CN110272040B - Preparation method of high-purity graphene oxide - Google Patents
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Abstract
The invention relates to a preparation method of high-purity graphene oxide, and belongs to the field of nano materials and preparation methods. The preparation method of the graphene oxide is simple in process, high in oxidation degree, economical, environment-friendly and easy to scale. The method is that electrodes made of graphite materials are inserted into deionized water in parallel; and promoting the oxidation and stripping of the graphite layer under the conditions of water flow cutting and direct current voltage through the action of electrochemical oxidation, and drying the obtained graphene aqueous solution to obtain the high-purity graphene oxide. The method has the advantages of simple process, easy large-scale preparation and the like, and the prepared graphene oxide has high purity, high oxidation degree, good water solubility and easy dispersion, and is particularly suitable for being used as an electrode material or a conductive additive of an energy storage device, a catalyst carrier and the fields of biological imaging, probes/sensing, medical treatment and the like.
Description
Technical Field
The invention relates to a preparation method of high-purity graphene oxide, belonging to the field of nano materials and preparation.
Background
Graphene draws a great deal of attention in the fields of electronics, information, energy, materials, biomedicine and the like by virtue of unique optical, mechanical, electrical, quantum and other properties, such as high electrical conductivity, high thermal conductivity, high hardness, high strength and the like, and with the rapid development of micro-sodium or atomic-level manufacturing and processing technologies, research on electronic device chips related to graphene is also deepened continuously and related products, such as graphene chips, are proposed. Meanwhile, graphene is used as a structural material, and various different work is derived due to different structuresThe material comprises graphene oxide, graphene strips, graphene nanotubes and the like. Among the materials, the graphene oxide plane contains-OH and C-O-C, and the edge of the sheet layer contains C = O and COOH, compared with graphene, the oxidized functional groups endow the graphene oxide with more abundant physicochemical properties, and the graphene oxide has good wetting property and surface activity, can be peeled off after being intercalated by small molecules or polymers, has adjustable semiconductor band gap, plays a very important role in improving the comprehensive properties of the materials such as thermal property, electricity and mechanics, and is widely applied to the fields of energy storage, chemical adsorption, catalysis, biomedicine, drug controlled release and the like. For example, graphene oxide has a large specific surface area, and can provide sufficient loading space for gold, iron rhodium alloy, palladium, platinum and other nano-catalysts. And the load proportion, the modification mode and the like can be regulated and controlled, so that the catalytic performance of the catalyst can be regulated and optimized, and the catalyst can be used as a chemical sensing electrode and a catalytic electrode of a fuel cell. Graphene can also be used as an electrode material (LiFePO) in a plurality of energy storage devices 4 、LiNi 0.5 Mn 1.5 O 4 、Li 4 Ti 5 O 12 、Si、Sn、FeO x And the like) to form a highly conductive advanced electrode, the graphene oxide can promote the capacity of the electrode active material to be greatly exerted and relieve the volume effect of the active material in the charging and discharging processes, and therefore, the electrode can often show excellent cycle stability, high power or high specific energy performance. When the graphene oxide is partially reduced, the graphene oxide itself can be used as a high specific volume negative electrode material of a lithium ion/sodium ion battery, and can also be used as a semiconductor for a solar battery or an electronic element. In biology, shanghai applied physics research discovers that the application of graphene oxide in PCR technology can significantly improve the specificity, sensitivity and amplification yield of PCR, eliminate primer dimers formed in amplification, has a wide optimization interval, and can be widely applied to DNA templates with various concentrations and complexity. Compared with other carbon nano materials applied to the PCR technology, the graphene oxide has more excellent comprehensive effect on the optimization of PCR. In addition, the graphene has extremely low toxicity and high biocompatibility,can be used as a drug carrier to realize drug slow release in a living body, and can also be used as a targeted drug for treating cancer or realize infrared thermal treatment after surface functionalization. In the aspect of structural design, due to the processability of the graphene oxide, the graphene oxide can be used as a wave-absorbing material with excellent performance after being subjected to certain metamaterial structural processing, and can be applied to national defense construction. In summary, graphene oxide has a very wide range of applications and very important research values.
At present, the methods for preparing graphene oxide are more, and are roughly divided into a top-down method and a bottom-up method. The former idea is to prepare graphene oxide by splitting crystalline flake graphite and the like through strong oxidation, and is represented by three methods of traditional Brodie, staudenmai and Hummers. The latter is formed by chemical vapor deposition of various organic micromolecular carbon sources such as ethylene, propane and the like. At present, the preparation processes for preparing graphene oxide by the Brodie method, the Staudenmier method and the Hummers method are relatively mature, are still in use today, and part of the methods are slightly improved on the basis of the methods. The preparation principle of the methods is that graphite forms a graphite interlayer compound under the combined action of strong acid and a small amount of strong oxidant, then the interlayer compound continuously undergoes deep liquid phase oxidation reaction under the action of excessive strong oxidant, graphite oxide is obtained after hydrolysis, finally, the mixture of the graphite oxide and water is stirred by ultrasound or for a long time to obtain the graphene oxide, the oxidation degree of the product and the synthesis process are related to the reaction time, and the oxidation degree and the synthesis process can be measured by the atomic ratio of C to O. The Brodie method and the Staudenmaeer method have high oxidation degree, but ClO is generated in the reaction process 2 、NO 2 Or N 2 O 4 Harmful gases and long reaction time; the Hummers method has short reaction time and no toxic gas ClO 2 However, the process factors to be controlled in the reaction process are more, and excessive permanganate ions can cause potential pollution, so that a large amount of H is required in the preparation process 2 O, is not economical and environment-friendly, and causes the obtained graphene to have higher cost. In view of the above problems, in recent years, many researchers have searched for a better preparation method in order to obtain graphene oxide. For example, matsuoy employs electrochemicalChemical method graphite in strong acid, hg/Hg 2 SO 4 And putting the electrode into water after electrolytic oxidation, and drying to obtain the graphene oxide. Daniela C Marcano et al in KMnO 4 And 9: 1 (by volume) of H 2 SO 4 /H 3 PO 4 As an oxidizing agent, without addition of NaNO 3 The method also can be used for preparing the graphene oxide, the effectiveness of the oxidation process is improved, the hydrophilicity of the obtained product is enhanced, toxic gas is not generated in the reaction process, the environmental pollution is small, and the reaction temperature is easy to control. The Shen Jianfeng et al uses benzoyl peroxide as an oxidant to rapidly prepare the graphene oxide, thereby shortening the preparation time. Use of [ C ] by Na Liu etc 8 mim] + [PF 6 ] - And taking the solution of water as electrolyte, taking a graphite rod as an electrode, and preparing the ionic liquid modified graphene oxide by an electrochemical oxidation method. In the above methods, other conductive ions are introduced when electrochemical oxidation is performed. Although the introduction of the conductive ions accelerates the formation of graphene, the introduction of the conductive ions causes the electrolytic decomposition of water, and hydrogen and oxygen are rapidly generated on the electrode, so that the graphene peeled off from the electrode is too thick, and is not sufficiently oxidized, and the degree of oxidation is not high. In addition, the graphene oxide solution obtained by the above method may contain other impurity ions, i.e., conductive ions, which may cause impurities in the finally dried graphene powder, and thus the obtained graphene may not have universality as a raw material. So far, no simple method for preparing high-purity graphene oxide in batches is available. Based on the consideration, the method combines electrochemical oxidation and water flow cutting to promote graphite to be oxidized and stripped in a high-purity water system, and because water used in the electrochemical oxidation process is deionized high-purity water and graphite is also a material with the purity of analysis and the purity, the prepared graphene solution is determined to have extremely high purity and can be applied to other various production and research as a high-purity raw material. The graphene prepared by the method designed by the patent has high oxidation degree, good water solubility, rich surface functional groups and few layers, and can be used for energy storage, catalysis, biological probe/imaging, drug slow release, cancer infrared thermal radiation treatment, chemical sensing, adsorption/wasteThe water treatment and other aspects have wide application space.
Disclosure of Invention
The invention aims to solve the preparation problem of high-purity graphene oxide, and provides a preparation method of high-purity graphene oxide, which is simple in process, uniform in finished product and easy to scale.
The technical scheme adopted by the invention is as follows: the preparation method of the high-purity graphene oxide comprises the following steps:
step 1) inserting graphite with a fixed shape into a negative electrode in parallel to ensure that the conductivity is 1-30M omega cm -1 In the deionized water, the distance of the graphite electrode is kept between 0.5 and 100cm;
step 2) putting a magnetic stirrer at the bottom of the ionic water container with the device, vertically putting the whole electrochemical reaction system on the magnetic stirrer, and rotating the magnetic stirrer at the speed of 10-3000 r/min to promote the deionized water to rotate at a constant speed;
step 3) applying 1-100V direct current voltage between the two graphite electrodes by using a conventional direct current power supply, keeping the voltage and the magnetic stirring speed unchanged, carrying out electrochemical reaction for 1-200 hours, and stopping the reaction after the deionized water is changed into brownish black suspension;
step 4) filtering the brownish black suspension liquid for 1-10 times by using filter paper to obtain a brownish yellow aqueous solution, and drying under a freezing or supercritical condition to obtain high-purity graphene oxide with the diameter of 0.001-10 mu m;
the graphite material is made into a rod shape, a cuboid shape or a round cake shape; the graphite material is analytically pure or spectrally pure;
the length of the magnetic stirrer is 1-10 cm, and the diameter of the magnetic stirrer is 0.1-1 cm;
the bottom of the container filled with the deionized water is provided with a magnetic stirrer which rotates at a constant speed, and the magnetic stirrer and the graphite electrode are kept at a distance of 1-5 cm and cannot be contacted with the graphite electrode;
the filter paper for filtering the brown-black suspension is qualitative or quantitative filter paper;
the method for drying the graphene solution is freezing or supercritical drying;
high purity graphene oxide prepared by the method for preparing high purity graphene oxide according to any one of the preceding claims, wherein the purity of the graphene is more than 99.99%.
The principle of the preparation method of the high-purity graphene oxide provided by the invention is as follows: firstly, inserting electrodes made of graphite materials into deionized water in parallel; and promoting the oxidation and stripping of the graphite layer by the action of electrochemical oxidation under the conditions of water flow cutting and direct current voltage, and drying the obtained graphene solution to obtain high-purity graphene oxide powder.
The invention has the beneficial effects that: the method does not need a complex preparation method, can prepare the graphene oxide with extremely high purity and higher oxidation degree in large scale and is easy for batch production; expensive instruments are not needed, the method is different from the traditional graphene oxide preparation method, the prepared graphene oxide is high in conductivity, and the graphene oxide has rich oxidation functional groups such as carboxyl, hydroxyl and the like; therefore, the method has the advantages of simple process, easiness in large-scale preparation, environmental friendliness and the like, and the prepared graphene oxide is high in purity, few in layer number, good in water solubility and easy to disperse, and is particularly suitable for being used as an electrode material or a conductive additive of an energy storage device, a chemical sensor, a catalyst, biomedicine and the like.
Drawings
FIG. 1A flow chart for preparing graphene oxide
In the figure: 1. a direct current power supply; 2. a wire; 3. a graphite electrode; 4. a container; 5. deionized water; 6. a magnetic stirrer; 7. a magnetic stirrer.
FIG. 2 Infrared Spectrum of graphene oxide
The ordinate is the infrared absorption intensity of the sample, and has no unit; the abscissa is the wave number of the infrared spectrum in cm -1 。
FIG. 3 Raman spectra of graphene oxide
The ordinate is the intensity of the raman signal, without unit; the abscissa is the shift of the Raman spectrum in cm -1 。
FIG. 4 Transmission Electron microscopy pictures of graphene oxide
Detailed Description
Example 1
Firstly, 400 ml of high-purity water (18.4M omega) is measured, a fish-shaped magnetic stirrer with the diameter of 4cm is placed in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct-current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are immersed in the high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then vertically placing the whole beaker device on a magnetic stirrer, and adjusting the magnetic stirrer to ensure that the rotating speed of a magnetic stirrer reaches 2000rpm; at the same time, the voltage on the dc power supply was adjusted to maintain the voltage field between the graphite electrodes at 30V, and the dc power supply instrument showed a current of substantially 0A between the graphite electrodes due to the low conductivity of the deionized water.
After the device is stabilized, maintaining the high-speed rotation of the direct-current voltage field and the magnetic stirrer; and (3) after the electricity is added for 96 hours, the colorless and transparent high-purity water gradually becomes a brownish black solution, the reaction is immediately stopped, the brownish black solution is taken out and filtered for 3 times by using qualitative filter paper to obtain a brownish yellow graphene oxide solution, and the graphene oxide solution is frozen and dried to obtain high-purity graphene oxide powder. The powder is tested by an infrared absorption spectrum (figure 2), a Raman spectrum (figure 3) and a transmission electron microscope (figure 4), and the test results show that the prepared graphene powder has high oxidation degree, few layers, rich functional groups and good water solubility.
Example 2
Firstly, 400 ml of deionized water (15.0M omega) is measured, a fish-shaped magnetic stirrer with the diameter of 4cm is placed in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and are used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are not in high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then vertically placing the whole beaker device on a magnetic stirrer, and adjusting the magnetic stirrer to ensure that the rotating speed of a magnetic stirrer reaches 2000rpm; meanwhile, the voltage on the direct current power supply is adjusted to keep the voltage field between the graphite electrodes at 30V, and the direct current power supply instrument shows that the current between the graphite electrodes is basically 0A due to the deionized water with lower conductivity.
After the device is stabilized, maintaining the high-speed rotation of the direct-current voltage field and the magnetic stirrer; and after the electricity is added for 96 hours, the colorless and transparent high-purity water gradually becomes a brownish black solution, the reaction is immediately stopped at the moment, the brownish black solution is taken out, the solution is filtered for 3 times by qualitative filter paper to obtain a brownish yellow graphene oxide solution, and the graphene oxide solution is freeze-dried to obtain high-purity graphene oxide powder.
Example 3
Firstly, 400 ml of deionized water (18.4M omega) is measured, a fish-shaped magnetic stirrer with the diameter of 4cm is placed in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and are used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are not in high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then vertically placing the whole beaker device on a magnetic stirrer, but not starting the magnetic stirrer, and keeping the magnetic stirrer at the bottom of the solution; the voltage on the dc power supply was adjusted to maintain the voltage field between the graphite electrodes at 30V, which showed a current of substantially 0A between the graphite electrodes on the dc power supply meter due to the low conductivity deionized water.
After the device is stabilized, maintaining a direct current voltage field, electrifying for 96 hours, gradually changing colorless and transparent high-purity water into light brown yellow, stopping the reaction, filtering for 3 times by using qualitative filter paper to obtain a brown yellow solution with extremely low graphene content, and freeze-drying the graphene solution to obtain high-purity graphene oxide powder, but the yield is extremely low, so that the uniform stirring of deionized water is helpful for stripping the graphene oxide layer.
Example 4
Firstly, 400 ml of deionized water (5M omega) and a fish-shaped magnetic stirrer with the diameter of 4cm are measured and put in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and are used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply by leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are placed in high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then the whole beaker device is placed on a magnetic stirrer, and the magnetic stirrer is adjusted to ensure that the rotating speed of a magnetic stirrer reaches 2000rpm; meanwhile, the voltage on the direct current power supply is adjusted to keep the voltage field between the graphite electrodes at 30V, and the direct current power supply instrument shows that the current between the graphite electrodes is basically 0A due to the deionized water with lower conductivity.
After the device is stabilized, maintaining the high-speed rotation of the direct-current voltage field and the magnetic stirrer; after 72 hours of electrification, the colorless and transparent high-purity water gradually becomes a brownish black solution, at the moment, the reaction is immediately stopped, the brownish black solution is taken out and filtered for 3 times by qualitative filter paper, and then, a brownish yellow graphene oxide solution can be obtained, but the oxidation degree of the graphene is not as high as that in the example 1, and the particles are larger.
Example 5
Firstly, 400 ml of hydrochloric acid solution (pH = 1) and a fish-shaped magnetic stirrer with the diameter of 4cm are measured and placed in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are immersed in high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then the whole beaker vertical device is placed on a magnetic stirrer, and the magnetic stirrer is adjusted to ensure that the rotating speed of a magnetic stirrer reaches 2000rpm; meanwhile, the voltage on the direct current power supply is adjusted to keep the voltage field between the graphite electrodes at 30V, and the direct current power supply instrument shows that the current between the graphite electrodes jumps all the time due to the hydrochloric acid solution, and bubbles continuously emerge from the electrodes, and after a period of time, the solution becomes a black turbid liquid, so that high-purity graphene oxide cannot be obtained, and graphite powder with low oxidation degree is obtained.
Example 6
Firstly, 400 ml of sodium hydroxide solution (pH = 14) and a fish-shaped magnetic stirrer with the diameter of 4cm are measured and put into a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and are used as supporting jacks of fixed electrodes, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are placed in high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker. Then vertically placing the whole beaker system on a magnetic stirrer, and adjusting the magnetic stirrer to enable the rotating speed of a magnetic stirrer to reach 2000 revolutions per minute; meanwhile, the voltage on the direct current power supply is adjusted to keep the voltage field between the graphite electrodes at 30V, and the solution has high conductivity due to the sodium hydroxide solution, the current between the graphite electrodes is shown on the instrument of the direct current power supply to jump all the time, and bubbles continuously emerge from the graphite electrodes, after a period of time, the solution becomes black turbid liquid, high-purity graphene oxide cannot be obtained, and graphite powder with low oxidation degree and large particles is obtained.
Example 7
Firstly, 400 ml of absolute ethyl alcohol and a fish-shaped magnetic stirrer with the diameter of 4cm are weighed in a 500 ml beaker, a polytetrafluoroethylene plate with the thickness of 1cm is covered on the beaker, two holes with the distance of 7.5cm and the diameter of 0.7cm are arranged on the plate and are used as supporting jacks of a fixed electrode, two carbon rods with the diameter of 0.6cm are respectively connected to a positive electrode and a negative electrode of a direct current power supply through leads and are inserted into the holes of the polytetrafluoroethylene in parallel, and most of graphite electrodes are immersed in high-purity water and keep a certain distance with a magnetic stirrer at the bottom of the beaker. Then vertically placing the whole beaker system on a magnetic stirrer, and adjusting the magnetic stirrer to enable the rotating speed of a magnetic stirrer to reach 2000 revolutions per minute; meanwhile, the voltage on the direct current power supply is adjusted to keep the voltage field between the graphite electrodes at 30V, and the direct current power supply instrument shows that the current between the graphite electrodes is basically 0A due to the fact that the absolute ethyl alcohol with extremely low conductivity is adopted.
After the device is stabilized, keeping the high-speed stirring of the voltage and the magnetic stirrer; after 120 hours of electrification, the solution system has basically no change.
The graphene oxide in the above examples 1 and 2 has high purity, few layers, high oxidation degree, good water solubility, and abundant yield, the reaction system can be flexibly replaced, the size of the graphene oxide can be appropriately controlled by the conductivity of water, and the method is simple and easy to implement, and is green and environment-friendly. The method for preparing the high-purity graphene oxide system is realized for the first time.
Claims (2)
1. A preparation method of high-purity graphene oxide is characterized by comprising the following steps:
step 1) graphite with fixed shape is used as a positive electrode and a negative electrode (3) and is parallelly inserted into a position with the conductivity of 15.0-18.4M omega cm -1 In the deionized water (5), the distance of the graphite electrode is kept between 7.5 and 100cm;
step 2) a magnetic stirrer (6) is placed at the bottom of the deionized water container (4), the whole electrochemical reaction system is vertically placed on a magnetic stirrer (7), and the magnetic stirrer rotates at a speed of 2000-3000 rpm to promote the deionized water to rotate at a constant speed;
step 3) applying 30V direct current voltage between the two graphite electrodes by using a conventional direct current power supply (1) and a lead (2), keeping the voltage and the magnetic stirring speed unchanged, carrying out an electrochemical reaction for 96 hours, and stopping the reaction after deionized water becomes a brownish black suspension;
step 4) filtering the brownish black suspension liquid for 1-10 times by using filter paper to obtain a brownish yellow aqueous solution, and drying under a freezing or supercritical condition to obtain high-purity graphene oxide with the diameter of 0.001-10 mu m;
the graphite material is made into a rod shape, a cuboid shape or a round cake shape; the graphite material is analytically pure or spectrally pure;
the length of the magnetic stirrer is 1-10 cm, and the diameter of the magnetic stirrer is 0.1-1 cm;
the bottom of the container filled with the deionized water is provided with a magnetic stirrer which rotates at a constant speed, and the magnetic stirrer and the graphite electrode are kept at a distance of 1-5 cm and cannot be contacted with the graphite electrode;
the filter paper for filtering the brown-black suspension is qualitative or quantitative filter paper;
the purity of the graphene is greater than 99.99%.
2. A preparation method of high-purity graphene oxide is characterized by comprising the following steps:
400 ml of a sample with a conductivity of 15.0 or 18.4M Ω cm are first measured -1 Putting high-purity water and a fish-shaped magnetic stirrer with the diameter of 4cm into a 500-milliliter beaker, covering the beaker with a polytetrafluoroethylene plate with the thickness of 1cm, connecting two holes with the distance of 7.5cm and the diameter of 0.7cm on the plate as supporting jacks of a fixed electrode, respectively connecting two carbon rods with the diameter of 0.6cm on a positive electrode and a negative electrode of a direct-current power supply by leads, and parallelly inserting the carbon rods into the holes of the polytetrafluoroethylene to ensure that most of graphite electrodes are immersed in the high-purity water and keep a certain distance with the magnetic stirrer at the bottom of the beaker; then vertically placing the whole beaker device on a magnetic stirrer, and adjusting the magnetic stirrer to ensure that the rotating speed of a magnetic stirrer reaches 2000rpm; meanwhile, the voltage on the direct current power supply is adjusted, so that the voltage field between the graphite electrodes is kept at 30V, and the direct current power supply instrument shows that the current between the graphite electrodes is basically 0A due to the deionized water with low conductivity; after the device is stabilized, maintaining the high-speed rotation of the direct-current voltage field and the magnetic stirrer; adding electricity for 96 hours, gradually changing colorless and transparent high-purity water into a brownish black solution, immediately stopping the reaction, taking out the brownish black solution, filtering the solution for 3 times by using qualitative filter paper to obtain a brownish yellow graphene oxide solution, and freeze-drying the graphene oxide solution to obtain high-purity graphene oxide powder; the purity of the graphene is greater than 99.99%.
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