CN104591120A - Preparation of rough-surface microspherical manganese dioxide and application to supercapacitors - Google Patents

Preparation of rough-surface microspherical manganese dioxide and application to supercapacitors Download PDF

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Publication number
CN104591120A
CN104591120A CN201310528353.4A CN201310528353A CN104591120A CN 104591120 A CN104591120 A CN 104591120A CN 201310528353 A CN201310528353 A CN 201310528353A CN 104591120 A CN104591120 A CN 104591120A
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China
Prior art keywords
preparation
microspherical
rough
manganese dioxide
ellipsoid shape
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CN201310528353.4A
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Chinese (zh)
Inventor
谷涛
沈绍典
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WUXI HUAZHEN NEW ENERGY TECHNOLOGY Co Ltd
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WUXI HUAZHEN NEW ENERGY TECHNOLOGY Co Ltd
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Priority to CN201310528353.4A priority Critical patent/CN104591120A/en
Publication of CN104591120A publication Critical patent/CN104591120A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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Abstract

The invention relates to a preparation method for ellipsoid-shaped mesoporous carbon, especially relates to a method which comprises taking ellipsoid-shaped mesoporous silicon dioxide as a hard template, filling tunnels of silicon dioxide with grease and carbonizing at inert atmosphere for forming porous carbon with corresponding morphologies. The invention discloses a preparation method for rough-surface microspherical manganese dioxide applicable as a supercapacitor material. Namely, rough-surface microspherical manganese dioxide is prepared by employing a hydrothermal process to process a potassium permanganate solution in the presence of a nonionic surfactant by employing an acidic medium and using copper as a reducing agent. The method is simple in operation, and the obtained rough-surface microspherical manganese dioxide has relatively high ion transmission performance and is applicable as a supercapacitor material.

Description

The preparation of uneven surface microspheroidal Manganse Dioxide and the application in electrochemical capacitance
Technical field
The present invention relates to a kind of preparation method of ellipsoid shape mesoporous carbon, more particularly relating to a kind of ellipsoid shape mesoporous silicon oxide is hard mould agent, in its duct, insert grease, and carbonization is the method for corresponding pattern porous carbon under an inert atmosphere.
Background technology
Ordered mesopore carbon is novel non-silicon-based mesoporous material, have that pore passage structure is regular, high specific surface area, compared with large pore volume, narrower pore size distribution, the better feature such as chemistry and thermostability, make it in catalysis, separating-purifying, biomaterial and Novel assembling material etc., have huge applications potentiality, and carbon material is nontoxic and pollution-free, be novel environmental repair materials, particularly as the preparation field etc. of support of the catalyst to novel supported catalyst, there is better application prospect.
The preparation method of current known mesoporous carbon is: utilize nonionogenic tenside and the self-assembly of polymer presoma, in aqueous, under certain temperature, concentration and pH value, polymer presoma can around tensio-active agent further crosslinking polymerization, form the stable polymer-nonionogenic tenside matrix material with ordered mesostructure (two-dimentional six sides or three-dimensional cubic structure).To be extracted by solvent refluxing or under inert atmosphere, roasting can remove tensio-active agent wherein, obtain the mesoporous polymer material of high-sequential, bigger serface.Or by mesoporous polymer material further high temperature cabonization under an inert atmosphere, obtain the meso-porous carbon material of corresponding construction.Equally, polymer-nonionogenic tenside matrix material also can obtain meso-porous carbon material by direct carbonization.
Report is had for the preparation method of ellipsoid shape mesoporous carbon in document, but what prepare in known technology at present is smooth microballoon, and the present invention has the surface irregularity microballoon of surface irregularity, there is larger specific surface area, thus there is better electrochemical activity.
Summary of the invention
Be hard mould agent with axiolitic mesoporous silicon oxide, in mesopore orbit, insert liquid fat, carbonization in an inert atmosphere after oven dry, after removing silicon-dioxide, obtain axiolitic mesoporous carbon.Prepared uneven surface microspheroidal manganese bioxide material is through scanning electron microscope test, there is larger specific surface area, thus there is better electrochemical activity, in electro-chemical test, show good performance, be expected to obtain in super capacitor material field apply widely.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of ellipsoid shape mesoporous carbon of the present invention.By potassium permanganate solution under nonionogenic tenside exists, be prepared from by hydrothermal method by making reductive agent with copper in acidic medium.To achieve these goals, adopt following technical scheme to comprise the following steps:
1. the preparation of material: at the coarse microballoon of the surface irregularity of 5 microns sized by the product obtained;
2. the sign of material: carry out XRD to coarse microballoon and characterize, obtains the XRD figure spectrum of coarse microspheroidal Manganse Dioxide;
3. electro-chemical test: the chemical property of test uneven surface microballoon, arrives sample within the scope of 0.6V-0.4 relative to Hg/HgO electrode at potential windows with scanning constant speed, analyzes its electrochemical behavior.
The invention has the beneficial effects as follows:
The preparation method of a kind of uneven surface microspheroidal Manganse Dioxide of the present invention, owing to remaining duct shorter in mesoporous carbon, surface irregularity is comparatively coarse, thus has larger surface area, thus has good chemical property.Further, working method of the present invention is simple, with low cost, can repeat.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope image of uneven surface microspheroidal Manganse Dioxide.
Fig. 2 is the X-ray diffracting spectrum of uneven surface microspheroidal Manganse Dioxide.
Fig. 3 is the cyclic voltammetry curve figure of uneven surface microspheroidal Manganse Dioxide, test condition: by sample with scanning constant speed (A-5mv/s,
B-10mv/s, C-15mv/s, D-20mv/s) arrive 0.65V within the scope of relative to Hg/HgO electrode-0.4 at potential windows, the electrochemical behavior in 3M KOH ionogen electrolyte solution.
Embodiment
Below by way of specific embodiment, also the invention will be further described by reference to the accompanying drawings, but the present invention is not limited to following examples.
Described method if no special instructions, is ordinary method.Described material if no special instructions, all can be bought from open commercial sources and obtain.
Embodiment 1
1.58 grams of potassium permanganate are dissolved in 85 ml deionized water, then the vitriol oil of 2 milliliters is slowly added wherein, stir and add nonionogenic tenside F127 1.2 grams again after 15 minutes, continuing stirring added in above-mentioned mixing solutions by 0.64 gram of copper scale after 15 minutes, then 100 milliliters are transferred to in teflon-lined autoclave, sealing also leaves standstill 24 hours under 120 degree, naturally cooled to room temperature afterwards, filter, product deionized water is repeatedly washed neutrality.Lower dry 12 hours of vacuum drying oven 60 degree.

Claims (3)

1. the present invention relates to a kind of preparation method of ellipsoid shape mesoporous carbon, especially relating to a kind of ellipsoid shape mesoporous silicon oxide is hard mould agent, grease is inserted in its duct, carbonization is the method for corresponding pattern porous carbon under an inert atmosphere, it is characterized in that described ellipsoid shape mesoporous silicon oxide, its major axis is 0.45 ~ 4.0 micron, and minor axis is 0.3 ~ 0.8 micron, and ratio and the axial ratio of major axis and minor axis are 1.5 ~ 5.0.
2. the preparation method of described ellipsoid shape mesoporous carbon according to claim 1, it is characterized in that described hard mould agent--axiolitic mesoporous silica particles, its major axis is 1.3 microns, and minor axis is 0.61 micron, and ratio and the axial ratio of major axis and minor axis are 2.36.
3. the preparation method of described ellipsoid shape mesoporous carbon according to claim 1, it is characterized in that there is shorter duct in mesoporous carbon, surface irregularity is comparatively coarse.
CN201310528353.4A 2013-10-31 2013-10-31 Preparation of rough-surface microspherical manganese dioxide and application to supercapacitors Pending CN104591120A (en)

Priority Applications (1)

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CN201310528353.4A CN104591120A (en) 2013-10-31 2013-10-31 Preparation of rough-surface microspherical manganese dioxide and application to supercapacitors

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109579032A (en) * 2018-12-13 2019-04-05 重庆工商大学 A kind of method of the copper-based catalyst CO completely burned of bi-component

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372325A (en) * 2008-04-30 2009-02-25 中国科学院上海硅酸盐研究所 Carbon nitride polyporous material and use thereof for hydrogen storage
CN102765782A (en) * 2012-07-17 2012-11-07 上海大学 Method for preparing hierarchical porous carbon capacitive deionization electrode
CN103346303A (en) * 2013-06-19 2013-10-09 奇瑞汽车股份有限公司 Silicon-carbon composite material and preparation method thereof, and lithium ion battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372325A (en) * 2008-04-30 2009-02-25 中国科学院上海硅酸盐研究所 Carbon nitride polyporous material and use thereof for hydrogen storage
CN102765782A (en) * 2012-07-17 2012-11-07 上海大学 Method for preparing hierarchical porous carbon capacitive deionization electrode
CN103346303A (en) * 2013-06-19 2013-10-09 奇瑞汽车股份有限公司 Silicon-carbon composite material and preparation method thereof, and lithium ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴张雄: "新型碳基有序介孔碳材料的合成、功能化及性质与应用", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109579032A (en) * 2018-12-13 2019-04-05 重庆工商大学 A kind of method of the copper-based catalyst CO completely burned of bi-component

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Application publication date: 20150506