CN106298249A - A kind of K1.33mn8o16preparation method and application - Google Patents

A kind of K1.33mn8o16preparation method and application Download PDF

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CN106298249A
CN106298249A CN201610828381.1A CN201610828381A CN106298249A CN 106298249 A CN106298249 A CN 106298249A CN 201610828381 A CN201610828381 A CN 201610828381A CN 106298249 A CN106298249 A CN 106298249A
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preparation
potassium
acid
salt
colloidal sol
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CN106298249B (en
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钱东
蒋剑波
李俊华
李军
刘昆
闵紫嫣
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Central South University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/04—Hybrid capacitors
    • H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • 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

Abstract

The invention discloses a kind of K1.33Mn8O16Preparation method and application.Manganous salt, potassium salt and organic carboxyl acid are mixed with water, stirring reaction, obtain colloidal sol；Described colloidal sol, through drying and dewatering, obtains gel；Described gel, through calcining, obtains K1.33Mn8O16.This preparation method is simple and easy to do, has green, environmental protection, safe and cost-effective honest and clean advantage.The K of preparation1.33Mn8O16Make electrode of super capacitor as electrode material, show high reversible the embedding de-behavior of potassium ion and can charge-discharge performance, 110F g can be obtained under 0～1.2V‑1Ratio electric capacity, there is good reversibility and the wide advantage of operating potential window.

Description

A kind of K1.33Mn8O16Preparation method and application
Technical field
The present invention relates to K1.33Mn8O16Preparation method and K1.33Mn8O16Application in ultracapacitor, belongs to super Technical field of capacitor preparation.
Background technology
In recent years, along with the rise of ultracapacitor with electrode material for super capacitor research is goed deep into, embeddedization Compound shows preferable chemical property as electrode material for super capacitor, attracts attention.Wherein, manganio alkali Metal ion intercalation compound because its raw material resources are abundant, low cost and environmental friendliness and the most noticeable.
At present, the manganio alkali metal ion as electrode material for super capacitor is intercalation compound, it has been reported that have three The LiMn of dimension tunnel structure2O4, 3 × 2 Na mixing tunnel structure with 3 × 14Mn9O18(Na0.44MnO2) and layer structure NaMnO2、K0.19MnO2、K0.17MnO2、K0.15MnO2、K0.27MnO2·0.6H2O, etc..
K1.33Mn8O16It is the compound of a kind of synthetic, its crystal structure and the cryptomelane formed in nature (cryptomelane), hollandite (hollandite), side cesarolite (coronadite) identical, for 2 × 2 one-dimensional tunnel knot Structure, the difference with mineral crystal is in its crystal tunnel only to embed K+A kind of ion, and do not have other foreign ion to embed. K1.33Mn8O16Be by Strobel et al. early than nineteen eighty-two purpose based on research, by be electrolysed under 778K potassium vanadate with MnCO3Fused salt and obtain, and first determine its crystal structure (Vicat J, Fanchon E, Strobel P, et al.The structure of K1.33Mn8O16and cation ordering in hollandite-type structures.Acta Crystallographica Section B,1986,42(2):162-167.)。
Chinese patent CN 103288139A discloses one and prepares α-Fe2O3Hollow-core construction and α-Fe2O3/K1.33Mn8O16Receive The method of rice noodle, relates to K1.33Mn8O16Preparation, this patent uses hydrothermal treatment consists potassium permanganate and ammonium fluoride to obtain K1.33Mn8O16 Nano wire.The preparation K identical with this patent1.33Mn8O16The method of nano wire, is also found in other document (Wu J, Wang J, Li H,et al.Designed synthesis of hematite-based nanosorbents for dye removal.Journal of Materials Chemistry A,2013,1(34):9837-9847；Wu J,Li H,Wang J,et al.Swift adsorptive removal of Congo red from aqueous solution by K1.33Mn8O16nanowires.Journal of Nanoscience&Nanotechnology,2013,13(8):5452- 5460)。
Additionally, some documents there was reported and K1.33Mn8O16Structure identical such as AxMn8O16The preparation method of compound.Ratio As, Yamamoto et al. reports and prepares Rb by hydro-thermal method1.5Mn8O16(Yamamoto N,Oka Y,Tamada O.Single crystal growth and structure determination of Rb1.5Mn8O16hollandite.Journal of Mineralogical and Petrological Sciences,1990,15(2):41-49)；Takeuchi et al. reports A kind of synthesis AgxMn8O16Method, too be use hydro-thermal method (Takeuchi K J, Yau S Z, Menard M C, et al.Synthetic control of composition and crystallite size of silver hollandite,AgxMn8O16:Impact on electrochemistry.ACS applied materials& interfaces,2012,4(10):5547-5554)；Lan et al. describes employing molten-salt growth method and is prepared for Na2-xMn8O16Nanometer rods (Lan C,Gong J,Liu S,et al.Synthesis and magnetic properties of single- crystalline Na2-xMn8O16nanorods.Nanoscale Research Letters,2011,6:133)。
About K1.33Mn8O16Application, except reported remove at dyestuff, in addition to application in terms of waste water process, not yet See K1.33Mn8O16Report as electrode material for super capacitor.
Summary of the invention
K is obtained for prior art1.33Mn8O16Technological means limited, existing electrolysis molten-salt growth method energy consumption is big, cost Height, and hydro-thermal method realizes large-scale production and has any problem, and to use the potassium permanganate with strong oxidizing property be raw material, there is safety the most hidden Suffer from；It is an object of the invention to be to provide one to prepare K based on sol-gel process1.33Mn8O16Method, the method energy consumption is low, Low cost, safety and environmental protection, can be with large-scale production.
Another object of the present invention is to be to provide described K1.33Mn8O16As electrode material in ultracapacitor Application, the electrode of preparation has advantage higher than electric capacity, that good reversibility, operating potential window are wide.
In order to realize above-mentioned technical purpose, the invention provides a kind of K1.33Mn8O16Preparation method, the method is by two Valency manganese salt, potassium salt and organic carboxyl acid mix with water, 40～80 DEG C of stirring reactions, obtain colloidal sol；Described colloidal sol is through 80～150 DEG C drying and dewatering, obtains gel；Described gel is placed in 200～800 DEG C of temperature lower calcinations, to obtain final product.
Preferably scheme, the ratio of potassium salt, manganous salt and organic carboxyl acid is by K: Mn: the amount ratio of the material of organic carboxyl acid is 0.17～0.25: 1: 1～3 meterings.Most preferably scheme, potassium salt (KHCO3), manganous salt (Mn (Ac)2·H2And citric acid O) Ratio by K: the amount ratio of the material of Mn: organic carboxyl acid be 0.17: 1: 1 metering.
More preferably scheme, manganous salt includes at least one in manganese acetate, manganese acetate hydrate and manganese carbonate.More excellent Elect a hydration manganese acetate as.
More preferably scheme, potassium salt includes at least in potassium acetate, potassium acetate hydrate, potassium carbonate and potassium bicarbonate Kind.More preferably potassium acetate or potassium bicarbonate.
More preferably scheme, organic carboxyl acid includes at least one in citric acid, tartaric acid and oxalic acid.More preferably Fructus Citri Limoniae Acid.
More preferably scheme, manganous salt, potassium salt and organic carboxyl acid and water, 65～75 DEG C of stirring reactions, obtain colloidal sol. Preferred reaction temperature is 70 DEG C.The time of stirring reaction is until various raw material fully dissolves, and has a large amount of vitreosol Being formed, this belongs to the category that originally those of skill will appreciate that.
More preferably scheme, colloidal sol is through 105～115 DEG C of drying and dewaterings.Preferred drying temperature is 110 DEG C.
More preferably scheme, gel is placed in 400～700 DEG C of temperature lower calcinations.Preferred calcining heat is 550 DEG C.Forge The burning time is generally 2～12h, suitably regulates according to the size of calcining heat.
Present invention also offers described K1.33Mn8O16Application, this application is by K1.33Mn8O16Apply as electrode material In preparing ultracapacitor.
Preferably scheme, by K1.33Mn8O16, conductive agent and bonding agent mixing after, coating on a current collector, prepare super electricity Container electrode.
More preferably scheme, by K1.33Mn8O16(as active substance), acetylene black (conventional conductive agent) and politef (conventional binding agent) is according to mass ratio K1.33Mn8O16: the ratio mixing of acetylene black: politef=80:10～15:5～10； Collector uses the 316L stainless (steel) wire of 300～400 mesh；Electrolyte is 0.1～0.64mol L-1Potassium sulfate solution or 0.5～3.13mol L-1Alkitrate.Further preferred version is 0.5mol L for using concentration-1Sulphuric acid Aqueous solutions of potassium or 2mol L-1Alkitrate.
Hinge structure, the Advantageous Effects that technical scheme is brought is:
1, technical scheme, uses the oxidation pathway of Mn (II) → Mn (IV) to prepare K1.33Mn8O16, rather than Mn (VII) original route of going back of → Mn (IV) prepares K1.33Mn8O16, it is to avoid traditional method need to use KMnO4For raw material, and there is peace The drawback of full hidden danger, thus preparation technology has the more preferable advantage of safety.
2, technical scheme, uses without Cl-Or NO3 -Manganous salt be raw material, it is to avoid in calcination process Because of containing Cl-Or NO3 -HCl, the NO produced2Deng the shortcoming of toxic and harmful, thus preparation technology have green, environmental protection excellent Point.
3, technical scheme, realizes the preparation of colloidal sol and gel at a lower temperature, and at middle cryogenic conditions Under carry out roasting, it is achieved K1.33Mn8O16Preparation, there is the advantage that preparation technology energy consumption is relatively low.
4, technical scheme, the cost of material of employing is cheap, preparation is simple and energy consumption is low, thus tool There are low cost and the advantage of applicable large-scale production.
5, technical scheme, the K of preparation1.33Mn8O16It is used for preparing electrode of super capacitor as electrode material, Embedding-de-behavior of potassium ion with high reversible and can charge-discharge performance, 110F g can be obtained under 0～1.2V-1Ratio electricity Hold, the advantages such as reversibility of electrode is good, operating potential window width, K1.33Mn8O16Can use as the electrode material of a kind of high-quality In ultracapacitor, widen K1.33Mn8O16Range of application.
Accompanying drawing explanation
[Fig. 1] is the K of embodiment 1 preparation1.33Mn8O16XRD figure.
[Fig. 2] is the K of embodiment 2 preparation1.33Mn8O16FTIR figure.
[Fig. 3] is K in embodiment 31.33Mn8O16Positive pole is 1mV s at potential scan rate-1Time, different termination scans electricity Cyclic voltammetry curve under gesture.
[Fig. 4] is K in embodiment 41.33Mn8O16Positive pole is when voltage range is 0～1.2V (vs.SCE), and different electric currents are close Charging and discharging curve under Du.
Detailed description of the invention
Following example are more fully described present invention, but are not limiting as the protection domain of the claims in the present invention.
Embodiment 1
By a certain amount of Mn (Ac)2·H2O and citric acid (CA) mixing, make the amount of material ratio for Mn/CA=1, add 60mL Distilled water, is placed in 70 DEG C of water-baths heating magnetic agitation, makes mixture fully dissolve.Add a certain amount of again in this solution KHCO3, make the amount of material ratio for K/Mn=0.17, after being sufficiently stirred for dissolving, products therefrom is colourless through laser pen candling Bright colloidal sol.Colloidal sol is dried at 110 DEG C, obtains white gels.By finely ground for the above-mentioned gel porcelain being placed on 60cm × 90cm In boat and will be equipped with the porcelain boat of gel and be placed in Muffle furnace, with 8 DEG C of min-1Ramp to 550 DEG C, and be incubated 6h.Cold To room temperature, take out porcelain boat, obtain product.Products therefrom is carried out thing on X-ray powder diffractometer (Dandong, Y-3000) Facies analysis, test condition is: tube current 25mA, voltage 40KV, slit width 2nm, and 2 θ angular scan ranges are 10 °～80 °.Test Result is shown in accompanying drawing 1.It will be noted from fig. 1 that the XRD diffraction maximum of product and K1.33Mn8O16Standard card (PDF#77-1796) Cause, show that products therefrom is K1.33Mn8O16。
Embodiment 2
By a certain amount of MnCO3And citric acid (CA) mixing, make the amount of material distill than for Mn/CA=1, addition 70mL Water, is placed in 60 DEG C of water-baths heating magnetic agitation, makes mixture fully dissolve.Add a certain amount of again in this solution K2CO3, the amount making material is 0.25 than K/Mn, be sufficiently stirred for dissolve after products therefrom through laser pen candling be water white transparency Colloidal sol.Colloidal sol is dried at 110 DEG C, obtains white gels.By finely ground for the above-mentioned gel porcelain boat being placed on 60cm × 90cm In and will be equipped with the porcelain boat of gel and be placed in Muffle furnace, with 8 DEG C of min-1Ramp to 650 DEG C, and be incubated 4h.It is cooled to After room temperature, take out porcelain boat, obtain product.Through XRD analysis, this product proves that with the product in embodiment 1 be same substance.Should Product (Thermo scientific, Nicolet iS10) on FT-IR spectrogrph carries out infrared spectrum analysis, test condition For: number of sample scan 32, resolution 4.0, gain 8.0 of sampling, wave number sweep limits 400～4000cm-1.Test result is shown in attached Fig. 2.From fig. 2 it can be seen that 400～700cm-1Occur in that 4 absworption peaks in wave-number range, lay respectively at 694,594, 522 and 481cm-1, this is caused by the lattice vibration of Mn-O, meets tunnel structure MnO2Characteristic infrared absorption, show institute Obtain product and there is one-dimensional tunnel structure.
Embodiment 3
By K prepared in embodiment 11.33Mn8O16Powder, acetylene black and politef (PTFE) press 80:15:5's Mass ratio mixes, after adding a small amount of distilled water and ethanol, continuously stirred, is rubber pureed to mixture, is rolled into thickness Degree be about 10 μm thin film, thin film is cut into the thin slice of a size of 1cm × 1cm, by thin slice under the pressure of 12MPa with 300 Mesh 316L stainless (steel) wire pressure knot together, is placed in 120 DEG C of vacuum drying ovens and is dried 8h, make electrode slice.With platinum plate electrode it is To electrode, saturated calomel electrode is reference electrode, prepared K1.33Mn8O16Electrode is working electrode, with 0.5mol L-1Sulfur Acid potassium solution is electrolyte, uses CHI760d electrochemical workstation, and arranging potential scan rate is 1mV s-1, respectively 0～ 0.1V (vs.SCE), 0～0.2V (vs.SCE), 0～0.3V (vs.SCE), 0～0.5V (vs.SCE), 0～0.6V (vs.SCE), 0～0.7V (vs.SCE), 0～0.8V (vs.SCE), 0～0.9V (vs.SCE), 0～1.0V (vs.SCE) and 0～1.1V (vs.SCE) volt-ampere test it is circulated in potential range.Test result is shown in accompanying drawing 3.It can be seen in figure 3 that terminate in difference Under scanning electromotive force, K1.33Mn8O16The transverse axis that the cyclic voltammetry curve of positive pole all presents along zero crossing is almost specular Symmetry, shows K1.33Mn8O16Just having the K of high reversible+Abjection-embedded performance.
Embodiment 4
According to method preparation work electrode and the assembling three-electrode system of embodiment 3, with 2mol L-1Potassium nitrate solution is Electrolyte, uses CHI760d electrochemical workstation, respectively 100,500 and 1000mA g-1Electric current density under carry out charge and discharge Electrical testing.Test result is shown in accompanying drawing 4.It can be seen from figure 4 that K1.33Mn8O16Positive pole shows good fake capacitance characteristic, and And charging and discharging curve is symmetrical, shows that electrode material has good charge-discharge performance.
The explanation of above example is only the method and the core concept thereof that help to understand the present invention.It should be pointed out that, for this For the those of ordinary skill of technical field, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out some Improve and modify, within these improve and modify the protection domain falling into the claims in the present invention.

Claims (10)

1. a K1.33Mn8O16Preparation method, it is characterised in that: manganous salt, potassium salt and organic carboxyl acid are mixed with water, 40～80 DEG C of stirring reactions, obtain colloidal sol；Described colloidal sol, through 80～150 DEG C of drying and dewaterings, obtains gel；Described gel is placed in 200～800 DEG C of temperature lower calcinations, to obtain final product.
K the most according to claim 11.33Mn8O16Preparation method, it is characterised in that: potassium salt, manganous salt and organic carboxylic The ratio of acid is by K: the amount ratio of the material of Mn: organic carboxyl acid is 0.17～0.25: 1: 1～3 meterings.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: described manganous salt includes At least one in manganese acetate, manganese acetate hydrate and manganese carbonate.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: described potassium salt includes acetic acid At least one in potassium, potassium acetate hydrate, potassium carbonate and potassium bicarbonate.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: described organic carboxyl acid includes At least one in citric acid, tartaric acid and oxalic acid.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: manganous salt, potassium salt and organic Carboxylic acid and water, 65～75 DEG C of stirring reactions, obtain colloidal sol.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: colloidal sol is through 105～115 DEG C Drying and dewatering.
K the most according to claim 1 and 21.33Mn8O16Preparation method, it is characterised in that: gel is placed in 400～700 DEG C Temperature lower calcination.
9.K1.33Mn8O16Application, it is characterised in that: be applied to prepare ultracapacitor as electrode material.
K the most according to claim 91.33Mn8O16Application, it is characterised in that: by K1.33Mn8O16, conductive agent and bonding After agent mixing, coating on a current collector, prepares electrode of super capacitor.
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CN109830671A (en) * 2019-03-06 2019-05-31 四川大学 A kind of tunnel recombination structure material and the sodium-ion battery positive material using tunnel recombination structure material preparation

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