CN111924844A - Doping method and application of bio-based carbon material based on ricepaper pith - Google Patents
Doping method and application of bio-based carbon material based on ricepaper pith Download PDFInfo
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- CN111924844A CN111924844A CN202010848183.8A CN202010848183A CN111924844A CN 111924844 A CN111924844 A CN 111924844A CN 202010848183 A CN202010848183 A CN 202010848183A CN 111924844 A CN111924844 A CN 111924844A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 38
- 244000290970 Tetrapanax papyrifer Species 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 9
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- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- -1 nitrogen-containing compound Chemical class 0.000 claims description 7
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- CSJLBAMHHLJAAS-UHFFFAOYSA-N diethylaminosulfur trifluoride Chemical compound CCN(CC)S(F)(F)F CSJLBAMHHLJAAS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
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- 238000002791 soaking Methods 0.000 claims description 6
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- 239000002482 conductive additive Substances 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- TVVNZBSLUREFJN-UHFFFAOYSA-N 2-(4-chlorophenyl)sulfanyl-5-nitrobenzaldehyde Chemical compound O=CC1=CC([N+](=O)[O-])=CC=C1SC1=CC=C(Cl)C=C1 TVVNZBSLUREFJN-UHFFFAOYSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- MZJUGRUTVANEDW-UHFFFAOYSA-N bromine fluoride Chemical compound BrF MZJUGRUTVANEDW-UHFFFAOYSA-N 0.000 claims description 2
- CODNYICXDISAEA-UHFFFAOYSA-N bromine monochloride Chemical compound BrCl CODNYICXDISAEA-UHFFFAOYSA-N 0.000 claims description 2
- 239000007810 chemical reaction solvent Substances 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- CBEQRNSPHCCXSH-UHFFFAOYSA-N iodine monobromide Chemical compound IBr CBEQRNSPHCCXSH-UHFFFAOYSA-N 0.000 claims description 2
- 229920000767 polyaniline Polymers 0.000 claims description 2
- 229920000128 polypyrrole Polymers 0.000 claims description 2
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 claims description 2
- FQFKTKUFHWNTBN-UHFFFAOYSA-N trifluoro-$l^{3}-bromane Chemical compound FBr(F)F FQFKTKUFHWNTBN-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 3
- 238000004146 energy storage Methods 0.000 claims 2
- 150000004985 diamines Chemical class 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 7
- 230000003213 activating effect Effects 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
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- 239000011347 resin Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 235000011201 Ginkgo Nutrition 0.000 description 2
- 241000218628 Ginkgo Species 0.000 description 2
- 235000008100 Ginkgo biloba Nutrition 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
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- QLSWIGRIBOSFMV-UHFFFAOYSA-N 1h-pyrrol-2-amine Chemical compound NC1=CC=CN1 QLSWIGRIBOSFMV-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
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- 239000002019 doping agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention belongs to the technical field of bio-based carbon materials, and particularly relates to a doping method of a bio-based carbon material based on ricepaper pith, which comprises the following steps: mixing the ricepaperplant pith bio-based carbon material, the doping compound and the solvent, and carrying out microwave reaction for 3-8h at 60-240 ℃ in an inert gas atmosphere to obtain the ricepaperplant pith bio-based microwave doping carbon material. The doping method based on the ricepaper pith bio-based carbon material provided by the invention is low in reaction temperature, high in doping rate, simple in process, high in yield and suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of bio-based carbon materials, and particularly relates to a doping method of a bio-based carbon material based on ricepaper pith and application thereof.
Background
The biomass carbon material has good mechanical properties, but part of the carbon material has no energy band gap, the conductivity of the carbon material cannot be completely controlled like that of a traditional semiconductor, and the surface of the carbon material is inert and is not beneficial to compounding with other materials, so that the main carriers are changed into an electron type or a cavity type by doping in the prior art, the band gap of the biomass carbon material is opened, the conductivity, the stability, the surface chemical activity and the energy density of the carbon material are improved, and the application of the biomass carbon material is diversified.
Patent CN107680832A discloses a method for preparing nitrogen-doped carbon material, comprising the following steps: synthesizing a nitrogen-doped lignin resin precursor under an alkaline condition by using lignin as a carbon source, melamine as a nitrogen source and aldehyde as an additive; heating and pressurizing the nitrogen-doped lignin resin precursor to obtain a pretreated resin precursor, carrying out pyrolysis treatment on the pretreated resin precursor under the action of a catalyst to obtain powdery particles, and carrying out acid pickling and drying to obtain the catalyst.
Patent CN108529621A discloses a preparation method of nitrogen-doped porous carbon material, comprising the following steps: the preparation method comprises the steps of placing the ginkgo leaves in a tubular furnace for low-temperature carbonization to obtain a carbon precursor, mixing the carbon precursor with a nitrogen-containing compound and an alkaline inorganic substance, soaking in deionized water, drying, and calcining and activating under the protection of nitrogen to obtain the ginkgo leaf carbon.
In the prior art, the doped porous carbon material is prepared by adopting a heat treatment means, but the process is complex, the reaction temperature is high, the heating program is not accurately controlled, and the doping rate is not high.
Disclosure of Invention
The invention aims to provide a doping method of a bio-based carbon material based on ricepaper pith and application thereof, so as to solve one or more of the problems.
According to one aspect of the present invention, there is provided a method for doping bio-based carbon material based on ricepaper pith, comprising the steps of:
mixing the dried ricepaperplant pith bio-based carbon material, the doping compound and the solvent, and carrying out microwave reaction for 3-8h at the temperature of 60-240 ℃ in an inert gas atmosphere to obtain the ricepaperplant pith bio-based microwave doped carbon material.
In some embodiments, the mass ratio of the ricepaperplant pith bio-based carbon material, the doping compound and the solvent is 1 (1-5) to (1-5).
In some embodiments, the steps further comprise: and (3) carrying out vacuum filtration, cleaning a reaction solvent in the ricepaperplant pith bio-based microwave doped carbon material by using deionized water to obtain ricepaperplant pith bio-based microwave doped carbon material slurry, and freeze-drying the ricepaperplant pith bio-based microwave doped carbon material slurry to obtain ricepaperplant pith bio-based microwave doped carbon material powder.
In some embodiments, the microwave reaction may be carried out at high pressures of 300-500 kpa. Thereby, the doping rate can be improved.
In some embodiments, the dried ricepaperplant bio-based carbon material, the doping compound, the solvent are placed in a microwave reactor and stirred for 0.5-2 hours.
In some embodiments, the microwave reaction is carried out in a microwave reactor, the microwave reactor being one of a microwave closed reactor, a microwave atmospheric reactor, a microwave continuous reactor.
In some embodiments, the dopant compound is one of a doped nitrogen-containing compound, a doped fluorine-containing compound, a doped boron-containing compound, a doped bromine-containing compound, wherein,
the nitrogen-containing compound can be one of amino, pyrrole and pyridine structure nitrogen sources such as urea, melamine, polypyrrole, polyaniline, hydrazine, hexamethylenetetramine, dihydroamine and the like;
the fluorine-containing compound can be 10-70% of hydrofluoric acid and BF3Diethyl etherate, diethylaminosulfur trifluoride (DAST), hexafluorophosphoric acid (HPF)6) One of fluorine sources containing fluorine bonds;
the boron-containing compound may be boric acid;
the bromine-containing compound may be one of bromine chloride, bromine fluoride, bromine trifluoride, bromine pentafluoride, and bromine iodide.
In some embodiments, the solvent is absolute ethanol or acetonitrile.
In some embodiments, the inert gas may be one or more of argon, nitrogen, hydrogen.
In some embodiments, the reaction sequence for the microwave reaction is: maintaining at 40-60 deg.C for 20-40min, heating to 100-140 deg.C, maintaining for 20-40min, heating to 150-240 deg.C, and maintaining for 180-420 min. This reduces side reactions and improves the doping rate.
In some embodiments, the ricepaper pith bio-based carbon material can be prepared by the following method:
firstly, drying the ricepaperplant pith in an oven, removing moisture, putting the dried ricepaperplant pith into a tubular furnace, introducing inert gas, and carbonizing for 4-12h at 400-1200 ℃ to obtain a ricepaperplant pith carbon material;
then, grinding the ricepaperplant pith carbon material and an activating agent (the mass ratio is 1:0.5-6) together by using a mortar, and then putting the ricepaperplant pith carbon material and the activating agent into an oven at 50-110 ℃ for 1-12 h;
and finally, putting the mixture of the carbon material of the ricepaperplant pith and the activating agent into a tubular furnace, introducing inert gas, reacting for 0.5-3h at 300-800 ℃, then respectively cleaning the activating agent with HCl by adopting suction filtration, washing with deionized water until the cleaning solution is neutral, and freeze-drying to obtain the ricepaperplant pith bio-based carbon material.
In the preparation process of the ricepaper pith bio-based carbon material, the inert gas is one or more of argon, nitrogen and hydrogen; active agentIs calcium carbonate, KOH, H3PO4Or ZnCl2One or more of them.
Compared with the traditional doping methods, such as a vapor phase growth method, a ball milling method, a plasma method, a hydrothermal method and the like, the microwave doping method has the following advantages:
(1) the reaction temperature is low, the reaction time is greatly shortened, because the working principle of the microwave reaction generator is that reactant molecules are enabled to move violently through microwaves, and the microwave field acts on Lorentz force of ions and polar molecules to enable relative movement among the particles to have particularity, so that less reaction temperature and time can be used, energy consumption is greatly reduced, and production efficiency is improved.
(2) The method has the advantages that the doping rate is high, the previous doping mode is completed under atmospheric pressure, and the doped carbon material with the doping rate exceeding 15% is difficult to produce, so that the method can reduce the reaction potential barrier and greatly improve the reaction rate under the high-pressure environment, reduce the atom spacing and change the atom bonding and stacking mode and the electronic structure, thereby obtaining higher doping rate; the generation of side reactions is reduced by precise control of the reaction program.
(3) The method has the advantages that the process is simple, the yield can reach 80-95%, the vapor deposition method and the plasma method need harsh preparation conditions, the complexity of the process determines the cost and the efficiency of actual production, and the ricepaperplant pith bio-based microwave doped carbon material with high doping rate can be obtained by simple operation.
According to another aspect of the invention, the ricepaperplant-based bio-based microwave doped carbon material obtained by the preparation method has the specific surface area of 600-800m2The micropore size is 20nm-40 nm.
The bio-based microwave doped carbon material has good conductivity and wettability, which greatly contributes to the rate performance and long-cycle performance of the material, so that the super capacitor and the lithium ion battery can have excellent performance, and an opportunity is provided for high added value utilization of bio-based materials in daily life.
According to another aspect of the present invention, a method for preparing a lithium ion battery pole piece is provided, which comprises the following steps:
grinding and mixing the ricepaperplant-based microwave-doped carbon material obtained by the preparation method with an active substance, a conductive additive, a binder and a solvent, and then performing ultrasonic treatment to obtain uniformly dispersed pole piece slurry;
and cutting the copper-plated carbon cloth into pole pieces, soaking the pole pieces in the slurry, taking out and drying to obtain the lithium ion battery pole pieces.
In some embodiments, the post-soaking drying step of the pole piece is as follows: taking out the pole piece soaked in the slurry for 5-20min, and drying in a vacuum drying oven at 50-150 deg.C for 5-12 h.
In some embodiments, sulfur, silicon, phosphorus, graphite, and the like can be used as the active material of the lithium battery pole piece material.
In some embodiments, the binder is one or more of polyacrylic acid (PAA), polyvinylidene fluoride (PVDF), sodium carboxymethyl cellulose (CMC), and other common binders for lithium ion batteries.
In some embodiments, the conductive additive is one or more of multi-walled carbon nanotubes, single-walled carbon nanotubes, Super P, ketjen black, and the like.
In some embodiments, the solvent is one of water, ethanol, N-methylpyrrolidone.
Drawings
FIG. 1 is an optical photograph of medulla Tetrapanacis.
Fig. 2 and 3 are SEM images of ricepaper pith bio-based carbon material.
Fig. 4 is a graph of the cycle curve and coulombic efficiency of the lithium sulfur battery in example 1.
Fig. 5 is a rate performance graph of the lithium sulfur battery in example 1.
Fig. 6 is a cyclic voltammogram of the supercapacitor in example 2.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Unless otherwise specified, the following chemicals are commercially available.
FIG. 1 shows an optical photograph of a rice stem used in the present invention, from which it can be seen that the thickness of the rice stem is about 4.320 mm.
The ricepaperplant pith bio-based carbon material used in the embodiment of the invention can be prepared by the following method:
firstly, drying the ricepaperplant pith in an oven, removing moisture, putting the dried ricepaperplant pith in a tubular furnace, introducing nitrogen, and carbonizing at 800 ℃ for 10 hours to obtain a ricepaperplant pith bio-based carbon material;
then grinding the ricepaperplant pith bio-based carbon material and an activating agent (the mass ratio is 1:2) together by using a mortar, and then putting the ricepaperplant pith bio-based carbon material into an oven at 80 ℃ for 6 hours;
and finally, putting the mixture of the ricepaperplant pith bio-based carbon material and KOH in a tube furnace, introducing nitrogen, reacting for 2h at 500 ℃, then respectively cleaning the activating agent by using HCl by adopting a suction filtration method, washing by using deionized water until the cleaning solution is neutral, and freeze-drying to obtain the ricepaperplant pith bio-based carbon material.
The electron microscope scanning is carried out on the ricepaperplant pith bio-based carbon material obtained by the preparation method, and the result is shown in fig. 2 and fig. 3, and it can be seen from the figure that the ricepaperplant pith bio-based carbon material presents a two-dimensional porous lamellar structure, the porous structure provides an active position for ion adsorption, and an ion transmission path is also reduced.
The results of comparing the component contents of the doped carbon material obtained by the microwave doping method of the present invention with those of the doped carbon material obtained by the conventional doping method are shown in table 1, and it can be seen from the comparison in table 1 that the doping rate of the doped carbon material obtained by the microwave doping method of the present invention is higher than that of the conventional art.
TABLE 1 comparison of the component ratios of the doped products of different doping methods
Example 1
The preparation method of the ricepaperplant pith bio-based microwave-doped carbon material powder comprises the following preparation methods:
(1) drying the ricepaperplant pith bio-based carbon material in an oven, and removing water;
(2) will be driedPutting the ricepaperplant pith bio-based carbon material and 40% hydrofluoric acid into a microwave reactor, stirring, and introducing inert gas N2Carrying out microwave reaction for 7h at 120 ℃ to obtain a ricepaper pith bio-based microwave doped carbon material solution;
(3) vacuum filtration is adopted, and deionized water is used for cleaning a solvent in the ricepaper pith bio-based microwave doped carbon material solution to obtain ricepaper pith bio-based microwave doped carbon material slurry;
(4) and (3) freeze-drying the ricepaperplant pith bio-based microwave doped carbon material slurry to obtain ricepaperplant pith bio-based microwave doped carbon material powder.
The yield of the ricepaperplant pith bio-based microwave doped carbon material powder obtained in the embodiment is 90%, and the ricepaperplant pith bio-based microwave doped carbon material powder obtained in the embodiment is used for preparing a sulfur positive electrode of a lithium sulfur battery, and the method comprises the following specific steps:
1) mixing a ricepaperplant pith bio-based microwave doped carbon material, a conductive additive and elemental sulfur in a mass ratio of 1:1:2, grinding for 1h, and filling into a polytetrafluoroethylene reaction kettle lining;
2) filling the reaction kettle liner into a glove box, locking, discharging air in the reaction kettle, and preventing the reaction of moisture and oxygen in the air;
3) heating the reaction kettle for 12 hours at 160 ℃ under a vacuum condition to obtain a sulfur-carbon compound containing the ricepaperplant pith bio-based microwave doped carbon material;
4) grinding and mixing a sulfur-carbon compound containing a ricepaperplant biobased microwave doped carbon material with an active substance, a binder and a solvent, and performing ultrasonic treatment for 1h to obtain uniformly dispersed anode slurry;
5) and cutting the copper-plated carbon cloth into pole pieces, soaking the pole pieces in the positive electrode slurry for 5min, and then putting the pole pieces into a vacuum drying oven to dry for 8h at the temperature of 60 ℃ to obtain the positive pole pieces.
The positive electrode plate prepared in example 1 was used in a lithium sulfur battery, and the cycle test and the rate test were performed on the lithium sulfur battery, and the test results are shown in fig. 4 and 5.
It can be seen from the figure that the sulfur positive electrode of the lithium sulfur battery using the ricepaper pith bio-based fluorine-doped carbon material has good reversible capacity and rate capability, and defects can be formed on the surface due to the introduction of fluorine atoms with extremely high electronegativity, so that the conductivity and energy density are improved, the chemical reaction activity is increased, and the wettability is also improved.
Example 2
The preparation method of the ricepaperplant pith bio-based microwave doped carbon material powder comprises the following preparation methods:
(1) drying the ricepaperplant pith bio-based carbon material in an oven, and removing water;
(2) mixing the dried ricepaperplant pith bio-based carbon material and urea in a mass ratio of 4:1, putting the obtained mixture into a microwave reactor, stirring, introducing inert gas, and carrying out microwave reaction for 7 hours at 120 ℃ to obtain ricepaperplant pith bio-based microwave doped carbon material solution;
(3) vacuum filtration is adopted, and deionized water is used for cleaning a solvent in the ricepaper pith bio-based microwave doped carbon material solution to obtain ricepaper pith bio-based microwave doped carbon material slurry;
(4) and (3) freeze-drying the ricepaperplant pith bio-based microwave doped carbon material slurry to obtain ricepaperplant pith bio-based microwave doped carbon material powder.
The yield of the ricepaperplant pith bio-based microwave doped carbon material powder obtained in the embodiment is 92%, and the ricepaperplant pith bio-based microwave doped carbon material powder prepared in the embodiment 2 is used for preparing a sulfur positive electrode of a lithium sulfur battery, and the specific steps are as follows:
1) mixing a ricepaperplant pith bio-based microwave doped carbon material, a conductive additive and elemental sulfur in a mass ratio of 1:1:2, grinding for 1h, and filling into a polytetrafluoroethylene reaction kettle lining;
2) filling the reaction kettle liner into a glove box, locking, discharging air in the reaction kettle, and preventing the reaction of moisture and oxygen in the air;
3) heating the reaction kettle at 160 ℃ for 12h under a vacuum condition to obtain a sulfur-carbon compound containing the ricepaper pith bio-based doped carbon material;
4) grinding and mixing a sulfur-carbon compound containing a ricepaperplant biobased microwave doped carbon material with an active substance, a binder and a solvent, and performing ultrasonic treatment for 1h to obtain uniformly dispersed anode slurry;
5) and cutting the copper-plated carbon cloth into pole pieces, soaking the pole pieces in the positive electrode slurry for 5min, and then putting the pole pieces into a vacuum drying oven to dry for 8h at the temperature of 60 ℃ to obtain the positive pole pieces.
The positive electrode plate obtained in example 2 was used for a supercapacitor cell, and cyclic voltammetry tests were performed, and the test results are shown in fig. 6.
As can be seen from the figure, the ultra-large specific surface area provides a high electric double layer capacitance capacity for the supercapacitor using the ricepaperplant pith bio-based nitrogen-doped carbon material. The doping can generate pseudo-capacitance capacity on one hand, and can promote electron transfer on the other hand, and the transfer resistance of charges in the electrode under high current density is reduced, so that the capacitance performance is improved, and the super capacitor has great application potential.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. The doping method of the bio-based carbon material based on the ricepaperplant pith is characterized by comprising the following steps of:
mixing the ricepaperplant pith bio-based carbon material, the doping compound and the solvent, and carrying out microwave reaction for 3-8h at 60-240 ℃ in an inert gas atmosphere to obtain the ricepaperplant pith bio-based microwave doping carbon material.
2. The doping method according to claim 1, characterized by further comprising the steps of:
and (3) carrying out vacuum filtration, cleaning a reaction solvent in the ricepaperplant pith bio-based microwave doped carbon material by using deionized water to obtain ricepaperplant pith bio-based microwave doped carbon material slurry, and freeze-drying the ricepaperplant pith bio-based microwave doped carbon material slurry to obtain ricepaperplant pith bio-based microwave doped carbon material powder.
3. The doping method according to claim 1 or 2, wherein the reaction procedure of the microwave reaction is as follows: maintaining at 40-60 deg.C for 20-40min, heating to 100-140 deg.C, maintaining for 20-40min, heating to 150-240 deg.C, and maintaining for 180-420 min.
4. The doping method according to claim 3, wherein the doping compound is one of a nitrogen-containing doping compound, a fluorine-containing doping compound, a boron-containing doping compound, and a bromine-containing doping compound.
5. The doping method according to claim 4, wherein the nitrogen-containing compound is one of urea, melamine, polypyrrole, polyaniline, hydrazine, hexamethylenetetramine, and diamine;
the fluorine-containing compound is 10-70% of one of hydrofluoric acid, BF3 diethyl ether, diethylaminosulfur trifluoride and hexafluorophosphoric acid;
the boron-containing compound is boric acid;
the bromine-containing compound is one of bromine chloride, bromine fluoride, bromine trifluoride, bromine pentafluoride and bromine iodide.
6. A ricepaperplant-based bio-based microwave doped carbon material obtained by the doping method of claim 5.
7. A preparation method of a lithium battery pole piece comprises the following steps:
grinding and mixing the ricepaperplant-based bio-based microwave doped carbon material as claimed in claim 6 with active substances, conductive additives, binders and solvents, and then performing ultrasonic treatment to obtain uniformly dispersed slurry;
and cutting the copper-plated carbon cloth into pole pieces, soaking the pole pieces in the slurry, taking out and drying to obtain the pole pieces.
8. A pole piece obtained by the preparation method of claim 7.
9. Use of the pole piece of claim 8 in an energy storage device.
10. Use according to claim 9, wherein the energy storage device is a lithium battery or a super capacitor battery.
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