CN116514099A - Preparation method and application of high-performance bamboo charcoal nano material - Google Patents
Preparation method and application of high-performance bamboo charcoal nano material Download PDFInfo
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- CN116514099A CN116514099A CN202310509620.7A CN202310509620A CN116514099A CN 116514099 A CN116514099 A CN 116514099A CN 202310509620 A CN202310509620 A CN 202310509620A CN 116514099 A CN116514099 A CN 116514099A
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- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 141
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 141
- 241001330002 Bambuseae Species 0.000 title claims abstract description 141
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 141
- 239000011425 bamboo Substances 0.000 title claims abstract description 141
- 239000003610 charcoal Substances 0.000 title claims abstract description 105
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 238000000967 suction filtration Methods 0.000 claims abstract description 11
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 9
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 9
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 9
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 29
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000007772 electrode material Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011112 process operation Methods 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 239000003990 capacitor Substances 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 11
- 230000014759 maintenance of location Effects 0.000 description 9
- 229910000474 mercury oxide Inorganic materials 0.000 description 8
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 8
- 238000004146 energy storage Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 239000004966 Carbon aerogel Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- -1 pyrrole compound Chemical class 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241000609240 Ambelania acida Species 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Classifications
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- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- 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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- 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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
-
- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- 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
- Y02E60/13—Energy storage using capacitors
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- Inorganic Chemistry (AREA)
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- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Environmental & Geological Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to the technical field of nano material preparation, and discloses a preparation method and application of a high-performance bamboo charcoal nano material. The said makingThe preparation method comprises the following steps: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning, standing, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying; mixing the dried bamboo charcoal with FePO 4 Mixing and ball milling the nano particles, and treating the ball-milled mixture with plasma to obtain a bamboo charcoal compound; sequentially mixing a cobalt nitrate solution, a sodium molybdate solution, a bamboo charcoal compound and ethylene glycol, and calcining at a high temperature; ball milling the calcined product to obtain the bamboo charcoal nano material. The preparation method has the characteristics of simple process operation, high repeatability, low cost, wide raw material sources and the like.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method and application of a high-performance bamboo charcoal nano material.
Background
Supercapacitors, as a critical class of energy storage devices, have many advantages, such as: higher power density, high charging speed, strong discharging capability under high current, high energy conversion efficiency and small loss in the process, the energy circulation efficiency can reach more than 90%, the longer circulation service life has wide working temperature range, and the energy circulation device is environment-friendly, green and pollution-free, and is an ideal environment-friendly power supply. In recent years, the method is widely applied to various fields of automobiles, electronic equipment, communication products and the like.
Supercapacitors, also known as electrochemical capacitors, double layer capacitors, are a new type of element between batteries and traditional capacitors that use polarized electrolyte to store energy. Supercapacitors can be classified into electric double layer capacitors based on an electrode/electrolyte interface and pseudocapacitors based on a highly reversible rapid redox reaction occurring at an electrode/electrolyte interface, depending on the energy storage mechanism. The electrode materials of the electric double layer capacitor are mainly various carbon materials with high specific surface area, such as active carbon, carbon nano tube, carbon aerogel and the like. Due to the price factors of carbon nanotubes and carbon aerogels, activated carbon has been widely used due to its low price. However, the specific volume of the supercapacitor of the activated carbon material is generally not high.
In recent years, new energy fields using electric power as power are vigorously developed, and super capacitors become one of important applications of biomass energy materials in the field of energy storage materials. Although tobacco stems, rice hulls, bagasse and the like are widely used as capacitor materials, the use of a large amount of binder may block part of pore channels, increase the overall resistance of the electrode material, reduce the specific surface area of the electrode material and reduce the overall capacitance of the electrode. The bamboo resources in China are rich, and the bamboo industry is one of ten green rich industries which are developed mainly in forestry, and is one of countries with the largest bamboo yield in the world. Bamboo is used in the background of timber resource shortage and low carbon economy developmentIs a non-woody resource and increasingly shows the resource value. The bamboo charcoal is a porous solid material formed by taking bamboo as a raw material and calcining at high temperature, and has the characteristics of higher specific surface area, considerable pore size structure and excellent conductivity, so that the bamboo charcoal can be used as an electrode material of a supercapacitor. However, few reports on bamboo resources as precursors of supercapacitor materials are made. The supercapacitor electrode material commonly known in the art, namely the bamboo charcoal/metal oxide composite, is used as the electrode material, although MnO 2 Has excellent theoretical high specific capacity and low price, and is widely applied to pseudocapacitance electrode materials. However, in practical application studies, mnO was found 2 Poor conductivity results in poor cycling stability of the composite material during high current density charge and discharge.
Disclosure of Invention
In view of the above, in order to solve the problems of poor long-term cycle performance and the like of the existing manganese-loaded carbon-based composite material serving as a supercapacitor material, the invention aims to provide a preparation method and application of a nano material with bamboo charcoal serving as a supercapacitor electrode. The preparation method has the characteristics of simple process operation, high repeatability, low cost, wide raw material sources and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the high-performance bamboo charcoal nano material comprises the following steps:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1-2 h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60-80 ℃ for 12-36 h;
step two: mixing the dried bamboo charcoal with FePO 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling for 10-12 h, and treating the ball-milled mixture with plasma for 40-80 s to obtain a bamboo charcoal compound;
step three: sequentially mixing cobalt nitrate solution, sodium molybdate solution, bamboo charcoal compound and ethylene glycol, placing the mixture in a stainless steel high-pressure reaction kettle, preserving heat for 10-12 h at 180 ℃, and calcining for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and ball milling for 8-10 hours to obtain the bamboo charcoal nano material.
Preferably, before the bamboo is prepared into the bamboo charcoal, the method further comprises the following treatment processes: slicing untreated bamboo along the cross section, and drying in a blast oven at 60-80 ℃ for 12-24 hours; crushing dried bamboo, sieving with a 50-100 mesh sieve, adding 5-10 parts by weight of sieved bamboo powder into 10-15 parts by weight of 1 mmol/ferric trichloride solution, slowly dripping 0.5-2 parts by weight of pyrrole with a dropper, performing ultrasonic treatment for 30min after dripping, transferring the mixed solution into a vacuum bottle, soaking for 12-24 h under the vacuum pressure of 0.1MPa, filtering, washing the precipitate with deionized water until the precipitate is colorless, drying under the vacuum condition at 65 ℃, and crushing into powder to obtain modified bamboo.
Preferably, the ultrasonic power is 200-800W and the frequency is 25-45 kHz during ultrasonic treatment.
Preferably, the preparation method of the bamboo charcoal comprises the steps of mixing 5-10 parts by weight of dodecyl dimethyl benzyl ammonium chloride and 10-100 parts by weight of water, placing the mixture in a heating and stirring container, heating to 200 ℃ at a heating rate of 1 ℃/min at a rotating speed of 300r/min, adding 5-10 parts by weight of sodium chloride, continuously stirring for 30min, adding 30-50 parts by weight of modified bamboo, heating to 900 at a heating rate of 5 ℃/min, preserving heat for 2h, taking out carbide after automatically cooling to room temperature, grinding the carbide into powder by using a mortar, soaking the powder in ultrapure water for 12-24 h, carrying out suction filtration, and drying at 60-80 ℃ for 5-10 h to obtain the modified bamboo charcoal.
Preferably, in the third step, 0.1 to 10 parts by weight of the bamboo charcoal compound, 6 to 10 parts by weight of 1mmol/L cobalt nitrate solution, 6 to 10 parts by weight of 1mmol/L sodium molybdate solution and 10 to 20 parts by weight of ethylene glycol are added.
Preferably, in the second step, 0.1 to 10 parts by weight of bamboo charcoal and FePO are added 4 0.1 to 10 portions of nano particles.
Preferably, in the second and fourth steps, the ball milling is performed by an omnibearing planetary ball mill.
Preferably, the rotation speed in the ball milling in the second step is 450r/min; and in the fourth step, the rotating speed is 500r/min during ball milling.
Preferably, the prepared bamboo charcoal nanomaterial is applied as an electrode material of a supercapacitor.
According to the technical scheme, the invention discloses a preparation method of the high-performance bamboo charcoal nano material, and the preparation method has the characteristics of simplicity and easiness in operation, strong repeatability, low cost, no pollution to the environment and the like. The bamboo charcoal nano material prepared by the preparation method provided by the invention is used as an electrode material of the super capacitor, so that the specific capacitance of the super capacitor can be further improved, and the cycle performance of the super capacitor is enhanced.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, the bamboo is pretreated, ferric trichloride and pyrrole are mixed and then are subjected to dipping treatment together with vacuum operation, the bamboo carbon/pyrrole compound is formed through the dipping treatment, nitrogen atoms are successfully doped into the bamboo, and the bamboo carbon material has a good pore structure and a high specific surface area through the later carbonization process, so that a good foundation is laid for applying the bamboo carbon to the electrode material of the supercapacitor in the later stage.
2. According to the invention, not only is bamboo modified, but also sodium chloride and a surfactant are added when the bamboo charcoal is prepared, and the rare gas which is filled with milk when the bamboo charcoal is calcined at high temperature is successfully replaced by adding the sodium chloride, so that the added sodium chloride can completely isolate air to completely wrap the bamboo charcoal when the bamboo charcoal is calcined at high temperature, the pores formed by carbonizing the bamboo charcoal at high temperature are more uniform, and the diameter of the pores inside the bamboo charcoal is reduced after the added surfactant is mixed with the bamboo charcoal and calcined at high temperature, so that the nano charcoal structure is formed in order.
3. The invention not only carries out modification process on bamboo and bamboo charcoal respectively in the earlier stage, but also carries out the preparation process when preparing the bamboo charcoal nano materialAdding FePO4 nano particles in one step, and carrying out plasma treatment to ensure that the bamboo charcoal and the FePO are prepared 4 The nano particles are fully fused and activated, so that the high specific surface area of the bamboo charcoal is utilized while the good conductivity is provided for the electrode material prepared in the future, the energy storage performance of the electrode material of the super capacitor is obviously improved, namely the pseudocapacitance of the electrode material is obviously improved.
4. The invention not only improves the energy storage performance of the electrode material, but also improves the energy storage performance of the electrode material by adopting CoMoO 4 The nano hybrid material is formed by further compounding the bamboo charcoal, so that the long-term durability of the electrode material of the supercapacitor is improved, namely the cycle performance of the supercapacitor is remarkably improved, and the capacitance retention rate of the supercapacitor is remarkably improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The application method of the bamboo charcoal nano material as the electrode material of the super capacitor specifically comprises the following steps:
the bamboo charcoal nano material prepared by the invention and the polytetrafluoroethylene solution with the mass fraction of 5% of acetylene black are mixed according to the mass ratio of 8:1:1, uniformly mixing, ultrasonically dispersing for 30min, stirring for 30min, drying in a 100 ℃ oven for 6h, pouring the dried powder on a 60 ℃ electric hot plate, dripping a proper amount of absolute ethyl alcohol for infiltration, repeatedly kneading and pressing the mixture to bond the mixture together and spread the mixture into slices with the thickness of 2.5mm, and drying in the 80 ℃ oven for 4h; the sheet was cut into an electrode sheet of about 2mg, and the electrode sheet was loaded on a 1cm×0.5cm (length×width) foam nickel under 8MPa by an oil press to prepare a bamboo charcoal electrode.
Example 2
The preparation method of the high-performance bamboo charcoal nano material comprises the following steps:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60 ℃ for 24h;
step two: 10 parts of dried bamboo charcoal and 10 parts of FePO are mixed according to parts by weight 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling the mixture for 11 hours at a speed of 450r/min by using an omnibearing planetary ball mill, and treating the ball-milled mixture with plasma for 80 seconds to obtain a bamboo charcoal compound;
step three: according to parts by weight, 6 parts of 1mmol/L cobalt nitrate solution, 6 parts of 1mmol/L sodium molybdate solution, 1 part of bamboo charcoal compound and 15 parts of ethylene glycol are sequentially mixed and then placed in a stainless steel high-pressure reaction kettle, heat preservation is carried out for 11h at 180 ℃, and calcination is carried out for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and performing ball milling for 9 hours at a speed of 500r/min by using an omnibearing planetary ball mill to obtain the bamboo charcoal nano material. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific charge/discharge capacity of 283F/g for the first time under the current density of 10A/g, and after 5000 times of long-cycle charge/discharge test, the specific charge capacity can still be kept at 263F/g, and the specific charge capacity retention rate is 93%.
Example 3
The preparation method of the high-performance bamboo charcoal nano material comprises the following steps:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60 ℃ for 24h;
step two: 10 parts of dried bamboo charcoal and 10 parts of FePO are mixed according to parts by weight 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling the mixture for 11 hours at a speed of 450r/min by using an omnibearing planetary ball mill, and treating the ball-milled mixture with plasma for 40 seconds to obtain a bamboo charcoal compound;
step three: according to parts by weight, 6 parts of 1mmol/L cobalt nitrate solution, 6 parts of 1mmol/L sodium molybdate solution, 1 part of bamboo charcoal compound and 15 parts of ethylene glycol are sequentially mixed and then placed in a stainless steel high-pressure reaction kettle, heat preservation is carried out for 11h at 180 ℃, and calcination is carried out for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and performing ball milling for 9 hours at a speed of 500r/min by using an omnibearing planetary ball mill to obtain the bamboo charcoal nano material. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific charge/discharge capacity of 282F/g for the first time under the current density of 10A/g, and after 5000 times of long-cycle charge/discharge test, the specific charge capacity can still be kept at 262F/g, and the specific charge capacity retention rate is 92.9%.
Example 4
The preparation method of the high-performance bamboo charcoal nano material comprises the following steps:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60 ℃ for 24h;
step two: according to the weight parts, 1 part of dried bamboo charcoal and 10 parts of FePO 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling the mixture for 11 hours at a speed of 450r/min by using an omnibearing planetary ball mill, and treating the ball-milled mixture with plasma for 80 seconds to obtain a bamboo charcoal compound;
step three: according to parts by weight, 6 parts of 1mmol/L cobalt nitrate solution, 6 parts of 1mmol/L sodium molybdate solution, 1 part of bamboo charcoal compound and 15 parts of ethylene glycol are sequentially mixed and then placed in a stainless steel high-pressure reaction kettle, heat preservation is carried out for 11h at 180 ℃, and calcination is carried out for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and performing ball milling for 9 hours at a speed of 500r/min by using an omnibearing planetary ball mill to obtain the bamboo charcoal nano material. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific capacitance of 278F/g for the first time under 10A/g current density, and after 5000 times of long-cycle charge-discharge test, the specific capacitance is 256F/g and the specific capacitance retention rate is 92.09%.
Example 5
The preparation method of the high-performance bamboo charcoal nano material comprises the following steps:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60 ℃ for 24h;
step two: 10 parts of dried bamboo charcoal and 1 part of FePO are mixed according to parts by weight 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling the mixture for 11 hours at a speed of 450r/min by using an omnibearing planetary ball mill, and treating the ball-milled mixture with plasma for 80 seconds to obtain a bamboo charcoal compound;
step three: according to parts by weight, 6 parts of 1mmol/L cobalt nitrate solution, 6 parts of 1mmol/L sodium molybdate solution, 1 part of bamboo charcoal compound and 15 parts of ethylene glycol are sequentially mixed and then placed in a stainless steel high-pressure reaction kettle, heat preservation is carried out for 11h at 180 ℃, and calcination is carried out for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and performing ball milling for 9 hours at a speed of 500r/min by using an omnibearing planetary ball mill to obtain the bamboo charcoal nano material. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific charge/discharge capacity of 275F/g for the first time under the current density of 10A/g, and after 5000 times of long-cycle charge/discharge test, the specific charge capacity is 248F/g, and the specific charge capacity retention rate is 90.18%.
Example 6
The preparation method of the bamboo charcoal comprises the steps of mixing 8 parts of dodecyl dimethyl benzyl ammonium chloride and 40 parts of water according to parts by weight, placing the mixture in a heating and stirring container, heating to 200 ℃ at a heating rate of 1 ℃/min at a rotating speed of 300r/min, adding 5 parts of sodium chloride, continuously stirring for 30min, adding 30 parts of modified bamboo, heating to 900 at a heating rate of 5 ℃/min, preserving heat for 2h, taking out a carbide after the carbide is automatically cooled to room temperature, grinding the carbide into powder by using a mortar, soaking the powder in ultrapure water for 12h, carrying out suction filtration, and drying at 60 ℃ for 5h to obtain the modified bamboo charcoal. The remaining process parameters and procedures were exactly the same as in example 2. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific capacitance of 289F/g for the first time under 10A/g current density, and after 5000 times of long-cycle charge-discharge test, the specific capacitance can still be kept at 272F/g, and the specific capacitance retention rate is 94.12%.
Example 7
The preparation method of the bamboo charcoal comprises the steps of mixing, by weight, 8 parts of dodecyl dimethyl benzyl ammonium chloride and 80 parts of water, placing the mixture in a heating and stirring container, heating to 200 ℃ at a heating rate of 1 ℃/min at a rotating speed of 300r/min, adding 8 parts of sodium chloride, continuously stirring for 30min, adding 40 parts of modified bamboo, heating to 900 at a heating rate of 5 ℃/min, preserving heat for 2h, taking out a carbide after the bamboo charcoal is automatically cooled to room temperature, grinding the carbide into powder by using a mortar, soaking the powder in ultrapure water for 18h, carrying out suction filtration, and drying at 80 ℃ for 10h to obtain the modified bamboo charcoal. The remaining process parameters and procedures were exactly the same as in example 2. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has initial charge-discharge specific capacitance of 291F/g under 10A/g current density, and after 5000 times of long-cycle charge-discharge test, the specific capacitance can still be maintained at 275F/g, and the specific capacitance retention rate is 94.5%.
Example 8
Before the bamboo is prepared into the bamboo charcoal, the method further comprises the following treatment processes: slicing untreated bamboo along the cross section, and drying in a blast oven at 60deg.C for 12 hr; pulverizing dried bamboo, sieving with a 50-mesh sieve, adding 5 parts of sieved bamboo powder into 10 parts of 1 mmol/ferric trichloride solution according to parts by weight, slowly dripping 0.5 part of pyrrole with a dropper, performing ultrasonic treatment for 30min after dripping, transferring the mixed solution into a vacuum bottle, soaking for 12h under the vacuum pressure of 0.1MPa, filtering, washing the precipitate with deionized water until the precipitate is colorless, drying under the vacuum condition at 65 ℃, and pulverizing into powder to obtain modified bamboo; the ultrasonic power is 200W and the frequency is 25kHz during ultrasonic treatment; the remaining process parameters and procedure were exactly the same as in example 7. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific charge/discharge capacity of 301F/g for the first time under the current density of 10A/g, and after 5000 times of long-cycle charge/discharge test, the specific charge capacity can still be kept at 286F/g, and the specific charge capacity retention rate is 95.02%.
Example 9
Before the bamboo is prepared into the bamboo charcoal, the method further comprises the following treatment processes: slicing untreated bamboo along the cross section, and drying in a blast oven at 80deg.C for 18 hr; pulverizing dried bamboo, sieving with a 50-mesh sieve, adding 5 parts of sieved bamboo powder into 15 parts of 1 mmol/ferric trichloride solution according to parts by weight, slowly dripping 1 part of pyrrole with a dropper, performing ultrasonic treatment for 30min after dripping, transferring the mixed solution into a vacuum bottle, soaking for 24h under vacuum pressure of 0.1MPa, filtering, washing the precipitate with deionized water until the precipitate is colorless, drying under vacuum condition at 65 ℃, and pulverizing into powder to obtain modified bamboo; the ultrasonic power is 450W and the frequency is 30kHz during ultrasonic treatment. The remaining process parameters and procedure were exactly the same as in example 7. The three-electrode device with 6mol/LKOH as electrolyte, mercury oxide as reference electrode, platinum sheet as counter electrode and bamboo charcoal electrode as working electrode has a specific charge/discharge capacity of 308F/g for the first time under the current density of 10A/g, and after 5000 times of long-cycle charge/discharge test, the specific charge capacity can still be kept at 295F/g, and the specific charge capacity retention rate is 95.78%.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the high-performance bamboo charcoal nano material is characterized by comprising the following steps of:
step one: adding bamboo charcoal into a beaker filled with concentrated hydrochloric acid, ultrasonically cleaning for 30min, standing for 1-2 h, performing suction filtration, cleaning the precipitate with deionized water for multiple times, and drying at 60-80 ℃ for 12-36 h;
step two: mixing the dried bamboo charcoal with FePO 4 Mixing the nano particles, putting the mixture into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, ball milling for 10-12 h, and treating the ball-milled mixture with plasma for 40-80 s to obtain a bamboo charcoal compound;
step three: sequentially mixing cobalt nitrate solution, sodium molybdate solution, bamboo charcoal compound and ethylene glycol, placing the mixture in a stainless steel high-pressure reaction kettle, preserving heat for 10-12 h at 180 ℃, and calcining for 3h at 300 ℃ under the protection of nitrogen;
step four: and (3) putting the calcined product into a ball milling tank, adding zirconia balls according to a ball-to-material ratio of 20:1, and ball milling for 8-10 hours to obtain the bamboo charcoal nano material.
2. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 1, wherein in the third step, 0.1 to 10 parts by weight of the bamboo charcoal composite, 6 to 10 parts by weight of 1mmol/L cobalt nitrate solution, 6 to 10 parts by weight of 1mmol/L sodium molybdate solution and 10 to 20 parts by weight of ethylene glycol are added.
3. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 1, wherein in the second step, 0.1-10 parts by weight of bamboo charcoal and FePO are added 4 0.1 to 10 portions of nano particles.
4. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 1, wherein in the second and fourth steps, the ball milling is performed by an omnibearing planetary ball mill.
5. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 1, wherein the rotational speed during ball milling in the second step is 450r/min; and in the fourth step, the rotating speed is 500r/min during ball milling.
6. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 1, wherein the bamboo, before being prepared into bamboo charcoal, further comprises the following treatment process: slicing untreated bamboo along the cross section, and drying in a blast oven at 60-80 ℃ for 12-24 hours; crushing dried bamboo, sieving with a 50-100 mesh sieve, adding 5-10 parts by weight of sieved bamboo powder into 10-15 parts by weight of 1 mmol/ferric trichloride solution, slowly dripping 0.5-2 parts by weight of pyrrole with a dropper, performing ultrasonic treatment for 30min after dripping, transferring the mixed solution into a vacuum bottle, soaking for 12-24 h under the vacuum pressure of 0.1MPa, filtering, washing the precipitate with deionized water until the precipitate is colorless, drying under the vacuum condition at 65 ℃, and crushing into powder to obtain modified bamboo.
7. The method for preparing high-performance bamboo charcoal nanomaterial according to claim 6, wherein the ultrasonic power is 200-800W and the frequency is 25-45 kHz during ultrasonic treatment.
8. The method for preparing high-performance bamboo charcoal nano-material according to claim 1, wherein the method for preparing the bamboo charcoal is characterized in that, according to parts by weight, 5-10 parts of dodecyl dimethyl benzyl ammonium chloride and 10-100 parts of water are mixed and placed in a heating and stirring container, the heating rate is 1 ℃/min, the rotating speed is 300r/min, the heating is up to 200 ℃, 5-10 parts of sodium chloride is added, the stirring is continued for 30min, then 30-50 parts of modified bamboo is added, the heating rate is 5 ℃/min, the heating is up to 900, the heat preservation is carried out for 2h, the carbide is taken out after the bamboo charcoal is automatically cooled to room temperature, the carbide is ground into powder by a mortar, the ultra-pure water is used for soaking for 12-24 h, the suction filtration is carried out, and the modified bamboo charcoal is obtained after the modified bamboo charcoal is dried at 60-80 ℃.
9. A high-performance bamboo charcoal nano material is characterized in that: the high-performance bamboo charcoal nanomaterial prepared by the method of any one of claims 1 to 8.
10. Use of the high-performance bamboo charcoal nanomaterial according to claim 9 in supercapacitor electrode materials.
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