CN115636408A - Preparation method of graphene oxide - Google Patents
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- CN115636408A CN115636408A CN202211117958.XA CN202211117958A CN115636408A CN 115636408 A CN115636408 A CN 115636408A CN 202211117958 A CN202211117958 A CN 202211117958A CN 115636408 A CN115636408 A CN 115636408A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 58
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 48
- 239000010439 graphite Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000007800 oxidant agent Substances 0.000 claims abstract description 24
- 230000001590 oxidative effect Effects 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 9
- 239000012286 potassium permanganate Substances 0.000 claims description 9
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 230000008961 swelling Effects 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 description 28
- 230000003647 oxidation Effects 0.000 description 18
- 238000009830 intercalation Methods 0.000 description 14
- 230000002687 intercalation Effects 0.000 description 14
- 230000003287 optical effect Effects 0.000 description 11
- 238000005086 pumping Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- -1 3 Chemical class 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920006337 unsaturated polyester resin Polymers 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The scheme discloses a preparation method of graphene oxide, which comprises the following steps: mixing graphite and concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under a vacuum condition to obtain a mixture B; adding an oxidant into the mixture B, heating, vacuumizing, and reacting under a vacuum condition to obtain a mixture C; and carrying out suction filtration on the mixture C, and washing to obtain the graphene oxide. According to the method, the reaction rate is accelerated by a vacuumizing process, the using amount of an oxidant is reduced, and the high-stripping large-size graphene oxide is prepared.
Description
Technical Field
The invention relates to the technical field of two-dimensional material preparation, in particular to a preparation method of graphene oxide.
Background
Nowadays, graphene oxide has advantages in various fields, such as biomedicine, flexible conductive films, liquid crystal optical materials, energy storage materials, and the like. The transverse size of the graphene oxide is increased, so that the related mechanical and liquid crystal properties of a macroscopic assembly structure assembled by graphene oxide sheets can be improved, and the market hopes to prepare the large-size graphene oxide due to the advantages of few nodes, few edge contacts, high orientation and the like. However, the graphene oxide produced in large scale is prepared by premixing graphite and concentrated sulfuric acid, adding a large amount of potassium permanganate, and performing medium temperature oxidation and hydration reaction respectively by using the traditional Hummers method. Longer oxidation times and large amounts of oxidizing agent ensure the stripping effect, but introduce more defect sites. Through hydration and washing processes, the transverse size of the graphene oxide is greatly reduced under the action of water molecules and mechanical force, and the performance of a rear-end product is seriously influenced. In addition, the use of a large amount of an oxidizing agent not only increases the cost of use and post-treatment, but also causes environmental pollution. Therefore, it is urgently needed to develop a preparation method of graphene oxide with low cost, high exfoliation and large size.
Generally, graphene having a size of more than 50 μm is called large-sized graphene, and when large-sized graphene oxide is prepared by the Hummers method, large-sized graphite is required as a raw material. CN113860295, namely graphene oxide prepared from large-particle-size flake graphite, adopts large-particle-size graphite of 45 to 325 μm, firstly performs pre-intercalation with concentrated sulfuric acid and hydrogen peroxide to obtain expanded graphite, adds the expanded graphite into a concentrated sulfuric acid and phosphoric acid mixed acid solution to perform a protection reaction, and then performs an oxidation reaction and a hydration stage to prepare the large-size graphene oxide. However, the use and discharge of phosphoric acid causes environmental pollution problems and increases the use and purification costs. In order to make the preparation method relatively green and environment-friendly, CN107140632, "a preparation method of large-sized graphene oxide lamella with high mechanical strength", adopts large-sized flake graphite as a raw material, and prepares large-sized graphene oxide by adding potassium persulfate and performing ultrasonic-assisted intercalation reaction. Although the method has high oxidation and stripping efficiency, the size of graphene oxide is inevitably reduced to a certain extent by the ultrasonic assistance. In order to introduce a new method for accelerating the reaction rate, CN111925637, a rapid curing unsaturated polyester resin for vacuum introduction, introduces a compound accelerator E1 and the unsaturated polyester resin into a forming die for curing reaction under the vacuum-pumping process condition, greatly accelerates the curing reaction rate among systems, eliminates bubbles in the reaction process, shortens the demolding time and saves the cost.
Disclosure of Invention
One object of the present invention is to provide a method for preparing graphene oxide, which accelerates the reaction rate and reduces the amount of oxidant through a vacuum pumping process, and simultaneously prepares high-exfoliation large-size graphene oxide.
In order to achieve the purpose, the scheme is as follows:
a preparation method of graphene oxide comprises the following steps:
mixing graphite and concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under a vacuum condition to obtain a mixture B;
adding an oxidant into the mixture B, heating, vacuumizing, and reacting under a vacuum condition to obtain a mixture C;
and carrying out suction filtration on the mixture C, and washing to obtain the graphene oxide.
Preferably, the reaction temperature when the graphite and the concentrated sulfuric acid are mixed to obtain the mixture A is 10 to 15 ℃.
Preferably, the mixture A is vacuumized after adding the expanding agent to reach a vacuum degree of-0.07 MPa to-0.1 MPa.
Preferably, in the step of reacting under vacuum condition to obtain the mixture B, the reaction time is 0.8-1.5 h; the reaction temperature is 15-20 ℃.
Preferably, the method further comprises: after the mixture B is obtained, the temperature of the mixture B is reduced to 0-5 ℃, and then the oxidant is added.
Preferably, in the step of reacting the mixture C under vacuum condition, the reaction time is 1.5-2.2 h.
Preferably, the graphite is any one of crystalline flake graphite and expanded graphite, the mass percentage of carbon in the graphite is 95-99.99 wt.%, and the particle size of the graphite is 50-200 meshes.
Preferably, the expanding agent is persulfate, the persulfate comprises one or two of sodium persulfate and potassium persulfate, and the using amount of the expanding agent is 5.0-8.0 times that of the graphite.
Preferably, the oxidant is potassium permanganate, and the dosage of the oxidant is 1.5-2.0 times of that of graphite.
The scheme has the following beneficial effects:
1. the consumption of the oxidant required by the traditional Hummers method is usually 4.0 times of that of the graphite, and compared with the consumption of the oxidant required by the traditional Hummers method, the consumption of the oxidant used by the method is 2.0 times of that of the graphite, and is reduced by 50%.
2. The length of the primary oxidation stage in the traditional Hummers method needs 4 hours of reaction, and the method reduces the oxidation time to 2 hours by a vacuumizing process, thereby saving energy consumption and cost.
3. The average size of the graphene oxide prepared by the method is 90 mu m (D50), and the graphene oxide has the characteristic of uniform large size.
Drawings
In order to illustrate the implementation of the solution more clearly, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the solution, and that other drawings may be derived from these drawings by a person skilled in the art without inventive effort.
Fig. 1 is an optical microscope photograph of graphene oxide prepared in example 1;
FIG. 2 is an optical microscope photograph of graphene oxide prepared in example 2;
FIG. 3 is an optical microscope photograph of graphene oxide prepared in example 3;
fig. 4 is an optical microscope photograph of graphene oxide prepared in example 4;
FIG. 5 is an optical microscope photograph of graphene oxide prepared in example 5;
FIG. 6 is a graph showing the results of particle size analyzer measurements (see D50 particle size data).
Detailed Description
Embodiments of the present solution are described in further detail below. It is clear that the described embodiments are only a part of the embodiments of the present solution, and not an exhaustive list of all embodiments. It should be noted that, in the present embodiment, features of the embodiment and the embodiment may be combined with each other without conflict.
The state of stage1 in the present application is a state in which an intercalating agent is present between 2 adjacent graphene sheets.
As the traditional Hummers method for preparing the graphene oxide needs to add a large amount of oxidant in an oxidation stage, and the oxidation time is long. Resulting in excessive oxidation and breakage of the product and greatly reducing the transverse dimension of the graphene oxide. The small-size graphene oxide not only reduces the yield of finished products, but also influences the electric conduction and heat conduction performance of the graphene.
The inventor of the application proposes to adopt the process of evacuation processing respectively in pre-intercalation and oxidation stage, because the influence of vacuum, only can let the interlamellar spacing of scale graphite inseparabler and laminate, but persulfate has taken place chemical reaction under the concentrated acid system, its mechanism is when the intercalation stage, persulfate has generated hydrogen sulfate radical and oxygen under the system of concentrated acid, can accelerate the desorption of oxygen through the evacuation, hydrogen sulfate radical that produces is favorable to forming the graphite compound of stage1 state in the time of quickening reaction rate, the hydrogen sulfate radical that produces has slightly inserted the graphite interlayer, its volume phase has expanded several times than original scale graphite after leading to pre-intercalation.
The inventor of the application prepares the graphene oxide with low oxidation and large size by respectively performing vacuum pumping processes in a preamplification stage and an oxidation stage in a Hummers system.
Because the persulfate generates hydrogen sulfate and oxygen in a concentrated sulfuric acid system in the pre-intercalation stage, the removal of the oxygen can be accelerated by vacuumizing, the hydrogen sulfate generated while the reaction rate is accelerated is favorable for forming a graphitized intercalation substance in a stage1 state, the reaction is shown as a formula 1,
2S 2 O 8 2- +2H 2 O→4HSO 4 - +O 2 ↓ (reaction in concentrated acid environment) (1)
The vacuum pumping process during the oxidation stage can promote the diffusion of the oxidant (high manganese anhydride) between layers, thereby improving the utilization rate of the oxidant and avoiding the size reduction caused by long-time oxidation and stirring.
The reaction mechanism of the oxidation stage is shown in formula 2 and formula 3:
KMnO 4 +3H 2 SO 4 →k + +MnO 3 + +H 3 O + +3HSO 4 - (2)
MnO 3 + +MnO 4 - →Mn 2 O 7 (high manganese acid anhydride) (3)
According to the method, the vacuumizing reaction is carried out in the oxidation stage, so that the reaction rate can be accelerated, the reaction time can be shortened, the diffusion of the oxidant between graphite layers can be promoted, and the stripping and large-size characteristics of the graphene oxide can be guaranteed while the amount of the oxidant is small.
According to the method provided by the application, by adding a vacuumizing process in the stages of pre-intercalation and oxidation, the consumption of an oxidant is reduced by 50% and the consumption of sulfuric acid is reduced by 30% compared with the original Hummers method. And avoids the problems that the preparation time of the original Hummers method is long and the size of the prepared graphene oxide is influenced due to long-time mechanical force action, and the cost and the energy consumption are increased due to the use of excessive oxidant.
The present application is illustrated by the following specific examples.
Example 1
The preparation method of the graphene oxide by using the conventional Hummers method comprises the following steps:
1. placing 100-150 meshes of crystalline flake graphite and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. slowly adding potassium permanganate with the graphite dosage of 4.0 times into the mixture A in the step 1, slowly heating to 35 ℃, and carrying out oxidation reaction for 4 hours to obtain a mixture B;
3. and (3) slowly adding deionized water into the mixture B obtained in the step (2), and then carrying out suction filtration and washing processes to obtain the graphene oxide.
The obtained graphene oxide was placed under an optical microscope, and the characterization is shown in fig. 1, wherein a large number of thick pieces of graphene oxide and small particle size are observed, and the average size (D50) of the obtained product measured by a nanometer particle sizer is about 20 μm.
Example 2
A preparation method of low-oxidation large-size graphene oxide comprises the following steps:
1. putting 100-150 meshes of crystalline flake graphite and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. adding sodium persulfate with the amount of 5.0 times of that of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum pumping reaction (the vacuum degree is-0.07 MPa), keeping the temperature at 15 ℃, and carrying out intercalation for 1h;
3. after the vacuum is released, slowly adding potassium permanganate with the graphite dosage of 2.0 times into the mixture B in the step 2 to obtain a mixture C, slowly heating to 35 ℃, and continuing vacuumizing (the vacuum degree is-0.07 MPa) for oxidation reaction for 2 hours;
4. and (4) after the vacuum is relieved, slowly adding deionized water into the mixture C obtained in the step (3), and performing suction filtration and washing to obtain the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 2, the size of the graphene oxide prepared by adding the pre-intercalation stage and the vacuum pumping reaction is obviously increased, and the average size (D50) of the prepared product is 75 micrometers measured by a nanometer particle size analyzer.
Example 3
A preparation method of low-oxidation large-size efficient graphene oxide comprises the following steps:
1. placing 100-150 meshes of crystalline flake graphite and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. adding potassium persulfate with the amount of 5.0 times that of graphite into the mixture A in the step 1 to obtain a mixture B, performing vacuum pumping reaction (the vacuum degree is-0.1 MPa), keeping the temperature at 15 ℃, and performing intercalation for 1 hour;
3. after the vacuum is released, slowly adding potassium permanganate with the graphite dosage of 2.0 times into the mixture B in the step 2 to obtain a mixture C, slowly heating to 35 ℃, and continuing vacuumizing (the vacuum degree is-0.1 MPa) for oxidation reaction for 2 hours;
4. and (4) after the vacuum is relieved, slowly adding deionized water into the mixture C obtained in the step (3), and performing suction filtration and washing to obtain the graphene oxide.
The obtained graphene oxide was placed under an optical microscope, and the characterization is shown in fig. 3, and it can be observed that the size of the obtained graphene oxide was further increased after increasing the vacuum degree, and the average size (D50) of the obtained product was 85 μm as measured by a nano-particle sizer.
Example 4
A preparation method of low-oxidation large-size efficient graphene oxide comprises the following steps:
1. putting 100-150 meshes of crystalline flake graphite and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. adding potassium persulfate with the amount of 8.0 times that of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum pumping reaction (the vacuum degree is-0.1 MPa), keeping the temperature at 15 ℃, and carrying out intercalation for 1h;
3. after the vacuum is released, slowly adding potassium permanganate with the amount of 1.5 times that of the graphite into the mixture B in the step 2 to obtain a mixture C, slowly heating to 35 ℃, and continuing vacuumizing (the vacuum degree is-0.1 MPa) for oxidation reaction for 2 hours;
4. and (4) after the vacuum is relieved, slowly adding deionized water into the mixture C obtained in the step (3), and performing suction filtration and washing to obtain the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 4, the purpose of reducing cost by further increasing the consumption of persulfate and reducing the consumption of potassium permanganate can be observed, and the size is basically not changed. The average size (D50) of the product obtained was 88 μm as measured by a nanometer particle sizer.
Example 5
A preparation method of low-oxidation large-size efficient graphene oxide comprises the following steps:
1. placing expandable graphite of 100-150 meshes and concentrated sulfuric acid into a reaction kettle for premixing to obtain a mixture A, and setting the temperature to be 10 ℃;
2. adding potassium persulfate with the amount of 8.0 times that of graphite into the mixture A in the step 1 to obtain a mixture B, carrying out vacuum pumping reaction (the vacuum degree is-0.1 MPa), keeping the temperature at 15 ℃, and carrying out intercalation for 1h;
3. after the vacuum is released, slowly adding potassium permanganate with the amount being 1.5 times that of the graphite into the mixture B in the step 2 to obtain a mixture C, slowly heating to 35 ℃, and continuously vacuumizing (the vacuum degree is-0.1 MPa) for oxidation reaction for 2 hours;
4. and (4) after the vacuum is relieved, slowly adding deionized water into the mixture C obtained in the step (3), and performing suction filtration and washing to obtain the graphene oxide.
The prepared graphene oxide is placed under an optical microscope, the characterization is shown in fig. 5, and the stripping effect of the graphene oxide is better after the graphite raw material is replaced. The average size (D50) of the obtained product was 90um as measured by a nanometer particle size analyzer.
Compared with the prior art, the method can reduce the using amount of the oxidant and shorten the oxidation time through the vacuum pumping process in the pre-intercalation and oxidation stages, so that the large-size and high-stripping graphene oxide is obtained.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (9)
1. A preparation method of graphene oxide is characterized by comprising the following steps:
mixing graphite and concentrated sulfuric acid to obtain a mixture A, adding an expanding agent into the mixture A, vacuumizing, and reacting under a vacuum condition to obtain a mixture B;
adding an oxidant into the mixture B, heating, vacuumizing, and reacting under a vacuum condition to obtain a mixture C;
and carrying out suction filtration on the mixture C, and washing to obtain the graphene oxide.
2. The method according to claim 1, wherein the reaction temperature for mixing graphite with concentrated sulfuric acid to obtain the mixture A is 10 to 15 ℃.
3. The process according to claim 1, wherein the mixture A is evacuated to a degree of vacuum of-0.07 MPa to-0.1 MPa after the addition of the expanding agent.
4. The method according to claim 1, wherein in the step of reacting under vacuum to obtain the mixture B, the reaction time is 0.8 to 1.5 hours; the reaction temperature is 15-20 ℃.
5. The method of claim 1, further comprising:
after the mixture B is obtained, the temperature of the mixture B is reduced to 0-5 ℃, and then the oxidant is added.
6. The method of claim 1, wherein the reaction time is 1.5 to 2.2 hours in the step of reacting the mixture C under vacuum.
7. The preparation method according to claim 1, wherein the graphite is any one of flake graphite and expanded graphite, the mass percentage of carbon in the graphite is 95-99.99 wt%, and the particle size of the graphite is 50-200 mesh.
8. The production method according to claim 1, wherein the swelling agent is a persulfate, the persulfate includes one or both of sodium persulfate and potassium persulfate, and the amount of the swelling agent is 5.0 to 8.0 times that of the graphite.
9. The preparation method according to claim 1, wherein the oxidant is potassium permanganate, and the dosage of the oxidant is 1.5-2.0 times of that of graphite.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| US20150175426A1 (en) * | 2012-08-28 | 2015-06-25 | Wuhan University | Method for low-temperature preparation of graphene and of graphene-based composite material |
| CN105197918A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | High-quality graphene and quick preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935035A (en) * | 2010-09-02 | 2011-01-05 | 中国科学院宁波材料技术与工程研究所 | Ultra-low temperature thermal expansion preparation method of high specific area graphene |
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| US20150175426A1 (en) * | 2012-08-28 | 2015-06-25 | Wuhan University | Method for low-temperature preparation of graphene and of graphene-based composite material |
| CN105197918A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | High-quality graphene and quick preparation method thereof |
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