CN117945391A - Asphalt-based carbon material and preparation method and application thereof - Google Patents
Asphalt-based carbon material and preparation method and application thereof Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 55
- 239000010426 asphalt Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003763 carbonization Methods 0.000 claims abstract description 33
- 229920000642 polymer Polymers 0.000 claims abstract description 26
- 239000012298 atmosphere Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 239000007800 oxidant agent Substances 0.000 claims abstract description 17
- 230000001590 oxidative effect Effects 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 12
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000003245 coal Substances 0.000 claims description 7
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910021385 hard carbon Inorganic materials 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000004132 cross linking Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000002243 precursor Substances 0.000 description 5
- 239000010405 anode material Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000002194 amorphous carbon material Substances 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010505 homolytic fission reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of sodium ion battery materials, and discloses an asphalt-based carbon material, a preparation method and application thereof, wherein the preparation method comprises the following steps of crushing, ball milling and grading asphalt to obtain powder; mixing the powder with an oxidant, and performing oxidation treatment in the atmosphere to obtain an oxidized polymer; performing first carbonization treatment on the oxidized polymer in an inert atmosphere to obtain a low-temperature carbonized polymer; and performing second carbonization treatment on the low-temperature carbonized polymer in an inert atmosphere to obtain the pitch-based carbon material. The invention adopts the steps, takes the asphalt with low cost and high yield as the raw material, initiates the oxidative polymerization of the asphalt by introducing the organic oxidant, improves the crosslinking degree, and then carries out the first carbonization treatment and the second carbonization treatment to prepare the asphalt-based hard carbon material for the sodium ion battery with high performance.
Description
Technical Field
The invention relates to the technical field of sodium ion battery materials, in particular to an asphalt-based carbon material, a preparation method and application thereof.
Background
The sodium ion battery has wide application prospect in large-scale energy storage due to high sodium storage amount, low cost and good safety. The searching of the anode material with low price and excellent performance is a key for realizing the large-scale application of the sodium ion electrochemical energy storage system, and among various anode materials, the amorphous carbon material has higher specific capacity for storing sodium, has low cost and easily regulated structure, and is a research hot spot and mainstream selection of the anode material of the sodium ion battery at present.
Amorphous carbon materials are largely divided into soft carbon and hard carbon, wherein hard carbon has a loose porous structure, and compared with graphite with a layer spacing of 0.335. 0.335 nm, the layer spacing of hard carbon can reach 0.36-0.38 nm, sodium ions can be rapidly embedded and extracted in the gaps between the layers of hard carbon, and biomass, resin, polymer, heavy organic matters and the like are the main precursors for manufacturing hard carbon. But biomass-based precursors are greatly disturbed by climate and season, the cost of resin and polymer hard carbon materials is high, and the carbon yield is low.
Asphalt is an important heavy organic matter as a main byproduct in coal chemical industry or petrochemical industry, has the advantages of wide source, low price, high carbon yield and the like, and is a high-quality precursor for preparing the carbon anode material. However, in the high-temperature carbonization process, asphalt is easy to graphitize to form a highly ordered carbon layer structure, which is unfavorable for storage of sodium ions, so that the sodium storage capacity is low, namely about 90 mAh/g. At present, the preparation method of the asphalt-based hard carbon cathode mainly comprises a gas-phase pre-oxidation method, a template method and the like, but the method has the defects of low pre-oxidation effect, and complex post-treatment process, such as the template method which needs to use acid to remove template agent, time-consuming preparation process, environmental pollution and the like, thus preventing the practical process of the carbon cathode material.
Disclosure of Invention
The invention aims to provide an asphalt-based carbon material, a preparation method and application thereof, wherein the method is simple, no post-treatment is needed, the raw materials are easy to obtain, the cost is low, the carbon yield is high, and the asphalt-based carbon material is suitable for large-scale production.
In order to achieve the above object, the present invention provides a method for preparing a pitch-based carbon material, comprising the steps of,
S1, crushing, ball milling and grading asphalt to obtain powder;
s2, mixing the powder in the step S1 with an oxidant, and performing oxidation treatment in the atmosphere to obtain an oxidized polymer;
S3, performing first carbonization treatment on the oxidized polymer in the S2 in an inert atmosphere to obtain a low-temperature carbonized polymer;
s4, performing second carbonization treatment on the low-temperature carbonized polymer in the S3 in an inert atmosphere to obtain the pitch-based carbon material.
Preferably, in S1, the asphalt comprises one or more of low temperature coal asphalt, medium temperature coal asphalt, high temperature coal asphalt, petroleum asphalt and naphthalene asphalt.
Preferably, in S1, the rotational speed is 3000-9000 r/min during grinding, the ball milling rotational speed is 300-1000 rpm, and the ball milling time is 5-20 h.
In the invention, the rotating speeds of the crushing and ball milling are controlled within the range, and the particle size of asphalt is controlled in turn, so that the powder is convenient for subsequent operation.
Preferably, in S2, the oxidant is an organic oxidant, and the addition amount of the oxidant is 5-20% of the mass of the powder.
Preferably, in S2, the organic oxidizing agent includes one or more of hydrogen peroxide, dicumyl peroxide, benzoyl peroxide, di-t-butyl peroxide, dicumyl peroxide, diethylenetriamine.
Preferably, in S2, the temperature of the oxidation treatment is 30-200 ℃ and the time is 0.5-5 h, and the atmosphere is one or more of air or oxygen. More preferably, the temperature of the oxidation treatment is 120-200 ℃.
In the invention, oxidation treatment is carried out at the temperature, covalent electrons of the organic oxidant are subjected to homolytic cleavage to generate free radicals, hydrogen on a molecular chain of asphalt is removed to form asphalt free radicals, and then the asphalt free radicals are polymerized to form a precursor for three-dimensional crosslinking. The process can promote solid-phase carbonization of asphalt in the subsequent high-temperature carbonization process, prevent ordered growth of a microcrystalline structure and inhibit graphitization process of the asphalt.
Preferably, in S3, the temperature of the first carbonization treatment is 300-800 ℃, the heat preservation time is 0.5-5 h, and the inert atmosphere is one or more of nitrogen, helium and argon.
More preferably, the temperature of the first carbonization treatment is 300 to 600 ℃.
In the invention, the first carbonization treatment is a low-temperature carbonization treatment, a precursor is decomposed in the low-temperature carbonization treatment, some carbon atoms are recombined, and aliphatic hydrocarbon is converted into aromatic hydrocarbon to form a carbon network with higher stability. Meanwhile, gas small molecules such as CO or CO 2 and the like can be released in the low-temperature carbonization process to form an open pore structure.
Preferably, in S4, the temperature of the second carbonization treatment is 1000-2000 ℃, the heat preservation time is 0.5-5 h, the heating rate is 0.5-10 ℃/min, and the inert atmosphere is one or more of nitrogen, helium and argon.
More preferably, the temperature of the second carbonization treatment is 1200 to 1500 ℃.
In the invention, the second carbonization treatment is high-temperature carbonization treatment, and in the high-temperature carbonization treatment process, macromolecular aromatic hydrocarbon is polymerized to form a graphite layer. The treated asphalt has high crosslinking degree, so that graphite microcrystals are formed locally, and disordered micropore structures are formed by disordered stacking of the graphite microcrystals, thereby being beneficial to sodium ion storage.
In the invention, by setting the temperature rising rate, the open pore structure formed by low-temperature carbonization forms a closed pore structure along with the rising of the temperature, which is helpful for improving the specific capacity and the first coulombic efficiency of the pitch-based carbon material.
The pitch-based carbon material prepared by the preparation method of the pitch-based carbon material has the particle size of 2-40 mu m and the specific surface area of 1-20 m 2/g.
In the invention, the pitch-based carbon material has excellent specific capacity and first coulombic efficiency by controlling the particle size and specific surface area of the pitch-based carbon material.
The pitch-based carbon material is applied to preparing a negative electrode of a sodium ion secondary battery.
The mechanism of the invention is as follows:
the invention takes asphalt with low cost and high yield as raw material, initiates the oxidative polymerization of the asphalt by introducing an organic oxidant, improves the crosslinking degree, and then carries out low-temperature carbonization treatment and high-temperature carbonization treatment to prepare the asphalt-based carbon material for the sodium ion battery with high performance.
Therefore, the preparation method adopting the steps has the beneficial effects that:
1. the preparation method provided by the invention is simple, no post-treatment is needed, the raw materials are easy to obtain, the cost is low, the carbon yield is high, and the preparation method is suitable for large-scale production;
2. The asphalt-based carbon material prepared by the method has uniform particle size, specific surface area of 1-20 m 2/g, specific capacity of 208-300 mAh/g and initial coulomb efficiency of 85-89%, and is proved to have excellent electrochemical performance.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a graph of the first three charge and discharge cycles of the pitch-based carbon material of example 2 of the present invention;
FIG. 2 is an SEM image of a pitch-based carbon material of example 2 of the invention;
Fig. 3 is an XRD pattern of the pitch-based carbon material in example 2 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.
In the present invention, the raw materials used are all conventional commercial products in the art unless otherwise specified.
Example 1
S1, crushing, ball milling and grading high-temperature coal tar pitch, wherein the rotating speed is 9000 r/min, the ball milling rotating speed is 800 rpm, and the ball milling time is 15 h, so as to obtain powder.
S2, mixing the powder in the S1 with diethyl triamine serving as an oxidant, wherein the addition amount of the diethyl triamine is 20% of the mass of the powder, and performing oxidation treatment in an air atmosphere at the temperature of 150 ℃ for 3 h to obtain an oxidized polymer.
S3, performing first carbonization treatment on the oxidized polymer in the S2 in the nitrogen atmosphere of the rotary furnace, wherein the temperature is 400 ℃, and the heat preservation time is 2 h, so as to obtain the low-temperature carbonized polymer.
S4, performing second carbonization treatment on the low-temperature carbonized polymer in the S3 under nitrogen inert atmosphere, wherein the temperature is 1400 ℃, the heating rate is 5 ℃/min, the heat preservation time is 2h, and the asphalt-based carbon material with the particle size of 10 μm is obtained.
Example 2
S1, crushing, ball milling and grading petroleum asphalt, wherein the rotating speed is 5000 r/min during crushing; the ball milling rotating speed is 500 rpm, the ball milling time is 10h, and the powder is obtained.
S2, mixing the powder in the step S1 with benzoyl peroxide serving as an oxidant, wherein the addition amount of the benzoyl peroxide is 10% of the mass of the powder, and performing oxidation treatment in an air atmosphere at the temperature of 120 ℃ for 3 h to obtain an oxidized polymer.
S3, performing first carbonization treatment on the oxidized polymer in the S2 in the nitrogen atmosphere of the rotary furnace, wherein the temperature is 500 ℃, and the heat preservation time is 2 h, so as to obtain the low-temperature carbonized polymer.
S4, performing second carbonization treatment on the low-temperature carbonized polymer in the S3 under the nitrogen atmosphere, wherein the temperature is 1300 ℃, the heating rate is 10 ℃/min, the heat preservation time is 2h, and the asphalt-based carbon material with the particle size of 4 μm is obtained.
Example 3
S1, crushing, ball milling and grading medium-temperature coal tar pitch, wherein the rotating speed is 7000 r/min during crushing; the ball milling rotating speed is 600 rpm, the ball milling time is 10h, and the powder is obtained.
S2, mixing the powder in the S1 with dicumyl peroxide serving as an oxidant, wherein the addition amount of the dicumyl peroxide is 5% of the mass of the powder, and performing oxidation treatment in an air atmosphere at the temperature of 180 ℃ for 2h hours to obtain an oxidized polymer.
S3, performing first carbonization treatment on the oxidized polymer in the S2 under the argon atmosphere of the rotary furnace, wherein the temperature is 600 ℃, and the heat preservation time is 2 h, so as to obtain the low-temperature carbonized polymer.
S4, performing second carbonization treatment on the low-temperature carbonized polymer in the S3 under the argon atmosphere, wherein the temperature is 1300 ℃, the heating rate is 5 ℃/min, the heat preservation time is 2h, and the asphalt-based carbon material with the particle size of 10 μm is obtained.
Test example 1
A. Specific surface area test
The pitch-based carbon materials obtained in examples 1 to 3 were subjected to a specific surface area test, to obtain a specific surface area of 7m 2/g for the pitch-based carbon material in example 1, a specific surface area of 10m 2/g for the pitch-based carbon material in example 2, and a specific surface area of 12 m 2/g for the pitch-based carbon material in example 3.
B. asphalt-based carbon material performance test
The specific capacity of the pitch-based carbon material in example 1 was 300 mAh/g, the specific capacity of the pitch-based carbon material in example 2 was 280 mAh/g, and the specific capacity of the pitch-based carbon material in example 3 was 290 mAh/g.
The first coulombic efficiency of the pitch-based carbon material in example 1 was 85%, the first coulombic efficiency of the pitch-based carbon material in example 2 was 87%, and the first coulombic efficiency of the pitch-based carbon material in example 3 was 89%.
The charge and discharge test was performed on the pitch-based carbon material in example 2, and the first three circles of charge and discharge curves are shown in fig. 1, and it is understood that in example 2, the charge and discharge curve of the pitch-based carbon material prepared shows typical hard carbon characteristics, the first charge specific capacity of the pitch-based carbon material is 280 mAh/g, and the first charge and discharge efficiency is 87%.
C. SEM test
The results of the scanning electron microscope test on the pitch-based carbon material in example 2 are shown in fig. 2, and it is understood that in example 2, the pitch-based carbon material is prepared with irregular particles, and the particle size is 15-20 μm.
D. XRD testing
XRD measurements on the pitch-based carbon material of example 2 gave the results shown in fig. 3, and it was found that XRD of the pitch-based carbon material prepared in example 2 exhibited typical amorphous characteristics, indicating a disordered structure.
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 (10)
1. A preparation method of a pitch-based carbon material is characterized by comprising the following steps: comprises the steps of,
S1, crushing, ball milling and grading asphalt to obtain powder;
s2, mixing the powder in the step S1 with an oxidant, and performing oxidation treatment in the atmosphere to obtain an oxidized polymer;
S3, performing first carbonization treatment on the oxidized polymer in the S2 in an inert atmosphere to obtain a low-temperature carbonized polymer;
s4, performing second carbonization treatment on the low-temperature carbonized polymer in the S3 in an inert atmosphere to obtain the pitch-based carbon material.
2. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S1, the asphalt comprises one or more of low-temperature coal asphalt, medium-temperature coal asphalt, high-temperature coal asphalt, petroleum asphalt and naphthalene asphalt.
3. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S1, the rotational speed is 3000-9000 r/min during crushing, the ball milling rotational speed is 300-1000 rpm, and the ball milling time is 5-20 h.
4. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S2, the oxidant is an organic oxidant, and the addition amount of the oxidant is 5-20% of the mass of the powder.
5. The method for producing a pitch-based carbon material according to claim 4, wherein: in S2, the organic oxidizer includes one or more of hydrogen peroxide, dicumyl peroxide, benzoyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, and diethylenetriamine.
6. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S2, the temperature of the oxidation treatment is 30-200 ℃ and the time is 0.5-5 h, and the atmosphere is one or more of air or oxygen.
7. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S3, the temperature of the first carbonization treatment is 300-800 ℃, the heat preservation time is 0.5-5 h, and the inert atmosphere is one or more of nitrogen, helium and argon.
8. The method for preparing a pitch-based carbon material according to claim 1, wherein: in S4, the temperature of the second carbonization treatment is 1000-2000 ℃, the heat preservation time is 0.5-5 h, the heating rate is 0.5-10 ℃/min, and the inert atmosphere is one or more of nitrogen, helium and argon.
9. The pitch-based carbon material produced by the production method of a pitch-based carbon material according to any one of claims 1 to 8, having a particle diameter of 2 to 40 μm and a specific surface area of 1 to 20m 2/g.
10. The application of the pitch-based carbon material according to claim 9 in preparing a negative electrode of a sodium ion secondary battery.
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