CN117843999A - Method for preparing high-performance vulcanized polyacrylonitrile positive electrode material by solution uniform carbon doping method - Google Patents
Method for preparing high-performance vulcanized polyacrylonitrile positive electrode material by solution uniform carbon doping method Download PDFInfo
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- CN117843999A CN117843999A CN202311766493.5A CN202311766493A CN117843999A CN 117843999 A CN117843999 A CN 117843999A CN 202311766493 A CN202311766493 A CN 202311766493A CN 117843999 A CN117843999 A CN 117843999A
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- polyacrylonitrile
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- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 20
- 239000007774 positive electrode material Substances 0.000 title claims description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 21
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000010405 anode material Substances 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 239000011593 sulfur Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 71
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 21
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 239000003575 carbonaceous material Substances 0.000 claims description 10
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 9
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 239000003273 ketjen black Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000002048 multi walled nanotube Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 230000001351 cycling effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229920001021 polysulfide Polymers 0.000 description 3
- 239000005077 polysulfide Substances 0.000 description 3
- 150000008117 polysulfides Polymers 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910003003 Li-S Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007704 transition Effects 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
Abstract
The invention discloses a method for preparing high-performance vulcanized polyacrylonitrile by a solution uniform carbon-doped method. Adding sodium polysulfide solution into carbon-doped polyacrylonitrile organic solution, uniformly separating out elemental sulfur and polyacrylonitrile through acid solution to obtain a uniformly mixed mixture of carbon, sulfur and polyacrylonitrile, and carrying out heat treatment on the mixture to obtain the carbon-doped vulcanized polyacrylonitrile anode material. The method can greatly improve the electron transmission capacity and reaction kinetics of the vulcanized polyacrylonitrile anode. The stable circulation capacity can reach more than 700mAh/g when the battery is charged and discharged under the current density of 0.2C (1 C=1000 mAh/g). The battery is charged and discharged at the current density of 3C, and the stable circulation capacity still has 635mAh/g. The method has important promotion effect on the practical application of the lithium-sulfur battery.
Description
Technical Field
The invention designs a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method, and relates to the field of chemical power supplies.
Technical Field
The lithium-sulfur battery has higher theoretical specific capacity (1675 mAh g) -1 ) And energy density (2600 Wh kg) -1 ) As a next generation rechargeable battery, the battery has good application prospect in large-scale power grid application and long-distance transportation. Compared with elemental sulfur cathodes, sulfided Polyacrylonitrile (SPAN) can eliminate shuttling of lithium polysulfides, making it a viable sulfur-based cathode material substitute for Li-S batteries. It can be synthesized simply by heating Polyacrylonitrile (PAN) and sulfur powder under an inert atmosphere, and has good compatibility with carbonate-based electrolytes commonly used in lithium ion batteries. In addition, it can be conveniently adapted to the current manufacturing process of lithium ion batteries.
For the last decades, many studies have been made on the chemical structure, electrochemical properties and various redox reactions of SPAN. Chemical engineers are interested in vulcanizing polyacrylonitrile (SPAN) because of its excellent reversibility, cycling stability and high active substance utilization (about 100% coulombic efficiency). In PAN polymer structures, the-CN groups undergo cyclization to form stable conjugated polypyridine ring structures with c=n and c=c bonds. To create a stable molecular structure, sulfur is covalently bound to the polymeric backbone of the pyrolyzed PAN. Lithium-vulcanized polyacrylonitrile (Li-SPAN) cells are intended to minimize anode corrosion and provide excellent cycling stability by eliminating polysulfide shuttling. This phenomenon is due to the solid-solid transition during the reduction process, in which there is no dissolved polysulfide.
Although the vulcanized polyacrylonitrile has the advantage of stable circulation, the material has uneven sintering process, poor conductivity and poor reaction kinetics in a battery, which results in uneven performance and poor multiplying power performance of the vulcanized polyacrylonitrile anode material to a certain extent.
Therefore, a brand new preparation method of the vulcanized polyacrylonitrile needs to be developed, and the problem of non-uniform performance caused by non-uniform sintering process in the existing preparation method is solved.
Disclosure of Invention
The invention aims to solve the problems of uneven sintering process, poor conductivity and poor reaction kinetics in a battery of a vulcanized polyacrylonitrile positive electrode material, and provides a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method, so that carbon, sulfur and polyacrylonitrile in a vulcanized polyacrylonitrile precursor are uniformly mixed. The conductivity and the reaction kinetics of the vulcanized polyacrylonitrile anode material can be effectively improved by the added carbon material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method, which comprises the following steps:
s1: completely dissolving polyacrylonitrile in an organic solvent to obtain 10-40g/L polyacrylonitrile organic solution;
the molecular weight of the polyacrylonitrile is 50000 ~ 3000000;
s2: adding a carbon material into the polyacrylonitrile organic solution obtained in the step S1, and stirring to uniformly disperse the carbon material to obtain a carbon-containing polyacrylonitrile organic solution;
the mass ratio of the carbon material to the polyacrylonitrile is 1:20-1:30;
s3: preparing 100-200g/L sodium sulfide aqueous solution;
s4: dissolving elemental sulfur in the sodium sulfide aqueous solution obtained in the step S3, and stirring until the elemental sulfur is completely dissolved to obtain a sodium polysulfide solution; the content of elemental sulfur in the sodium polysulfide solution is 41-82g/L;
s5: adding the acid solution with the pH value of 1-6 and the sodium polysulfide solution obtained in the step S4 into the carbon-containing polyacrylonitrile solution obtained in the step S2, stirring, filtering and drying to obtain a uniform mixture of carbon, sulfur and polyacrylonitrile; the volume ratio of the added acid solution, sodium polysulfide solution and carbon-containing polyacrylonitrile solution is 1 (5-15) (3-10);
the acid solution is any one of hydrochloric acid, sulfuric acid, nitric acid and glacial acetic acid;
s6: and (3) carrying out heat treatment on the uniform mixture precursor obtained in the step (S5), and obtaining the vulcanized polyacrylonitrile anode material after natural cooling.
Preferably, the organic solvent in the step S1 is N-methylpyrrolidone or N, N-dimethylformamide.
Preferably, the carbon material in the step S2 includes any one or a mixture of two or more of ketjen black, single-walled carbon nanotubes, multi-walled carbon nanotubes, single-layered graphene, graphene oxide, and multi-layered graphene.
Preferably, the solution is kept stirred in the steps S1 to S5, and the stirring speed is 500-1000 revolutions/min.
Preferably, the dropping speed of the acid in the step S5 is 1-5mL/min; the dropping speed of the sodium polysulfide is 3-10mL/min.
Preferably, the drying temperature in the step S5 is 60-80 ℃ and the drying time is 8-24 h.
Preferably, the heating temperature in the step S6 is 200-400 ℃, and the heat preservation time is 3-12 h.
Preferably, the concentration of the polyacrylonitrile is 20g/L, and the mass ratio of the polyacrylonitrile to the carbon is 25:1, the concentration of sodium sulfide solution is 100g/L, the content of elemental sulfur is 42g/L, and acid solution is glacial acetic acid; the drying temperature in the step S5 is 60 ℃, the drying time is 24 hours, the dropping speed of the acid in the step S5 is 3mL/min, and the dropping speed of the sodium polysulfide is 5mL/min; the heating temperature in the step S6 is 350 ℃, and the heat preservation time is 5 hours; and (3) stirring the solution in the steps S1 to S5, wherein the stirring speed is 800 revolutions/min.
In a second aspect, the invention provides a high-performance vulcanized polyacrylonitrile anode material, which is prepared by the preparation method in the first aspect.
In a third aspect, the present invention provides a use of the vulcanized polyacrylonitrile positive electrode material according to the second aspect, applied to a positive electrode of a secondary battery.
The invention has the beneficial effects that: the polyacrylonitrile and the elemental sulfur are prepared into a solution, and then the solution is mixed to achieve uniform mixing at a microscopic level, so that the obtained vulcanized polyacrylonitrile anode material has uniform structure. The conductivity and the reaction kinetics of the vulcanized polyacrylonitrile anode material can be effectively improved by adding the carbon material in the process of preparing the polyacrylonitrile solution. The stable circulation capacity can reach more than 700mAh/g when the battery is charged and discharged under the current density of 0.2C (1 C=1000 mAh/g). The lithium sulfur battery is charged and discharged at the current density of 3C, the stable circulation capacity still has 635mAh/g, and the lithium sulfur battery has important promotion effect on the practicability of the lithium sulfur battery.
Drawings
FIG. 1 is a TEM photograph of a vulcanized polyacrylonitrile cathode material of example 1;
FIG. 2 is a graph showing the cycle performance of the lithium sulfur batteries prepared in examples 1 to 3 at a rate of 0.2C;
fig. 3 shows the lithium sulfur batteries prepared in examples 1 to 3 at 0.2C, 0.4C, 0.6C, 0.8C, 1.0C, 2.0C, 3.0C.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings and preferred examples for the purpose of facilitating understanding of the present invention, but the scope of the present invention is not limited to the following specific examples.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
The embodiment of the invention provides a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method, which comprises the following steps:
1g of polyacrylonitrile was dissolved in 50mL of anhydrous N, N dimethylformamide to form an organic solution of polyacrylonitrile. Adding 0.04g of ketjen black material into the polyacrylonitrile solution, and stirring to uniformly disperse the ketjen black material to obtain a uniform ketjen black-containing polyacrylonitrile solution.
12g of sodium sulfide is dissolved in 120mL of deionized water, stirred at room temperature until the sodium sulfide is completely dissolved, 120mL of sodium sulfide solution is obtained, 5g of elemental sulfur is dissolved in the sodium sulfide aqueous solution obtained above, and stirred until the sodium sulfide is completely dissolved, so as to obtain sodium polysulfide solution.
Adding 20mL of glacial acetic acid and the obtained sodium polysulfide solution into the obtained polyacrylonitrile solution containing ketjen black at the speed of 3mL/min and 5mL/min respectively, stirring, filtering and drying to obtain a precursor of a vulcanized polyacrylonitrile anode material;
and (3) placing the precursor of the vulcanized polyacrylonitrile anode material in a tube furnace, preserving heat for 5 hours at 350 ℃, and naturally cooling to obtain the vulcanized polyacrylonitrile anode material.
The stable circulation capacity of the material reaches 700mAh/g under the current density of 0.2C, and the average coulombic efficiency is more than 99 percent, as shown in figure 2. At a current density of 0.2C, the stable cycling capacity of the material reaches 634mAh/g, as shown in FIG. 3.
Example 2
The embodiment of the invention provides a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method.
1g of polyacrylonitrile was dissolved in 50mL of anhydrous N, N dimethylformamide to form an organic solution of polyacrylonitrile. Adding 0.04g of multi-wall carbon nano tube material into the polyacrylonitrile solution, and stirring to uniformly disperse the material, thereby obtaining the polyacrylonitrile solution containing the multi-wall carbon nano tube.
12g of sodium sulfide is dissolved in 120mL of deionized water, stirred at room temperature until the sodium sulfide is completely dissolved, 120mL of sodium sulfide solution is obtained, 5g of elemental sulfur is dissolved in the sodium sulfide aqueous solution obtained above, and stirred until the sodium sulfide is completely dissolved, so as to obtain sodium polysulfide solution.
Adding 20mL of glacial acetic acid and the obtained sodium polysulfide solution into the obtained polyacrylonitrile solution uniformly containing the multi-wall carbon nano tubes at the speed of 3mL/min and 5mL/min respectively, stirring, filtering and drying to obtain a precursor of the vulcanized polyacrylonitrile anode material;
and (3) placing the precursor of the vulcanized polyacrylonitrile anode material in a tube furnace, preserving heat for 5 hours at 350 ℃, and naturally cooling to obtain the vulcanized polyacrylonitrile anode material.
At a current density of 0.2C, the stable cycling capacity of the material reaches 658mAh/g, and the average coulomb efficiency is more than 99%, as shown in figure 2. At 3C current density, the stable circulation capacity of the material reaches 584mAh/g, as shown in figure 3.
Example 3
The embodiment of the invention provides a method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by a solution uniform carbon doping method.
1g of polyacrylonitrile was dissolved in 50mL of anhydrous N-methylpyrrolidone to form an organic solution of polyacrylonitrile. And adding 0.04g of the multilayer graphene material into the polyacrylonitrile solution, and stirring to uniformly disperse the multilayer graphene material to obtain the uniform polyacrylonitrile solution containing the multilayer graphene.
12g of sodium sulfide is dissolved in 120mL of deionized water, stirred at room temperature until the sodium sulfide is completely dissolved, 120mL of sodium sulfide solution is obtained, 5g of elemental sulfur is dissolved in the sodium sulfide aqueous solution obtained above, and stirred until the sodium sulfide is completely dissolved, so as to obtain sodium polysulfide solution.
Adding 20mL of glacial acetic acid and the obtained sodium polysulfide solution into the obtained polyacrylonitrile solution uniformly containing multiple layers of graphene at the speed of 3mL/min and 5mL/min respectively, stirring, filtering and drying to obtain a precursor of a vulcanized polyacrylonitrile anode material;
and (3) placing the precursor of the vulcanized polyacrylonitrile anode material in a tube furnace, preserving heat for 5 hours at 350 ℃, and naturally cooling to obtain the vulcanized polyacrylonitrile anode material.
At the current density of 0.2C, the stable circulation capacity of the material reaches 560mAh/g, and the average coulomb efficiency is more than 99%. See fig. 2. At a current density of 3C, the stable cycling capacity of the material reaches 448mAh/g, as shown in FIG. 3.
Claims (10)
1. The method for preparing the high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method is characterized by comprising the following steps of:
s1: completely dissolving polyacrylonitrile in an organic solvent to obtain 10-40g/L polyacrylonitrile organic solution;
the molecular weight of the polyacrylonitrile is 50000 ~ 3000000;
s2: adding a carbon material into the polyacrylonitrile organic solution obtained in the step S1, and stirring to uniformly disperse the carbon material to obtain a carbon-containing polyacrylonitrile organic solution;
the mass ratio of the carbon material to the polyacrylonitrile is 1:20-1:30;
s3: preparing 100-200g/L sodium sulfide aqueous solution;
s4: dissolving elemental sulfur in the sodium sulfide aqueous solution obtained in the step S3, and stirring until the elemental sulfur is completely dissolved to obtain a sodium polysulfide solution; the content of elemental sulfur in the sodium polysulfide solution is 41-82g/L;
s5: adding the acid solution with the pH value of 1-6 and the sodium polysulfide solution obtained in the step S4 into the carbon-containing polyacrylonitrile solution obtained in the step S2, stirring, filtering and drying to obtain a uniform mixture of carbon, sulfur and polyacrylonitrile; the volume ratio of the added acid solution, sodium polysulfide solution and carbon-containing polyacrylonitrile solution is 1 (5-15) (3-10);
the acid solution is any one of hydrochloric acid, sulfuric acid, nitric acid and glacial acetic acid;
s6: and (3) carrying out heat treatment on the uniform mixture precursor obtained in the step (S5), and obtaining the vulcanized polyacrylonitrile anode material after natural cooling.
2. The method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method according to claim 1, wherein the organic solvent in the step S1 is N-methylpyrrolidone or N, N-dimethylformamide.
3. The method for preparing a high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method according to claim 1, wherein the carbon material in the step S2 comprises any one or more than two of ketjen black, single-walled carbon nanotubes, multi-walled carbon nanotubes, single-layered graphene, graphene oxide and multi-layered graphene.
4. The method for preparing the high-performance vulcanized polyacrylonitrile positive electrode material by the solution uniform carbon-doped method according to claim 1, wherein the stirring speed of the solution is 500-1000 rpm in the steps S1-S5.
5. The method for preparing the high-performance vulcanized polyacrylonitrile positive electrode material by the solution uniform carbon-doped method according to claim 1, wherein the dropping speed of the acid in the step S5 is 1-5mL/min; the dropping speed of the sodium polysulfide is 3-10mL/min.
6. The method for preparing high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method according to claim 1, wherein the drying temperature in the step S5 is 60-80 ℃ and the drying time is 8-24 h.
7. The method for preparing high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method according to claim 1, wherein the heating temperature in the step S6 is 200-400 ℃, and the heat preservation time is 3-12 h.
8. The method for preparing the high-performance vulcanized polyacrylonitrile positive electrode material by using the solution uniform carbon-doped method according to claim 1, wherein the concentration of the polyacrylonitrile is 20g/L, and the mass ratio of the polyacrylonitrile to the carbon is 25:1, the concentration of sodium sulfide solution is 100g/L, the content of elemental sulfur is 42g/L, and acid solution is glacial acetic acid; the drying temperature in the step S5 is 60 ℃, the drying time is 24 hours, the dropping speed of the acid in the step S5 is 3mL/min, and the dropping speed of the sodium polysulfide is 5mL/min; the heating temperature in the step S6 is 350 ℃, and the heat preservation time is 5 hours; and (3) stirring the solution in the steps S1 to S5, wherein the stirring speed is 800 revolutions/min.
9. A high performance vulcanized polyacrylonitrile positive electrode material, which is characterized in that the material is prepared by the preparation method of any one of claims 1 to 8.
10. Use of the vulcanized polyacrylonitrile positive electrode material according to claim 9, characterized in that it is applied to a positive electrode of a secondary battery.
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