CN113201744A - Method for preparing graphene oxide by electrochemical method - Google Patents
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- CN113201744A CN113201744A CN202110535331.5A CN202110535331A CN113201744A CN 113201744 A CN113201744 A CN 113201744A CN 202110535331 A CN202110535331 A CN 202110535331A CN 113201744 A CN113201744 A CN 113201744A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002848 electrochemical method Methods 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 15
- 239000003792 electrolyte Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims description 22
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 6
- 230000001590 oxidative effect Effects 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000002791 soaking Methods 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a method for preparing graphene oxide by an electrochemical method, which comprises the following steps: taking a graphite rod as an anode and an inert electrode as a cathode, and inserting one end of the anode and one end of the cathode into electrolyte; and connecting the other ends of the anode and the cathode to a constant voltage power supply, electrifying for electrolysis, and generating the graphene oxide. The graphene oxide is prepared by adopting the electrochemical method, so that the use of strong acid, strong oxidant and strong reducing agent is avoided, the dispersibility of the graphene oxide in water is enhanced through surface modification, the preparation of the modified graphene by the electrochemical method is simple and convenient, the obtained modified graphene has few surface defects, and the method is suitable for large-scale continuous automatic production and has a simple process.
Description
Technical Field
The invention relates to the technical field of graphene oxide preparation, in particular to a method for preparing graphene oxide by an electrochemical method.
Background
Graphene oxide is a layered graphite oxide, with surface functional groups providing abundant and effective active sites. In addition, graphene oxide possesses tunable electronic properties. In general, due to the large number of sp3The hybrid carbon atoms combine with oxygen-containing groups to produce an insulating layer which allows a monolithic resistance of up to 1012Ωsq-1Or higher. Graphene oxide also exhibits excellent optical and mechanical properties, respectivelyThe field is widely applied to adjusting the light transmittance of the graphene oxide film by changing the thickness of the graphene oxide film and the reduction degree of the graphene oxide. Generally, a graphene oxide thin film suspended in water shows a dark brown to bright yellow state due to a difference in concentration. In general, the mechanical properties of graphene oxide are determined by the degree and thickness of oxidation, and the like. Although the graphene oxide has rich characteristics, the graphene oxide still has some defects in practical application, and the electrical performance and the specific surface area of the graphene oxide are affected by structural defects, poor dispersibility and multi-layer thickness. The insulating properties of conventional graphene oxide also limit its application in electronic devices and energy storage. However, the oxygen-containing functional group on the surface of graphene oxide itself can greatly increase its structure and chemical diversity by chemically modifying or functionally optimizing it. Therefore, graphene oxide and the composite material thereof have great potential in the application fields of energy storage conversion and environmental protection.
Due to the excellent properties of graphene, the preparation of graphene is receiving much attention, and among them, the chemical redox method is widely used. The graphene is prepared by an oxidation-reduction method, wherein graphite is treated by strong acid and strong oxidant to obtain expanded graphite with an oxide group intercalation, graphene oxide is obtained by ultrasonic stripping, and finally the graphene is obtained by reduction of a strong reducing agent (such as hydrazine hydrate). The strong acid, the strong oxidant and the strong reducing agent are used for preparing the graphene by using the method, so that the environment is polluted, the surface defects of the graphene prepared by using the method are more, and the graphene sheet layer is easy to fold and curl, so that the performance of the graphene is influenced; and the graphene obtained after reduction by the method has almost no oxide group on the surface, so that the surface is hydrophobic, and the graphene is easy to agglomerate and settle in water and some common organic solvents.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for preparing graphene oxide by an electrochemical method, and aims to solve the problems that the existing preparation method of graphene oxide has great environmental pollution and the prepared graphene oxide has poor performance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing graphene oxide by an electrochemical method comprises the following steps:
taking a graphite rod as an anode and an inert electrode as a cathode, and inserting one end of the anode and one end of the cathode into electrolyte;
and connecting the other ends of the anode and the cathode to a constant voltage power supply, electrifying for electrolysis, and generating the graphene oxide.
The method for preparing the graphene oxide by the electrochemical method comprises the step of preparing an electrolyte, wherein the electrolyte is one of sulfate or nitrate.
The method for preparing the graphene oxide by the electrochemical method comprises the step of preparing an electrolyte solution by the electrochemical method, wherein the concentration of the electrolyte solution is 0.1-0.2M.
The method for preparing the graphene oxide by the electrochemical method comprises the step of preparing the graphene oxide by the electrochemical method, wherein the voltage of the constant voltage power supply is 5-10V.
The method for preparing the graphene oxide by the electrochemical method comprises the step of electrifying for electrolysis, wherein the electrolysis time is 1-10 h.
The method for preparing the graphene oxide by the electrochemical method comprises the following steps of connecting the other ends of the anode and the cathode to a constant voltage power supply, and after electrifying for electrolysis, carrying out electrolysis:
carrying out vacuum filtration on the electrolyzed electrolyte, washing a filter cake with pure water, and dispersing the filter cake with ions removed into the pure water to obtain a dispersion liquid containing graphene oxide;
carrying out centrifugal separation on the dispersion liquid containing the graphene oxide, and taking an upper layer liquid;
and carrying out freeze drying on the upper layer liquid to obtain the graphene oxide.
The method for preparing the graphene oxide by the electrochemical method comprises the step of carrying out centrifugal separation on the dispersion liquid containing the graphene oxide, wherein the centrifugal separation speed is 5000-50000rpm, and the centrifugal separation time is 5-30 min.
Has the advantages that: the invention provides a method for preparing graphene oxide by an electrochemical method. The graphene oxide is prepared by adopting the electrochemical method, so that the use of strong acid, strong oxidant and strong reducing agent is avoided, the dispersibility of the graphene oxide in water is enhanced through surface modification, the preparation of the modified graphene by the electrochemical method is simple and convenient, the obtained modified graphene has few surface defects, and the method is suitable for large-scale continuous automatic production and has a simple process.
Drawings
Fig. 1 is a flowchart of a preferred embodiment of a method for preparing graphene oxide by an electrochemical method according to the present invention.
FIG. 2 is a schematic structural view of an electrolytic cell provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a diagram illustrating a method for preparing graphene oxide by an electrochemical method according to the present invention, which includes the following steps:
s10, taking a graphite rod as an anode and an inert electrode as a cathode, and inserting one end of the anode and one end of the cathode into electrolyte;
and S20, connecting the other ends of the anode and the cathode to a constant voltage power supply, electrifying and electrolyzing to generate the graphene oxide.
The method has the advantages that an electrochemical method is used, the preparation of the graphene oxide can be completed through a one-step method, strong acid, a strong oxidant and a strong reducing agent can be avoided, and the environmental pollution is low; the method provided by the embodiment has the advantages of simple process, high production efficiency and low cost, and is suitable for automatic control and large-scale continuous production; the graphene oxide prepared by the embodiment can be well dispersed in water, does not settle after standing for one month, and is stable in chemical property.
In some embodiments, the electrolyte is one of a sulfate or a nitrate, but is not limited thereto.
In some embodiments, the concentration of the electrolyte is 0.1 to 0.2M, but is not limited thereto.
In some embodiments, the graphite rod may be immersed in an electrolyte solution for a pre-soaking treatment before electrolysis, and the pre-soaking time may be 0 to 24 hours.
In some embodiments, the other end of the anode and the cathode is connected to a constant voltage power supply, and during electrolysis by electrifying, the voltage of the constant voltage power supply is 5-10V, and the electrolysis time is 1-10 h.
In some embodiments, the other end of the anode and the cathode is connected to a constant voltage power supply, and the method further comprises the following steps after the anode and the cathode are electrified for electrolysis: carrying out vacuum filtration on the electrolyzed electrolyte, washing a filter cake with pure water, and dispersing the filter cake with ions removed into the pure water to obtain a dispersion liquid containing graphene oxide; carrying out centrifugal separation on the dispersion liquid containing the graphene oxide, and taking an upper layer liquid; and carrying out freeze drying on the upper layer liquid to obtain the graphene oxide.
In this embodiment, in the step of performing centrifugal separation on the dispersion liquid containing graphene oxide, the centrifugal separation rate is 5000-50000rpm, and the centrifugal separation time is 5-30 min. The upper layer liquid obtained in this example is more than one fifth of the volume of the bottom of the centrifuge tube.
In some embodiments, the inert electrode is a platinum electrode or a gold electrode, but is not limited thereto.
The following provides a further explanation of the method for preparing graphene oxide by an electrochemical method according to the present invention by using specific examples:
example 1
Preparing 0.2M sodium sulfate, assembling equipment according to the figure 2, connecting a constant voltage power supply to a platinum electrode serving as a cathode and a graphite rod serving as an anode, introducing 5V voltage for 10h, carrying out vacuum filtration on the obtained liquid, washing a filter cake with pure water for three times, dispersing the filter cake into the pure water, carrying out centrifugal separation for 30min at 5000rpm by using a centrifugal machine, removing three fifths of liquid on the upper layer of a centrifugal tube, and carrying out freeze drying to obtain graphene oxide powder.
Example 2
Preparing 0.2M potassium nitrate, taking a gold electrode as a cathode and a graphite rod as an anode, pre-soaking the graphite rod in the solution for 12h, assembling equipment as shown in figure 2, connecting a constant-voltage power supply to the equipment, applying a voltage of 8V for 10h, performing vacuum filtration on the obtained liquid, washing a filter cake for three times by using pure water, dispersing the filter cake into the pure water, performing centrifugal separation for 30min at 8000rpm by using a centrifugal machine, removing three fifths of liquid on the upper layer of a centrifugal tube, and performing freeze drying to obtain graphene oxide powder.
Example 3
Preparing 0.15M sodium sulfate, taking a platinum electrode as a cathode and a graphite rod as an anode, pre-soaking the graphite rod in the solution for 12 hours, assembling equipment as shown in figure 2, connecting a constant voltage power supply to the equipment, applying a voltage of 10V for 10 hours, carrying out vacuum filtration on the obtained liquid, washing a filter cake for three times by using pure water, dispersing the filter cake into the pure water, carrying out centrifugal separation for 30 minutes by using a centrifugal machine at 10000rpm, removing liquid of four fifths of the upper layer of a centrifugal tube, and carrying out freeze drying to obtain graphene oxide powder.
In summary, the present invention provides a method for preparing graphene oxide by an electrochemical method, wherein a constant voltage is applied to an electrolyte, an inert metal is used as a cathode, a graphite rod is used as an anode, and the graphene oxide obtained by electrolysis can be stably dispersed in water. The graphene oxide is prepared by adopting the electrochemical method, so that the use of strong acid, strong oxidant and strong reducing agent is avoided, the dispersibility of the graphene oxide in water is enhanced through surface modification, the preparation of the modified graphene by the electrochemical method is simple and convenient, the obtained modified graphene has few surface defects, and the method is suitable for large-scale continuous automatic production and has a simple process.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. A method for preparing graphene oxide by an electrochemical method is characterized by comprising the following steps:
taking a graphite rod as an anode and an inert electrode as a cathode, and inserting one end of the anode and one end of the cathode into electrolyte;
and connecting the other ends of the anode and the cathode to a constant voltage power supply, electrifying for electrolysis, and generating the graphene oxide.
2. The method for preparing graphene oxide by the electrochemical method according to claim 1, wherein the electrolyte is one of sulfate or nitrate.
3. The method for preparing graphene oxide according to claim 1, wherein the concentration of the electrolyte is 0.1-0.2M.
4. The method for electrochemically preparing graphene oxide according to claim 1, wherein the voltage of the constant voltage power supply is 5-10V.
5. The method for electrochemically preparing graphene oxide according to claim 1, wherein in the step of electrolysis by energization, the electrolysis time is 1-10 h.
6. The method for preparing graphene oxide by the electrochemical method according to claim 1, wherein the other end of the anode and the other end of the cathode are connected to a constant voltage power supply, and the method further comprises the following steps after the constant voltage power supply is electrified for electrolysis:
carrying out vacuum filtration on the electrolyzed electrolyte, washing a filter cake with pure water, and dispersing the filter cake with ions removed into the pure water to obtain a dispersion liquid containing graphene oxide;
carrying out centrifugal separation on the dispersion liquid containing the graphene oxide, and taking an upper layer liquid;
and carrying out freeze drying on the upper layer liquid to obtain the graphene oxide.
7. The method for preparing graphene oxide by the electrochemical method according to claim 6, wherein in the step of centrifuging the dispersion liquid containing graphene oxide, the centrifugation rate is 5000-50000rpm, and the centrifugation time is 5-30 min.
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| CN202110535331.5A CN113201744A (en) | 2021-05-17 | 2021-05-17 | Method for preparing graphene oxide by electrochemical method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
| CN106591871A (en) * | 2016-12-01 | 2017-04-26 | 燕园众欣纳米科技（北京）有限公司 | Method for preparing graphene through electrochemical in-situ oxidation and reduction |
| CN107601488A (en) * | 2017-09-08 | 2018-01-19 | 深圳大学 | A kind of preparation method of graphene oxide |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
| US20190112195A1 (en) * | 2016-03-22 | 2019-04-18 | Institute Of Metal Research Chinese Academy Of Sciences | Method for Continuously Preparing Graphene Oxide Nanoplatelet |
-
2021
- 2021-05-17 CN CN202110535331.5A patent/CN113201744A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
| US20190112195A1 (en) * | 2016-03-22 | 2019-04-18 | Institute Of Metal Research Chinese Academy Of Sciences | Method for Continuously Preparing Graphene Oxide Nanoplatelet |
| CN106591871A (en) * | 2016-12-01 | 2017-04-26 | 燕园众欣纳米科技（北京）有限公司 | Method for preparing graphene through electrochemical in-situ oxidation and reduction |
| CN107601488A (en) * | 2017-09-08 | 2018-01-19 | 深圳大学 | A kind of preparation method of graphene oxide |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
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