CN115448302B - Method for preparing graphene oxide based on pressure regulation and continuous electrolysis - Google Patents
Method for preparing graphene oxide based on pressure regulation and continuous electrolysis Download PDFInfo
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Abstract
The invention belongs to the field of graphene oxide material preparation, and particularly relates to a method for preparing graphene oxide based on pressure regulation and continuous electrolysis. Graphite with a macroscopic continuous structure is used as a raw material and is used as a reaction anode, the reaction anode and the reaction cathode which are soaked in electrolyte are electrified, and the reaction anode sequentially performs intercalation reaction and oxidation reaction in a high-pressure area and a low-pressure area under the space limitation and extrusion of a conveying device. And stripping and cleaning the anode material after the oxidation reaction is completed to obtain the graphene oxide material. The method has the advantages of continuity, high efficiency, green, low cost and the like, and can be used for large-scale preparation of the graphene oxide material.
Description
Technical Field
The invention belongs to the field of graphene oxide material preparation, and particularly relates to a method for preparing graphene oxide based on pressure regulation and continuous electrolysis.
Background
Graphene oxide is an important derivative of graphene, and can be used as a precursor for preparing graphene, and meanwhile, the graphene oxide has good assemblability and dispersibility due to the existence of oxygen-containing functional groups. Graphene oxide has important applications in transparent conductive films, printed electronics, electrochemical capacitors, lithium batteries, polymer composites, and the like.
Currently, chemical oxidation methods typified by Hummers method are commonly used for preparing graphene oxide. In recent years, researchers have developed preparation processes such as electrochemical stripping of graphite, dry ball milling, ultrasonic treatment, and the like. Among the preparation methods, the chemical oxidation method is the most studied, and the chemical oxidation method is a preparation method for oxidizing and stripping graphite raw materials by using strong oxidizing agents such as potassium permanganate, potassium chlorate and the like. Graphene oxide prepared by a chemical oxidation method has high oxidation degree and stripping degree, is a main mode of the current large-scale preparation, but the strong oxidant introduced by the chemical oxidation method brings serious pollution to the environment, meanwhile, the preparation process has the risk of explosion, a large amount of water is required to be consumed in the cleaning process, and the problems are difficult to be effectively solved for many years. Electrochemical methods are considered to be the most likely alternative to chemical oxidation methods for the large-scale preparation of graphene oxide.
Unlike traditional chemical process, the electrochemical process for preparing graphene oxide does not use strong oxidant, and has the characteristics of green and environment protection. At present, graphene oxide prepared by a one-step electrochemical method generally has the problems of poor oxidation effect and insufficient stripping. The oxidation effect of graphene oxide can be remarkably improved by a two-step electrochemical method of pre-intercalation of graphite raw materials, and the effect of the traditional chemical oxidation method can be achieved, but the two-step electrochemical method of intercalation and oxidation is complex in process, the intercalation agent and the oxidant can be polluted with each other, the device is complex to realize, and industrial continuous production is difficult to realize. Thus, there is a need for an electrochemical process that combines both oxidation and simple manufacturing processes.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing graphene oxide based on pressure regulation and continuous electrolysis, which can realize continuous, efficient, green and low-cost preparation of graphene oxide materials by carrying out space limitation and pressure control on graphite raw materials in the conveying process and sequentially carrying out intercalation and oxidation reactions in a high-pressure area and a low-pressure area.
A method for preparing graphene oxide based on pressure regulation continuous electrolysis takes graphite with a macroscopic continuous structure as a raw material, and is used as a reaction anode, the reaction anode and a reaction cathode which are soaked in electrolyte are electrified, and the reaction anode sequentially carries out intercalation reaction and oxidation reaction in a high-pressure area and a low-pressure area under the space limitation and extrusion of a conveying device. Stripping and cleaning the anode material after the oxidation reaction is completed to obtain a graphene oxide material;
the device for realizing the method comprises a reaction anode 1, a conductive roller 2, a power supply 3, a guide roller 4, a reaction cathode 5, two groups of conveyor belts 6, a first roller group 7, a second roller group 8, a third roller group 9 and electrolyte 10, and has the following specific structure: the reaction anode 1 is wound on the conductive roller 2, one end of the reaction anode 1 is immersed in electrolyte 10, passes through between two groups of conveying belts 6, the two groups of conveying belts 6 are parallel and reversely rotated to enable the reaction anode 1 to be conveyed rightwards, the conveying belts 6 are sleeved on the guide rollers 4 and pass through a first roller group 7, a second roller group 8 and a third roller group 9, the first roller group 7, the second roller group 8 and the third roller group 9 respectively squeeze the conveying belts, the first roller group 7 and the second roller group 8 enable the left side of the conveying belts 6 to form a high-pressure area, the second roller group 8 and the third roller group 9 enable the right side of the conveying belts 6 to form a low-pressure area, the reaction cathode 5 is immersed in the electrolyte 10 and is placed on two sides of the reaction anode 1 in parallel, and the conductive roller 2 and the reaction cathode 5 are respectively connected on the positive electrode and the negative electrode of the power supply 3 through wires.
According to the method for preparing graphene oxide based on pressure regulation and continuous electrolysis, the graphite raw material with a macroscopic continuous structure is a sheet, a wire, a bar and a plate prepared from one or more than two of natural graphite, artificial graphite, blocky graphite, crystalline flake graphite, aphanitic graphite, expanded graphite or graphite powder.
The material of the reaction cathode comprises but is not limited to a plate, a net, a wire or a bar corresponding to platinum, copper, nickel, gold or graphite; the relative positions of the reaction anode and the reaction cathode include, but are not limited to, single cathode single anode facing, two cathodes sandwiching an anode or cathode surrounding the anode; the surface distance of the anode material and the cathode material is 0.1 mm-2 mm.
According to the method for preparing graphene oxide based on pressure regulation and continuous electrolysis, the electrolyte is a mixture of one or more than two non-reaction systems in acid or salt; wherein the acid includes, but is not limited to, sulfuric acid, nitric acid, perchloric acid, phosphoric acid, hydrochloric acid, acetic acid, trifluoroacetic acid, trifluoromethanesulfonic acid, chlorosulfonic acid, or magic acid, and the salt includes, but is not limited to, ammonium sulfate, potassium sulfate, sodium sulfate, magnesium sulfate, potassium perchlorate, or sodium persulfate; the mass concentration of the electrolyte in the electrolyte is 0.01% -100%, and the preferable range is 60% -98%.
According to the method for preparing graphene oxide based on pressure regulation and continuous electrolysis, the voltage applied between the reaction anode and the reaction cathode is continuous direct-current voltage, pulse direct-current voltage or alternating-current voltage, the voltage range is 0.1-10 kV, and the preferable range is 1-100V.
According to the method for preparing graphene oxide based on pressure regulation and continuous electrolysis, the movement rate of the reaction anode relative to the electrolyte in the transmission process is 0-1000 m/h, and the preferable range is 0.1 cm/h-100 m/h.
According to the method for preparing graphene oxide based on pressure regulation and continuous electrolysis, the reaction anode sequentially passes through the high-pressure area and the low-pressure area in the transmission process, and the pressure born by the reaction anode in the high-pressure area and the low-pressure area is constant or variable; the pressure range of the reaction anode in the high-pressure area and the low-pressure area is 0-40 MPa and 0-10 MPa respectively.
The method for preparing graphene oxide based on pressure-regulated continuous electrolysis is characterized in that the method for preparing graphene oxide based on pressure-regulated continuous electrolysis is used for carrying out space restriction and extrusion on a reaction anode in the transmission process, wherein the method comprises one or more modes of restricting an expansion space, fastening a spring, electrically pressurizing, pressurizing by a hydraulic device or pressurizing by a pneumatic device.
According to the method for preparing graphene oxide based on pressure-regulated continuous electrolysis, the anode material after the oxidation reaction is stripped by one or more modes of mechanical shearing, ultrasonic crushing, high-pressure homogenization and the like, and the anode material after the oxidation reaction is cleaned by one or more modes of centrifugal cleaning, filter pressing cleaning, cross-flow cleaning and the like.
In the high pressure region, the expansion of the graphite raw material is spatially limited, and the difficulty of ions entering the interlayer of graphite molecules is increased. Under the action of an electric field, the movement intensity of electrolyte ions is increased and is far greater than that of water molecules in the electrolyte, and ion intercalation can be realized through the regulation and control of pressure and the electric field applied to the graphite raw material, and meanwhile, the entry of water molecules is avoided. Ions entering the graphite interlayer can not be intercalated under the protection of an electric field. Due to intercalation, the volume of the graphite raw material expands to a certain extent, but due to space limitation, the graphite raw material still maintains a complete continuous structure in a macroscopic sense, has better structural strength and maintains a complete conductive path.
Along with the transportation of the conveying device, the intercalated graphite raw material enters a low-pressure area, the volume of the graphite raw material can be slowly expanded in the low-pressure area, water molecules gradually enter the interlayer of graphite molecules, an electrolytic reaction occurs, free radical ions generated by the decomposition of the water molecules oxidize the graphite raw material to generate graphite oxide, and the interlayer spacing of the graphite molecules is increased along with the pressure release and the use of gas generated in the electrolytic process.
And stripping the oxidized graphite raw material, separating a graphite molecular layer, and performing treatments such as cleaning to obtain the high-quality graphite oxide material.
The invention has the advantages and beneficial effects that:
1. the invention has intercalation and oxidation reaction in the same electrolyte, the electrolyte mass fraction in the product after the oxidation reaction is less than 70%, the cleaning is easy, and the water consumption is less than 50 times of the product mass.
2. The invention can realize continuous preparation of graphene oxide, and the mass ratio of graphene oxide products to graphite raw materials is 130% -150%.
3. The single-layer rate of the graphene oxide prepared by the method is more than 65%, and the carbon source molar ratio can reach 1.4.
Drawings
FIG. 1 is a schematic view of the construction and process of the apparatus used in the present invention;
FIG. 2 is a photograph of a microstructure of graphene oxide in example 1;
FIG. 3 is a graph showing Raman spectrum comparison of graphene (a) and graphene oxide (b) before and after the reaction;
in the figure, the anode is reacted at 1-, the roller is conducted at 2-, the power supply is 3-, the guide roller is 4-, the cathode is reacted at 5-, the conveyor belt is 6-, the first roller set is 7-, the second roller set is 8-, the third roller set is 9-and the electrolyte is 10-.
Description of the embodiments
The invention relates to a method for preparing graphene oxide based on pressure regulation and continuous electrolysis, which takes graphite with a macroscopic continuous structure as a raw material in a specific implementation process, and is used as a reaction anode to electrify a reaction anode and a reaction cathode which are soaked in electrolyte, wherein the reaction anode sequentially carries out intercalation reaction and oxidation reaction in a high-voltage area and a low-voltage area under the space limitation and extrusion of a conveying device. Stripping and cleaning the anode material after the oxidation reaction is completed to obtain a graphene oxide material;
as shown in fig. 1, a device for realizing the method comprises a reaction anode 1, a conductive roller 2, a power supply 3, a guide roller 4, a reaction cathode 5, two groups of conveyor belts 6, a first roller group 7, a second roller group 8, a third roller group 9 and electrolyte 10, wherein the specific structure is as follows: the reaction anode 1 is wound on the conductive roller 2, one end of the reaction anode 1 is immersed in electrolyte 10, passes through between two groups of conveying belts 6, the two groups of conveying belts 6 are parallel and reversely rotated to enable the reaction anode 1 to be conveyed rightwards, the conveying belts 6 are sleeved on the guide rollers 4 and pass through a first roller group 7, a second roller group 8 and a third roller group 9, the first roller group 7, the second roller group 8 and the third roller group 9 respectively squeeze the conveying belts, the first roller group 7 and the second roller group 8 enable the left side of the conveying belts 6 to form a high-pressure area, the second roller group 8 and the third roller group 9 enable the right side of the conveying belts 6 to form a low-pressure area, the reaction cathode 5 is immersed in the electrolyte 10 and is placed on two sides of the reaction anode 1 in parallel, and the conductive roller 2 and the reaction cathode 5 are respectively connected on the positive electrode and the negative electrode of the power supply 3 through wires.
The drawings and examples described herein illustrate embodiments of the invention in further detail, and the following three examples are illustrative of the invention and are not intended to limit the scope of the invention.
Example 1
In this embodiment, the reaction anode 1 is graphite paper 1, the reaction cathode 5 is graphite plate 5, the power supply 3 is a direct current power supply 3, and the electrolyte 10 is sulfuric acid electrolyte.
The device used in this embodiment 1 includes graphite paper 1, conductive roller 2, dc power supply 3, guide roller 4, graphite plate 5, conveyor belt 6, first roller set 7, second roller set 8, third roller set 9 and sulfuric acid electrolyte 10, and the specific structure is as follows: the graphite paper 1 is wound on the conductive roller 2, one end of the graphite paper 1 is immersed in sulfuric acid electrolyte 10, passes through the two groups of conveyor belts 6, the two groups of conveyor belts 6 rotate in parallel and reversely, so that the graphite paper 1 is conveyed rightwards, the conveyor belts 6 are sleeved on the guide roller 4 and pass through a first roller group 7, a second roller group 8 and a third roller group 9, the three roller groups 7,8 and 9 respectively squeeze the conveyor belts, the first roller group 7 and the second roller group 8 enable the left side of the conveyor belts 6 to form a high-pressure area, and the second roller group 8 and the third roller group 9 enable the right side of the conveyor belts 6 to form a low-pressure area. The graphite plate 5 is immersed in sulfuric acid electrolyte 10, placed on two sides of the graphite paper 1 in parallel, and the conductive roller 2 and the graphite plate 5 are respectively connected to the positive electrode and the negative electrode of the direct current power supply 3 through wires.
In this example, the thickness was 500 μm, the width was 40cm, and the density was 1.7g/cm 3 The graphite paper is used as a graphite raw material and used as a reaction anode, graphite plates with the thickness of 3mm, the width of 50cm and the length of 1m are used as reaction cathodes, the graphite plates are respectively placed on two sides of the graphite paper in parallel, the distance between the graphite paper and the graphite plates is 5cm, and direct-current voltage of 5.0V is loaded between the cathode and the anode. Sulfuric acid with the mass fraction of 70% is selected as electrolyte, and the cathode and anode are immersed in the electrolyte. The width of the conveying belts is 50cm, the length of the conveying belts is 1m, the two groups of conveying belts are in contact with graphite paper, so that the graphite paper in the electrolyte moves rightwards at a speed of 5cm/h, the three roller sets respectively provide pressures of 50KPa, 50KPa and 10KPa, a high-pressure area and a low-pressure area are formed between the conveying belts, and the graphite paper passes through the high-pressure area and the low-pressure area to complete electrochemical reaction. And collecting anode materials after the oxidation reaction is completed, and performing shearing and filter pressing treatment to obtain graphene oxide dispersion liquid. As shown in FIG. 3, the disorder degree of the graphite raw materials before and after the reaction is increased, the oxidation degree of the product is high, the ratio of a D peak to a G peak in a Raman spectrum is changed from 0.16 to 1.06, the single-layer rate of the obtained graphene oxide is 80%, as shown in FIG. 2, the sheet diameter distribution is 5-20 micrometers, the thickness range of the sheet layer is 0.5-10 nanometers, and the carbon-oxygen mole ratio is 1.6. The yield from the graphite starting material to the graphene oxide dispersion was 150%.
Example 2
The density of the sample is 1.7g/cm 3 The carbon rope with the diameter of 5mm is used as a graphite raw material, sulfuric acid with the mass fraction of 80% is used as electrolyte, graphene oxide is prepared, other device structures are the same as those of the embodiment 1, and specific preparation parameters of the embodiment are as follows:
and applying a direct-current voltage of 12V between the anode and the cathode, wherein the conveyor belt provides a transmission speed of 10cm/h of graphite raw material, the graphite raw material is spatially limited and extruded in the conveyor belt and sequentially passes through a high-pressure area and a low-pressure area, the pressure provided by the high-pressure area is 20KPa, and the pressure provided by the low-pressure area is a uniform gradient pressure of 20 KPa-5 KPa. And collecting anode materials after the oxidation reaction is completed, and carrying out ultrasonic and centrifugal treatment to obtain graphene oxide dispersion liquid. The single-layer rate of the graphene oxide is 85%, the sheet diameter distribution is 1-10 microns, the thickness range of the sheet is 0.5-5 nanometers, and the carbon-oxygen molar ratio is 1.5. The yield from the graphite starting material to the graphene oxide dispersion was 140%.
Example 3
The density of the sample is 1.7g/cm 3 Carbon cloth with the width of 20cm is used as a graphite raw material, sulfuric acid with the mass fraction of 60% is used as electrolyte, graphene oxide is prepared, other device structures are the same as those of the embodiment 1, and specific preparation parameters of the embodiment are as follows:
and applying 24V direct current voltage between the anode and the cathode, wherein the conveying belt provides a conveying speed of 20cm/h of graphite raw materials, the graphite raw materials are limited and extruded in space in the conveying belt and sequentially pass through a high-pressure area and a low-pressure area, the pressure provided by the high-pressure area is 30Kpa, and the pressure provided by the low-pressure area is uniform gradient pressure of 30 KPa-10 KPa. And collecting anode materials after the oxidation reaction is completed, and carrying out ultrasonic and centrifugal treatment to obtain graphene oxide dispersion liquid. The single-layer rate of the obtained graphene oxide is 60%, the sheet diameter distribution is 1-10 microns, the sheet thickness range is 0.5-10 nanometers, and the carbon-oxygen molar ratio is 2.0. The yield from the graphite starting material to the graphene oxide dispersion was 120%.
The result shows that the method can realize continuous preparation of the graphene oxide in the same electrolyte, is an efficient, green and low-cost large-scale preparation mode of the graphene oxide, and has great application value. The three examples above are further illustrative of the present invention in which the transfer device and the manner of pressurizing the graphite feedstock may be modified and adapted in several ways, and are also considered to be within the scope of the present invention without departing from the principles of the present invention.
Claims (7)
1. The method for preparing graphene oxide based on pressure regulation and continuous electrolysis is characterized in that graphite with a macroscopic continuous structure is used as a reaction anode, the reaction anode and a reaction cathode which are soaked in electrolyte are electrified, the reaction anode sequentially performs intercalation reaction and oxidation reaction in a high-pressure area and a low-pressure area under the space limitation and extrusion of a conveying device, and anode substances after the oxidation reaction are stripped and cleaned to obtain a graphene oxide material; the voltage applied between the reaction anode and the reaction cathode is continuous direct-current voltage, pulse direct-current voltage or alternating-current voltage, and the voltage range is 0.1-V-10 kV; the reaction anode sequentially passes through a high-pressure area and a low-pressure area in the transmission process, and the pressure born by the reaction anode in the high-pressure area and the low-pressure area is constant pressure or variable pressure; the pressure range of the reaction anode in the high-pressure area and the low-pressure area is 0-40 MPa and 0-10 MPa respectively;
the device for realizing the method comprises a reaction anode (1), a conductive roller (2), a power supply (3), a guide roller (4), a reaction cathode (5), two groups of conveyor belts (6), a first roller group (7), a second roller group (8), a third roller group (9) and electrolyte (10), and has the specific structure that: the reaction anode (1) winds on the conductive roller (2), one end of the reaction anode (1) is immersed in electrolyte (10), passes through between two groups of conveying belts (6), the two groups of conveying belts (6) rotate in parallel and reversely, so that the reaction anode (1) is conveyed rightwards, the conveying belts (6) are sleeved on the guide roller (4) and pass through a first roller set (7), a second roller set (8) and a third roller set (9), the first roller set (7), the second roller set (8) and the third roller set (9) respectively squeeze the conveying belts, the first roller set (7) and the second roller set (8) enable the left side of the conveying belts (6) to form a high-voltage area, the second roller set (8) and the third roller set (9) enable the right side of the conveying belts (6) to form a high-voltage area, the reaction cathode (5) is immersed in the electrolyte (10), and is placed on two sides of the reaction anode (1) in parallel, and the conductive roller set (2) and the reaction cathode (5) are respectively connected to the positive electrode and the negative electrode of the power supply (3) through wires.
2. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the graphite raw material with a macroscopic continuous structure is a sheet, wire, bar or plate prepared from one or more of natural graphite, artificial graphite, bulk graphite, flake graphite, aphanitic graphite, expanded graphite or graphite powder.
3. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the materials of the reaction cathode include, but are not limited to, plates, meshes, wires or bars corresponding to platinum, copper, nickel, gold or graphite; the relative positions of the reaction anode and the reaction cathode include, but are not limited to, single cathode single anode facing, two cathodes sandwiching an anode or cathode surrounding the anode; the surface distance of the anode material and the cathode material is 0.1 mm-2 mm.
4. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the electrolyte is a mixture of one or more non-reactive systems of acid or salt; wherein the acid includes, but is not limited to, sulfuric acid, nitric acid, perchloric acid, phosphoric acid, hydrochloric acid, acetic acid, trifluoroacetic acid, trifluoromethanesulfonic acid, chlorosulfonic acid, or magic acid, and the salt includes, but is not limited to, ammonium sulfate, potassium sulfate, sodium sulfate, magnesium sulfate, potassium perchlorate, or sodium persulfate; the mass concentration range of the electrolyte in the electrolyte is 0.01% -100%.
5. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the movement rate of the reaction anode relative to the electrolyte in the transmission process is 0-1000 m/h.
6. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the means for spatially restricting and compressing the reactive anode during transportation includes, but is not limited to, mixed application by one or more of restricting expansion space, spring tightening, electric pressurization, hydraulic pressurization, or pneumatic pressurization.
7. The method for preparing graphene oxide based on pressure-regulated continuous electrolysis according to claim 1, wherein the manner of stripping the anode material after the completion of the oxidation reaction comprises one or more of combination of mechanical shearing, ultrasonic crushing and high-pressure homogenization, and the manner of cleaning the anode material after the completion of the oxidation reaction comprises one or more of combination of centrifugal cleaning, filter-press cleaning and cross-flow cleaning.
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