CN109761232B - Device and method for preparing graphite intercalation compound - Google Patents
Device and method for preparing graphite intercalation compound Download PDFInfo
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- CN109761232B CN109761232B CN201910242215.7A CN201910242215A CN109761232B CN 109761232 B CN109761232 B CN 109761232B CN 201910242215 A CN201910242215 A CN 201910242215A CN 109761232 B CN109761232 B CN 109761232B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 81
- 239000010439 graphite Substances 0.000 title claims abstract description 81
- 238000009830 intercalation Methods 0.000 title claims abstract description 53
- 230000002687 intercalation Effects 0.000 title claims abstract description 53
- 150000001875 compounds Chemical class 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000007789 gas Substances 0.000 claims abstract description 58
- 239000010453 quartz Substances 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011261 inert gas Substances 0.000 claims abstract description 20
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000012670 alkaline solution Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 6
- 238000001962 electrophoresis Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 239000011593 sulfur Substances 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- -1 hydrogen ions Chemical class 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a device and a method for preparing a graphite intercalation compound, wherein the device comprises a sulfuric acid gas generating device, an electrochemical reaction device, an inert gas supply device and a sulfuric acid gas processing device; the electrochemical reaction device comprises a quartz tube, two porous electrode plates and a power supply; the two porous electrode plates are arranged in parallel in the quartz tube, the plane direction of the two porous electrode plates is vertical to the axial direction of the quartz tube, and the graphite raw material is fixed on the porous electrode plate connected with the positive electrode of the power supply; the gas outlet of the inert gas supply device is connected with the gas inlet of the quartz tube; the sulfuric acid gas generating device comprises a sulfur trioxide gas supply device and a water vapor generating device, an outlet of the sulfuric acid gas generating device extends into the middle of the two electrode plates, and a gas outlet of the quartz tube is connected with a gas inlet of the sulfuric acid gas processing device. The invention reduces the consumption of sulfuric acid in the preparation process of the graphite intercalation compound, saves the preparation cost and reduces the pollution degree to the environment.
Description
Technical Field
The invention relates to the technical field of graphite processing, in particular to a device and a method for preparing a graphite intercalation compound.
Background
Graphite is an important strategic resource in China. Expanded graphite is one of the important directions for the further processing of graphite. In graphite crystals, the layer-to-layer distances are large, about 0.335nm, and are bound by van der waals forces. Under appropriate conditions, natural flake graphite can be intercalated between graphite platelets by physical or chemical means with intercalant molecules to form a graphite intercalation compound, also known as expandable graphite. When the graphite is heated at high temperature, the compound inserted between the layers is heated and rapidly decomposed to generate gas, so that the graphite expands along the C-axis direction to form expanded graphite.
The expanded graphite has the characteristics of good adsorption, corrosion resistance, high temperature resistance and the like due to the unique network-shaped microporous structure. The expanded graphite and the products thereof have wide application temperature range, can keep excellent elasticity and compressibility under high temperature and low temperature conditions, and are widely used for manufacturing flexible graphite products, environment-friendly adsorption materials, high-energy battery electrode materials, fireproof flame-retardant materials, biomedical materials, sealing materials and the like.
The intercalation effect of the expandable graphite is the key to influence the performance of the flexible graphite product and the graphite adsorption material, and the existing preparation methods of the expandable graphite can be divided into a chemical oxidation method, an electrochemical method, an explosion method, a gas phase diffusion method and the like, wherein the chemical oxidation method adopts natural crystalline flake graphite as a raw material, hydrogen peroxide and the like as an oxidant, and concentrated sulfuric acid as a main intercalation agent for intercalation. The prepared graphite intercalation compound is expanded in a high temperature oven or a microwave oven. The expansion in the high temperature furnace is due to the pressure generated by the instantaneous volatilization of the gas immediately decomposed when the compound between the graphite layers is heated, the layer surface of the graphite is pushed away along the direction of the C axis by overcoming the Van der Waals force, and the thickness of the graphite sheet is expanded by a high factor, thereby forming the expanded graphite. The method has the problems of high sulfur content, high sulfuric acid consumption, high cost, poor intercalation effect, difficult control of intercalation order, large environmental pollution and the like of the prepared expanded graphite.
Disclosure of Invention
The invention aims to provide a device and a method for preparing a graphite intercalation compound, which are used for reducing the sulfur content of the graphite intercalation compound and the consumption of sulfuric acid during preparation of the graphite intercalation compound, reducing the cost and reducing the pollution to the environment.
In order to achieve the purpose, the invention provides the following scheme:
the invention discloses a device for preparing a graphite intercalation compound, which comprises a sulfuric acid gas generating device, an electrochemical reaction device, an inert gas supply device and a sulfuric acid gas processing device;
the electrochemical reaction device comprises a quartz tube, two porous electrode plates and a power supply; the two porous electrode plates are arranged in the quartz tube in parallel, the plane directions of the two porous electrode plates are vertical to the axial direction of the quartz tube, and graphite raw materials are fixed on the porous electrode plates connected with the positive electrode of the power supply; the two ends of the quartz tube are respectively provided with an air inlet and an air outlet, and the air outlet of the inert gas supply device is connected with the air inlet of the quartz tube;
the sulfuric acid gas generating device comprises a sulfur trioxide gas supply device and a water vapor generating device, wherein an outlet of the sulfuric acid gas generating device is formed by extending a gas inlet of the quartz tube into the middle of the porous electrode plate, and a gas outlet of the quartz tube is connected with a gas inlet of the sulfuric acid gas processing device.
Optionally, the apparatus for preparing a graphite intercalation compound further comprises a heating apparatus, and the heating apparatus heats the quartz tube to 105-800 ℃.
Optionally, the power supply is a dc stabilized voltage supply, the voltage of the dc stabilized voltage supply is adjustable, and the dc stabilized voltage supply provides working voltage for the two porous electrode plates.
Optionally, the sulfuric acid gas treatment device comprises an alkaline solution for absorbing sulfuric acid vapor discharged from the gas outlet of the quartz tube.
Optionally, the graphite raw material is flake graphite.
The invention also discloses a method for preparing the graphite intercalation compound, which is applied to the device for preparing the graphite intercalation compound and comprises the following steps:
arranging two porous electrode plates which are axially vertical to the quartz tube in the quartz tube, and fixing a graphite raw material on the porous electrode plates connected with the positive electrode of a power supply;
sulfuric acid mist generated by sulfur trioxide gas and water vapor is introduced into the middle position of the two porous electrode plates in the quartz tube;
applying a working voltage to the porous electrode plate;
the sulfuric acid mist is ionized and subjected to electrophoresis and intercalation reaction under the driving action of the working voltage; and after the intercalation reaction is finished, introducing inert gas into the gas inlet of the quartz tube, wherein the inert gas carries residual harmful gas in the quartz tube into an alkaline solution.
Optionally, the graphite raw material is flake graphite.
Optionally, the quartz tube is heated to a temperature of 105 to 800 ℃.
According to the invention content provided by the invention, the invention discloses the following technical effects: the invention provides a device and a method for preparing a graphite intercalation compound.A sulfuric acid molecule is introduced in a sulfuric acid vapor state, sulfuric acid gas molecules in the sulfuric acid vapor are ionized into hydrogen sulfate ions and hydrogen ions with small granularity, the electrophoretic movement of the hydrogen sulfate ions and the directional insertion between graphite layers are realized by virtue of electrostatic attraction and concentration difference, and the control of intercalation order and the improvement of intercalation effect can be realized by regulating and controlling voltage; the in-situ generation of the sulfuric acid vapor is adopted, the existence and the residue of redundant sulfuric acid molecules in a reaction system are reduced as much as possible, the sulfur content of the product is reduced, the product is more suitable for certain high-end application occasions with lower requirements on the sulfur content, and the preparation cost and the pollution degree to the environment are reduced at the same time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for preparing a graphite intercalation compound according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for preparing a graphite intercalation compound according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a device and a method for preparing a graphite intercalation compound, which can reduce the sulfur content of the graphite intercalation compound and the consumption of sulfuric acid during preparation of the graphite intercalation compound, thereby reducing the cost and reducing the environmental pollution.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a schematic structural diagram of an apparatus for preparing a graphite intercalation compound according to an embodiment of the present invention, and as shown in fig. 1, the apparatus for preparing a graphite intercalation compound according to the present invention includes: a sulfuric acid gas generator 102, an electrochemical reactor 101, an inert gas supplier 103, and a sulfuric acid gas treatment device 104;
the electrochemical reaction device 101 comprises a quartz tube, two porous electrode plates and a power supply; the two porous electrode plates are arranged in parallel in the quartz tube, the plane direction of the two porous electrode plates is vertical to the axial direction of the quartz tube, and the flake graphite raw material to be reacted is fixed on the porous electrode plate connected with the positive electrode of the power supply; the two ends of the quartz tube are respectively provided with an air inlet and an air outlet, and the air outlet of the inert gas supply device is connected with the air inlet of the quartz tube;
the sulfuric acid gas generating device 102 comprises a sulfur trioxide gas supply device and a water vapor generating device, an outlet of the sulfuric acid gas generating device 102 extends into the middle of the two porous electrode plates from a gas inlet of a quartz tube, and a gas outlet of the quartz tube is connected with a gas inlet of the sulfuric acid gas processing device 104.
The device for preparing the graphite intercalation compound also comprises a heating device, and the heating device heats the quartz tube to 105-800 ℃.
The power supply is a direct current stabilized voltage supply, the voltage of the direct current stabilized voltage supply can be adjusted, working voltage is provided for the two porous electrode plates, and driving force is provided for the electrophoresis of sulfuric acid vapor and the intercalation reaction of graphite.
The sulfuric acid gas treatment device 104 comprises an alkaline solution for absorbing sulfuric acid vapor discharged from the outlet of the quartz tube.
The inert gas supply device 103 provides stable inert gas for the quartz tube, after the intercalation reaction is finished, the stable inert gas is introduced into the electrochemical reaction device, and the inert gas carries all the waste gas in the electrochemical reaction device and is introduced into the sulfuric acid gas treatment device 104.
The present invention also provides a method for preparing a graphite intercalation compound, which is applied to the above apparatus for preparing a graphite intercalation compound, and fig. 2 is a schematic flow chart of a method for preparing a graphite intercalation compound according to the present invention, as shown in fig. 2, the method includes:
step 201: arranging two porous electrode plates which are axially vertical to the quartz tube in the quartz tube, and fixing the graphite raw material on the porous electrode plate connected with the positive electrode of the power supply;
step 202: sulfuric acid mist generated by sulfur trioxide gas and water vapor is introduced into the middle position of the two porous electrode plates in the quartz tube;
step 203: applying a working voltage to the porous electrode plate;
step 204: the sulfuric acid mist is ionized and is driven by working voltage to carry out electrophoresis and intercalation reaction; after the intercalation reaction is finished, introducing inert gas into the gas inlet of the quartz tube, and carrying residual harmful gas in the quartz tube into alkaline solution by the inert gas
Wherein the step 202 further comprises heating the quartz tube to make the temperature of the quartz tube be 105-800 ℃.
Wherein, step 204 further comprises: the sulfuric acid vapor is ionized to generate hydrogen sulfate ions and hydrogen ions; the hydrogen sulfate ions move to a porous electrode plate connected with the positive electrode of the power supply due to electrostatic attraction and concentration difference and contact with the graphite raw material fixed on the porous electrode plate; under the drive of working voltage, hydrogen sulfate ions enter the graphite interlayer to obtain a graphite interlayer compound;
and introducing inert gas into the electrochemical reaction device after obtaining the graphite intercalation compound, and carrying waste gas in the electrochemical reaction device, mainly sulfuric acid vapor, into the alkaline solution.
The invention provides a device and a method for preparing a graphite intercalation compound, wherein sulfuric acid is introduced in a sulfuric acid vapor state, sulfuric acid gas molecules in the sulfuric acid vapor are ionized into hydrogen sulfate ions and hydrogen ions with small granularity, the electrophoretic movement of the hydrogen sulfate ions and the directional insertion between graphite layers are realized by virtue of electrostatic attraction and concentration difference, and the control of intercalation orders and the improvement of intercalation effect can be realized by regulating and controlling voltage; the in-situ generation of the sulfuric acid vapor is adopted, so that the existence of redundant sulfuric acid molecules in a reaction system can be reduced as much as possible, the sulfur content of the product is reduced, the product is more suitable for certain high-end application occasions with lower requirements on the sulfur content, and the preparation cost and the pollution degree to the environment are reduced at the same time. The invention realizes the absorption treatment of the sulfuric acid gas through the inert gas supply device and the sulfuric acid gas treatment absorption device, and compared with the traditional method adopting liquid concentrated sulfuric acid, the method has the advantages of smaller treatment capacity of the waste sulfuric acid and high treatment efficiency.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (7)
1. An apparatus for preparing a graphite intercalation compound, comprising a sulfuric acid gas generation device, an electrochemical reaction device, an inert gas supply device and a sulfuric acid gas treatment device;
the electrochemical reaction device comprises a quartz tube, two porous electrode plates and a power supply; the two porous electrode plates are arranged in the quartz tube in parallel, the plane directions of the two porous electrode plates are vertical to the axial direction of the quartz tube, and graphite raw materials are fixed on the porous electrode plates connected with the positive electrode of the power supply; the two ends of the quartz tube are respectively provided with an air inlet and an air outlet, and the air outlet of the inert gas supply device is connected with the air inlet of the quartz tube;
the sulfuric acid gas generating device comprises a sulfur trioxide gas supply device and a water vapor generating device, and an outlet of the sulfuric acid gas generating device extends into the middle of the two porous electrode plates from an air inlet of the quartz tube; the gas outlet of the quartz tube is connected with the gas inlet of the sulfuric acid gas treatment device;
the sulfuric acid gas treatment device comprises alkaline solution used for absorbing sulfuric acid vapor discharged from the quartz tube gas outlet.
2. The apparatus for preparing a graphite intercalation compound according to claim 1, further comprising a heating means for heating the quartz tube to 105-800 ℃.
3. The apparatus for preparing a graphite intercalation compound according to claim 1, wherein the power supply is a regulated dc voltage supply, the voltage of which is adjustable, and the regulated dc voltage supply supplies an operating voltage to both of the porous electrode plates.
4. The apparatus for preparing a graphite intercalation compound according to claim 1, wherein the graphite raw material is flake graphite.
5. A method for preparing a graphite intercalation compound, characterized by being applied to the apparatus for preparing a graphite intercalation compound according to any one of claims 1 to 4, the method comprising:
arranging two porous electrode plates which are axially vertical to the quartz tube in the quartz tube, and fixing a graphite raw material on the porous electrode plates connected with the positive electrode of a power supply;
sulfuric acid mist generated by sulfur trioxide gas and water vapor is introduced into the middle position of the two porous electrode plates in the quartz tube;
applying a working voltage to the porous electrode plate;
the sulfuric acid mist is ionized and subjected to electrophoresis and intercalation reaction under the driving action of the working voltage; and after the intercalation reaction is finished, introducing inert gas into the gas inlet of the quartz tube, wherein the inert gas carries residual harmful gas in the quartz tube into an alkaline solution.
6. The method for preparing a graphite intercalation compound according to claim 5, wherein the graphite starting material is flake graphite.
7. The method for preparing a graphite intercalation compound according to claim 5, wherein the quartz tube is heated to a temperature of 105 to 800 ℃.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE663737A (en) * | 1964-05-11 | 1965-09-01 | ||
| CN1061388A (en) * | 1991-12-26 | 1992-05-27 | 清华大学 | Method for making expansible graphite |
| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
| CN105442072A (en) * | 2015-12-31 | 2016-03-30 | 哈尔滨工业大学 | Method for preparing super tough fibers of shell-simulation structures and helical structures simultaneously in batches |
| CN106698406A (en) * | 2017-02-17 | 2017-05-24 | 德阳烯碳科技有限公司 | Process for preparing graphite according to electrochemical method |
| CN107601488A (en) * | 2017-09-08 | 2018-01-19 | 深圳大学 | A kind of preparation method of graphene oxide |
| CN109264708A (en) * | 2018-07-25 | 2019-01-25 | 浙江普绿世新材料科技有限公司 | A kind of manufacturing method of two-dimensional material |
-
2019
- 2019-03-28 CN CN201910242215.7A patent/CN109761232B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE663737A (en) * | 1964-05-11 | 1965-09-01 | ||
| CN1061388A (en) * | 1991-12-26 | 1992-05-27 | 清华大学 | Method for making expansible graphite |
| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
| CN105442072A (en) * | 2015-12-31 | 2016-03-30 | 哈尔滨工业大学 | Method for preparing super tough fibers of shell-simulation structures and helical structures simultaneously in batches |
| CN106698406A (en) * | 2017-02-17 | 2017-05-24 | 德阳烯碳科技有限公司 | Process for preparing graphite according to electrochemical method |
| CN107601488A (en) * | 2017-09-08 | 2018-01-19 | 深圳大学 | A kind of preparation method of graphene oxide |
| CN109264708A (en) * | 2018-07-25 | 2019-01-25 | 浙江普绿世新材料科技有限公司 | A kind of manufacturing method of two-dimensional material |
Non-Patent Citations (4)
| Title |
|---|
| Electrochemistry of graphite intercalation compounds;M. Noel et al.;《Journal of Power Sources》;19981231;第72卷;第53-65页 * |
| Studies on the Kinetics of Intercalation of Graphite by FeC13 Vapor;W. METZ et al.;《Materials Science and Engineering》;19771231;第31卷;第119-121页 * |
| THE CHEMISTRY AND CHARACTERISTICS OF NITRIC ACID-GRAPHITE INTERCALATION;SOPHIA R. SU et al.;《Hat. Res. Soc. Symp. Proc.》;19831231;第20卷;第231-236页 * |
| 石墨插层技术的筛选和应用现状;罗立群;《现代化工》;20161130;第36卷(第11期);第32-38页 * |
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Effective date of registration: 20230719 Address after: 012100 West Zone of Fengzhen Industrial Park, Ulanqab, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Huayang high tech Material Technology Co.,Ltd. Address before: 100000 Beijing City, Haidian District Institute of Rutosids No. 11 Patentee before: CHINA University OF MINING AND TECHNOLOGY BEIJING |
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Inventor after: Li Jihui Inventor after: Ma Liqiang Inventor after: Huang Gen Inventor after: Shen Wanci Inventor after: Wei Luo Inventor after: Yang Yunlong Inventor after: Feng Meng Inventor after: Yang Yimin Inventor before: Li Jihui Inventor before: Ma Liqiang Inventor before: Huang Gen Inventor before: Huang Zhenghong Inventor before: Shen Wanci Inventor before: Wei Luo Inventor before: Yang Yunlong Inventor before: Feng Meng Inventor before: Yang Yimin |
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