CN116495727B - Preparation method and application of expanded graphene material by using popcorn machine - Google Patents
Preparation method and application of expanded graphene material by using popcorn machine Download PDFInfo
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- CN116495727B CN116495727B CN202310566012.XA CN202310566012A CN116495727B CN 116495727 B CN116495727 B CN 116495727B CN 202310566012 A CN202310566012 A CN 202310566012A CN 116495727 B CN116495727 B CN 116495727B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 25
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 19
- 241000482268 Zea mays subsp. mays Species 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 title abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 32
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002699 waste material Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007770 graphite material Substances 0.000 claims abstract description 15
- 238000009830 intercalation Methods 0.000 claims abstract description 14
- 230000002687 intercalation Effects 0.000 claims abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- -1 wherein S1 Substances 0.000 claims abstract description 9
- QTJOIXXDCCFVFV-UHFFFAOYSA-N [Li].[O] Chemical compound [Li].[O] QTJOIXXDCCFVFV-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 17
- WFLRGOXPLOZUMC-UHFFFAOYSA-N [Li].O=C=O Chemical compound [Li].O=C=O WFLRGOXPLOZUMC-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 5
- 229910013716 LiNi Inorganic materials 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000138 intercalating agent Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/52—Reclaiming serviceable parts of waste cells or batteries, e.g. recycling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses a preparation method and application of an expanded graphene material by using a popcorn machine, and relates to the technical field of graphite materials, wherein S1, waste graphite in a negative electrode of a waste lithium battery is added into deionized water, and a first suspension is obtained by stirring; s2, performing hydrothermal intercalation on the first suspension in the step S1 to obtain a second suspension; s3, washing the second suspension obtained in the step S2 with deionized water and ethanol for multiple times, and drying in a vacuum drying oven to obtain a dried product; s4, placing the dried product in the S3 into a popcorn machine for instantaneous expansion to obtain the expanded graphene material. The invention adopts the steps, and sequentially adopts the hydrothermal intercalation method and the method that the pressure rapidly disappears and the instant expansion is carried out when the popcorn machine is started to obtain the expanded graphite material, the obtained expanded graphite material has a petal-shaped loose porous structure, and the obtained expanded graphite material with a three-dimensional structure has extremely large specific surface area.
Description
Technical Field
The invention relates to the technical field of graphite materials, in particular to a preparation method and application of an expanded graphene material by using a popcorn machine.
Background
The positive reactant of the lithium-oxygen battery is inexhaustible oxygen, and the theoretical specific energy of the positive reactant is far more than that of a commercial lithium-ion battery and even is similar to that of gasoline, so that the positive reactant has great application prospect in the field of Electric Vehicles (EV). The electrolyte stability and basic positive electrode reaction of lithium-oxygen batteries have been extensively studied, but due to the solid positive electrode product Li during discharge 2 O 2 Reduces reaction kinetics and shortens cycle life.
Reasonable pore structure design and good anode catalytic capability are key to solving the problem, and carbon materials are widely applied to lithium-oxygen batteries due to high conductivity, low price and porous structure, however, the synthesis and preparation of the carbon materials are always influenced by raw materials at present, so that the large-scale practical application of the carbon materials is not facilitated.
In recent years, waste lithium ion batteries have received much attention, and the most common anode materials in LIBs are types of carbon (e.g., graphite, soft carbon, hard carbon, carbon nanotubes, etc.). Wherein the graphite has a special lamellar structure, and can relatively stably insert and extract Li + . It has good stability, high conductivity, lower lithium insertion potential and higher theoretical capacity compared to other carbon materials. Because of these advantages, graphite dominates the LIB negative electrode market.
The main method for recovering graphite from anode is to burn together with cathode in high-temperature metallurgical process and release a great amount of greenhouse gas. However, the energy efficiency and carbon emission requirements of such recovery processes are contrary to the global goal of achieving carbon neutralization. Therefore, it is necessary to design a method for cooperatively treating waste graphite, and to combine the concepts of lithium oxygen battery/lithium carbon dioxide battery and graphite recovery to build a complete waste graphite recovery and reuse system.
Disclosure of Invention
The invention aims to provide a preparation method and application of an expanded graphene material using a popcorn machine, wherein the expanded graphene material is used as a positive electrode material of a lithium-oxygen battery, can provide more reactive sites for electrochemical reaction, improves the utilization efficiency of the material, and is beneficial to storage of discharge products.
In order to achieve the above purpose, the invention provides a preparation method of an expanded graphene material by using a popcorn machine, which comprises the following steps: s1, adding waste graphite in a negative electrode of a waste lithium battery into deionized water, and stirring to obtain a first suspension;
s2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle, performing hydrothermal intercalation by taking deionized water as an intercalation agent, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension;
s3, washing the second suspension obtained in the step S2 with deionized water and ethanol for multiple times, and drying in a vacuum drying oven to obtain a dried product;
s4, placing the dried product in the S3 into a popcorn machine, and performing instantaneous expansion at 200-250 ℃ and 1.0-2.0MPa to obtain the expanded graphene material.
Preferably, in S1, the mass ratio of waste graphite to deionized water is 1: (50-100).
Preferably, in S2, the hydrothermal intercalation reaction temperature is 150-220 ℃ and the reaction time is 10-20h.
Preferably, in S3, the washing times of deionized water are 1-3 times, and the washing times of ethanol are 1-3 times.
Preferably, in S3, the drying temperature of the vacuum drying oven is 60-80 ℃ and the drying time is 8-12h.
The application of the expanded graphene material prepared by the method is the application of the expanded graphene material in the preparation of a lithium oxygen battery or a lithium carbon dioxide battery.
Therefore, the preparation method and the application of the expanded graphene material using the popcorn machine have the beneficial effects that:
1. sequentially using a hydrothermal intercalation method using deionized water as an intercalating agent and a transient expansion method for quickly eliminating pressure when a popcorn machine is started to prepare waste graphite into an expanded graphite material, wherein the popcorn machine rotates and uses the interior of the popcorn machine to be heated uniformly, and the transient expansion enables the expanded graphite material to have a petal-shaped loose porous structure, so that the expanded graphite material with a three-dimensional structure has a very large specific surface area;
2. the expanded graphite material is used as the anode material of the lithium oxygen battery/lithium carbon dioxide battery, can provide more reactive sites for electrochemical reaction, improves the utilization efficiency of the material, and is beneficial to the storage of discharge products;
3. the lithium oxygen battery/lithium carbon dioxide battery anode prepared by using the expanded graphite material has higher pore channel utilization rate and connectivity, stronger mass transfer capability, satisfactory specific capacity and excellent cycle performance.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a scanning electron microscope image of an expanded graphite material in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a comparative sample in comparative example 1 of the present invention;
FIG. 3 is a graph showing the discharge curve test of the lithium-oxygen battery of example 5 of the present invention;
FIG. 4 is a charge/discharge overpotential test chart of the lithium-oxygen battery of example 5 of the present invention;
FIG. 5 is a graph showing the discharge curve test of the lithium carbon dioxide battery in example 6 of the present invention;
fig. 6 is a charge-discharge overpotential test chart of the lithium carbon dioxide battery in example 6 of the present invention.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
The present invention will be explained in more detail by the following examples, and the purpose of the present invention is to protect all changes and modifications within the scope of the present invention, and the present invention is not limited to the following examples.
Example 1
S1, adding 1g of waste graphite in the negative electrode of the waste lithium battery into 60mL of deionized water, and stirring for 30min to obtain a first suspension.
S2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle with the specification of 100mL, performing hydrothermal intercalation at 180 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension.
S3, washing the second suspension obtained in the step S2 with deionized water and ethanol for 3 times in sequence, and removing the residual LiNi in the waste graphite x Co y Mn 1-x-y O 2 And metal impurities such as simple substance Cu, al, na and the like are washed away. Drying in a vacuum drying oven at 80 ℃ for 12 hours to obtain a dried product.
S4, placing the dried product in the S3 in a sealed popcorn machine, performing instantaneous expansion at 250 ℃ and 1.5MPa, preserving for 5min, and removing the seal to obtain the expanded graphene material, as shown in figure 1.
Example 2
S1, adding 1g of waste graphite into 60mL of deionized water, and stirring for 30min to obtain a first suspension.
S2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle with the specification of 100mL, performing hydrothermal intercalation by taking deionized water as an intercalating agent at 180 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension.
S3, washing the second suspension obtained in the step S2 with deionized water and ethanol for 3 times in sequence, and removing the residual LiNi in the waste graphite x Co y Mn 1-x-y O 2 And metal impurities such as simple substance Cu, al, na and the like are washed away. Drying in a vacuum drying oven at 80 ℃ for 12 hours to obtain a dried product.
S4, placing the dried product in the S3 in a sealed popcorn machine, performing instantaneous expansion at 250 ℃ and 1.0MPa, preserving for 5min, and removing the seal to obtain the expanded graphene material.
Example 3
S1, adding 1g of waste graphite in the negative electrode of the waste lithium battery into 60mL of deionized water, and stirring for 30min to obtain a first suspension.
S2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle with the specification of 100mL, performing hydrothermal intercalation by taking deionized water as an intercalating agent at 150 ℃ for 20h, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension.
S3, washing the second suspension obtained in the step S2 with deionized water and ethanol for 3 times in sequence, and removing the residual LiNi in the waste graphite x Co y Mn 1-x-y O 2 And metal impurities such as simple substance Cu, al, na and the like are washed away. Drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain a dried product.
S4, placing the dried product in the S3 in a sealed popcorn machine, performing instantaneous expansion at 200 ℃ and 2.0MPa, preserving for 5min, and removing the seal to obtain the expanded graphene material.
Example 4
S1, adding 1g of waste graphite in the negative electrode of the waste lithium battery into 60mL of deionized water, and stirring for 30min to obtain a first suspension.
S2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle with the specification of 100mL, performing hydrothermal intercalation by taking deionized water as an intercalating agent at 220 ℃ for 10 hours, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension.
S3, washing the second suspension obtained in the step S2 with deionized water and ethanol for 3 times in sequence, and removing the residual LiNi in the waste graphite x Co y Mn 1-x-y O 2 And metal impurities such as simple substance Cu, al, na and the like are washed away. Drying in a vacuum drying oven at 80 ℃ for 8 hours to obtain a dried product.
S4, placing the dried product in the S3 in a sealed popcorn machine, performing instantaneous expansion at 200 ℃ and 2.0MPa, preserving for 5min, and removing the seal to obtain the expanded graphene material.
Example 5
S1, uniformly mixing the expanded graphene material obtained in the embodiment 1, conductive carbon black and polyvinylidene fluoride according to the ratio of 7:2:1, and adding N-methyl pyrrolidone to stir into slurry.
S2, uniformly spraying the slurry obtained in the step S1 on carbon paper by using a spray gun, and drying the carbon paper in a vacuum drying oven at 80 ℃ for 12 hours.
S3, slicing the carbon paper dried in the step S2 by using a puncher, and punching out electrode plates with the diameter of 10 mm.
S4, selecting the electrode plate in S3 as an anode, 10mm metal lithium as a cathode, 1M lithium triflate as an electrolyte, tetraethylene glycol dimethyl ether as a solvent, a whatman glass fiber filter membrane as a diaphragm, and selecting a 2032 type battery shell with holes.
S5, assembling the materials in the S4 into a battery according to the sequence of a battery cathode shell, a cathode, a diaphragm, an anode, foam nickel and a battery anode shell, dropwise adding a proper amount of electrolyte to assemble the battery to obtain a lithium oxygen battery, and carrying out electrochemical test on the lithium oxygen battery.
As shown in FIG. 3, the initial specific capacity of the lithium-oxygen battery was 11375mAh/g when the current density was 200mA/g, and 6238mAh/g when the current density was increased to 800 mA/g.
As shown in FIG. 4, when the current density is 200mA/g and the capacity is 500mAh, the first pass potential reaches 1.56V.
Example 6
S1, uniformly mixing the expanded graphene material obtained in the embodiment 1, conductive carbon black and polyvinylidene fluoride according to the ratio of 7:2:1, and adding N-methyl pyrrolidone to stir into slurry.
S2, uniformly spraying the slurry obtained in the step S1 on carbon paper by using a spray gun, and drying the carbon paper in a vacuum drying oven at 80 ℃ for 12 hours.
S3, slicing the carbon paper dried in the step S2 by using a puncher, and punching out electrode plates with the diameter of 10 mm.
S4, selecting the electrode plate in S3 as an anode, 10mm metal lithium as a cathode, 1M lithium triflate as an electrolyte, tetraethylene glycol dimethyl ether as a solvent, a whatman glass fiber filter membrane as a diaphragm, and selecting a 2032 type battery shell with holes.
S5, assembling the materials in S4 into a battery according to the sequence of the open-cell battery cathode shell, the cathode, the diaphragm, the anode, the foam nickel and the battery anode shell, dripping a proper amount of electrolyte to assemble the battery to obtain a lithium carbon dioxide battery, and carrying out electrochemical tests on the lithium carbon dioxide battery, as shown in fig. 5 and 6.
Comparative example 1
S1, adding 1g of waste graphite in the negative electrode of the waste lithium battery into 60mL of deionized water, and stirring for 30min to obtain a first suspension.
S2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle with the specification of 100mL, performing hydrothermal intercalation at 180 ℃ for 12 hours, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension.
And S3, washing the second suspension obtained in the step S2 with deionized water and ethanol for multiple times, and drying in a vacuum drying oven at 80 ℃ for 12 hours to obtain a dried product.
S4, placing the dried product in the S3 in a muffle furnace, and preserving for 5min at 250 ℃ to obtain a comparison sample, as shown in figure 2.
As can be seen from comparison between fig. 1 and fig. 2, in example 1, the pressure is rapidly reduced after the popcorn machine is started, and the expansion is performed instantaneously, so that the expanded graphite material has a petal-shaped loose porous structure, and the obtained expanded graphite material has a three-dimensional structure and a very large specific surface area. While the high temperature environment of comparative example 1 did not allow the graphene material to expand, the specific surface area was much lower than the expanded graphene material of example 1.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (3)
1. An application of expanded graphite in preparing a lithium oxygen battery or a lithium carbon dioxide battery is characterized in that: the expanded graphite material is applied to the preparation of a lithium oxygen battery or a lithium carbon dioxide battery;
the preparation method of the expanded graphite comprises the following steps:
s1, adding waste graphite in a negative electrode of a waste lithium battery into deionized water, and stirring to obtain a first suspension;
in S1, the mass ratio of waste graphite to deionized water is 1: (50-100);
s2, transferring the first suspension in the step S1 into a polytetrafluoroethylene lining reaction kettle, performing hydrothermal intercalation by taking deionized water as an intercalation agent, and naturally cooling to room temperature after the reaction is finished to obtain a second suspension;
s2, the hydrothermal intercalation reaction temperature is 150-220 ℃ and the reaction time is 10-20h;
s3, washing the second suspension obtained in the step S2 by using deionized water and ethanol in sequence, and drying in a vacuum drying oven to obtain a dried product;
s4, placing the dried product in the S3 into a popcorn machine, and performing instantaneous expansion at 200-250 ℃ and 1.0-2.0MPa to obtain the expanded graphite material.
2. Use of expanded graphite according to claim 1 for the preparation of lithium oxygen or lithium carbon dioxide batteries, characterized in that: in S3, the washing times of deionized water are 1-3 times, and the washing times of ethanol are 1-3 times.
3. Use of expanded graphite according to claim 1 for the preparation of lithium oxygen or lithium carbon dioxide batteries, characterized in that: and S3, drying the materials in a vacuum drying oven at the temperature of 60-80 ℃ for 8-12 hours.
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| KR20140112826A (en) * | 2013-03-14 | 2014-09-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Expanded Graphite or Graphene Fabricated by Physical Process And Method for Fabricating the same |
| CN103199321A (en) * | 2013-04-08 | 2013-07-10 | 中国科学院长春应用化学研究所 | Lithium air cell positive electrode material and preparation method of material |
| CN103259062A (en) * | 2013-04-17 | 2013-08-21 | 清华大学深圳研究生院 | Method for regenerating graphene by recovering waste lithium ion battery |
| CN103367765A (en) * | 2013-07-25 | 2013-10-23 | 哈尔滨工业大学 | Preparation method of multilayer graphite and method for preparing lithium-air battery cathode by using multilayer graphite |
| CN105366668A (en) * | 2015-11-04 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Method for preparing graphene through supercritical fluid |
| CN105905889A (en) * | 2016-06-06 | 2016-08-31 | 南通伟德动力电池研究所（普通合伙） | Method for producing graphene through high pressure hydrothermal expansion method |
| CN113942998A (en) * | 2021-09-03 | 2022-01-18 | 天津艾克凯胜石墨烯科技有限公司 | Porous graphene powder and preparation method and application thereof |
| CN114956072A (en) * | 2022-06-08 | 2022-08-30 | 中国科学院过程工程研究所 | Method for expanding natural graphite spherical tailing by steam pressure |
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