphite oxide or graphene oxide encapsulated by the filter bag film in the step 1) is one of exfoliates, graphene oxide, graphite oxide, a mixture of graphite oxide and graphene oxide, which are used for preparing graphene through an electrochemical stripping method and have high oxygen content.
8. The method for preparing graphene through electrochemical continuous and synchronous exfoliation and reduction according to claim 6, wherein the graphite encapsulated by the filter bag film in the step 1) is one of a rod, a block, a sheet and a powder, and the graphite material is one of graphite foil, highly oriented pyrolytic graphite, natural flake graphite and graphite powder.
9. The method for preparing graphene through electrochemical continuous and synchronous stripping and reduction according to claim 6, wherein the filter bag membrane in step 1) is provided with a pore structure, and is acid-resistant, alkali-resistant and corrosion-resistant.
10. The method for preparing graphene through electrochemical continuous and synchronous stripping and reduction according to claim 6, wherein the power supply in step 1) is a DC stabilized power supply.
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