CN106082345A - A kind of preparation method of nano-manganese dioxide line - Google Patents
A kind of preparation method of nano-manganese dioxide line Download PDFInfo
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- CN106082345A CN106082345A CN201610416592.4A CN201610416592A CN106082345A CN 106082345 A CN106082345 A CN 106082345A CN 201610416592 A CN201610416592 A CN 201610416592A CN 106082345 A CN106082345 A CN 106082345A
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- manganese dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses the preparation method of a kind of nano-manganese dioxide line, comprise the steps: that (1) adds the material containing manganese weighing, reactant and additive in beaker, be subsequently adding deionized water and stir；(2) solution stirring is proceeded to carry out in polytetrafluoroethylene (PTFE) reactor hydro-thermal reaction, control reaction temperature and time, then it is cooled to room temperature with furnace temperature, through washing, drying to nano-manganese dioxide line.The method that the preparation method of the present invention is simple and controllability forces standby nano-manganese dioxide line, the material of preparation can individually or compound other type of materials application is in aspects such as lithium ion battery, ultracapacitor, catalysis and environment absorption.
Description
Technical field
The present invention relates to manganese dioxide technical field, specifically, relate to the preparation method of a kind of nano-manganese dioxide line.
Background technology
Nano material has the performances such as special electricity, optics, magnetics and calorifics because of it, has attracted that scientific research personnel's is emerging
Interest, also becomes the focus of research at present.Generally nano material includes the patterns such as particle, line, pipe and piece, identical material
The performance being shown when having different patterns also can be variant, is also therefore current science for the control of material morphology
One importance work of research.
The oxide of manganese generally has manganese oxide (MnO), manganese sesquioxide managnic oxide (Mn2O3) mangano-manganic oxide (Mn3O4) and titanium dioxide
Manganese (MnO2).Manganese dioxide be a kind of in terms of electrochemistry, catalysis, environment and the energy all can widely used material, generally have
The pattern such as bar-shaped, graininess, sheet, flower-shaped and wire.Research with regard to the nano-manganese dioxide application of wire there has been
Report, generally can by its individually or and other type of Material cladding prepare electrode material (Su, the X. of ultracapacitor
H.; Yu, L.; et al. High-performance alpha-MnO2 nanowire electrode for
supercapacitors. Appl Energ, 2015,153,94-100), or be used as catalysis material (Liu, Y.; Xu,
J.et al. Rational design and in situ fabrication of MnO2@NiCo2O4 nanowire
arrays on Ni foam as high-performance monolith de-NOx catalysts. J Mater Chem A,2015,3,11543-11553), it is also possible to be used for magnetic aspect (Yang, J. B.; Zhou, X. D et al.
Growth and magnetic properties of MnO2-delta nanowire microspheres. Appl Phys
Lett, 2004,85,3160-3162.) and separate membrane material (the CN 201310069197.X, Ye Fei etc., adsorbing
Plant the preparation method of functionalization manganese dioxide nanowire membrane).Therefore, report a kind of method preparing nano-manganese dioxide line for
The further performance of research manganese dioxide has great importance.
The method preparing nano-manganese dioxide line reported for work at present has a lot, common are liquid-phase coprecipitation, electricity sinks
(CN 201010291242.2, Wang Xin etc., SWCN is that template prepares manganese dioxide for area method, thermal decomposition method, template
The method of nano wire) and hydro-thermal method etc., these methods all have deficiency in terms of controllability.
Content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, provide a kind of step simple, the strong nano-silica of controllability
Change the preparation method of manganese line.The technical solution used in the present invention:
The preparation method of a kind of nano-manganese dioxide line, comprises the steps:
(1) it by the material containing manganese weighing, reactant and additive in beaker, is subsequently adding deionized water and stirs；
(2) solution stirring is proceeded to carry out in polytetrafluoroethylene (PTFE) reactor hydro-thermal reaction, control reaction temperature and time,
It is cooled to room temperature with furnace temperature again, through washing, drying to manganese dioxide nanowire.
In above-mentioned preparation method, described material containing manganese includes potassium permanganate, manganese acetate, the one of manganese sulfate etc. or
Several mixture of person.
In above-mentioned preparation method, described reactant includes urea (Co (NH2)2), ammonium carbonate (NH4)2CO3, carbonic acid
Hydrogen ammonium (NH4HCO3), ammoniacal liquor (NH4H2Etc. O) one or several the mixture in.
In above-mentioned preparation method, described additive includes polyvinylpyrrolidone (PVP) or polyethylene glycol
(PEG).
In above-mentioned preparation method, described reaction temperature is 100 ~ 220 DEG C, and the reaction time is 5 ~ 40h.
Compared with prior art, there is advantages that the preparation method of the present invention is simple and controllability
By force, the material of preparation can individually or be combined other type of materials application in lithium ion battery, ultracapacitor, catalysis and ring
The aspects such as border absorption.
Brief description
The X-ray diffractogram (XRD) of Fig. 1 nano-manganese dioxide line；
The scanning electron microscope diagram (SEM) of Fig. 2 nano-manganese dioxide line；
The transmission electron microscope figure (TEM) of Fig. 3 nano-manganese dioxide line；
Detailed description of the invention
The present invention is explained further below in conjunction with specific embodiment, but invention is not done any type of limit by embodiment
Fixed.
Embodiment 1:
KMnO is weighed in beaker4Co (the NH of powder 1.58g and 2.43g2)2Powder, is subsequently adding 100ml deionized water, then will
It is put into and carries out 60min stirring on magnetic stirrer, and control rotating speed is 300rpm.The solution stirring is transferred to PTFE anti-
Answering in kettle, reactor being put in the reacting furnace that a temperature controllable raises, the temperature resetting constant temperature is 150 DEG C, the time
For 20h, programming rate is 3 DEG C/min, and question response is cooled to room temperature with furnace temperature after terminating and further takes out sample, is then passed through 6 times and goes
After ionized water and the washing of 2 ethanol again by it in vacuum drying chamber 65 DEG C of dryings within 24 hours, i.e. obtain nano-manganese dioxide line,
Carried out corresponding performance test (XRD, SEM, TEM test) again.Wherein Fig. 1 is the XRD of nano-manganese dioxide line；Fig. 2
It is the SEM figure of nano-manganese dioxide line；The TEM figure of Fig. 3 nano-manganese dioxide line.The result of three figures please be briefly described,
So that the effect of the present invention to be described.
Embodiment 2:
KMnO is weighed in beaker4Powder 1.58g and Mn (CH3COO)2Powder 1.73g, then weigh 2.43gCo (NH2)2Powder,
Being subsequently adding 120ml deionized water, then putting it into and carry out 80min stirring on magnetic stirrer, control rotating speed is 320rpm.Will
The solution stirring is transferred in PTFE reactor, and reactor is put in the reacting furnace that a temperature controllable raises, then
Setting the temperature of constant temperature as 180 DEG C, the time is 15h, and programming rate is 3 DEG C/min, and question response is cooled to room with furnace temperature after terminating
Temperature further takes out sample, is then passed through 65 DEG C of dryings 24 in vacuum drying chamber by it again after 6 deionized waters and 2 ethanol washings
Hour i.e. obtains the nano-manganese dioxide nano wire of preparation, then is carried out corresponding performance test (XRD, SEM, TEM test).
Effect is basically identical with embodiment 1.
Embodiment 3:
KMnO is weighed in beaker4Powder 1.58g and MnSO4Powder 1.51g, then weigh 2.37g NH4HCO3Powder and 300
PVP, be subsequently adding 120ml deionized water, then put it into and on magnetic stirrer, carry out about 60min stirring, control rotating speed is
350rpm.The solution stirring is transferred in PTFE reactor, reactor is put into the anti-of a temperature controllable rising
Answering in stove, the temperature resetting constant temperature is 150 DEG C, and the time is 20h, and programming rate is 3 DEG C/min, question response terminate after with furnace temperature
Be cooled to room temperature and further take out sample, be then passed through after 6 deionized waters and the washing of 2 ethanol again by it in vacuum drying chamber 65
DEG C drying i.e. obtains the nano-manganese dioxide nano wire of preparation for 24 hours, then carried out corresponding performance test (XRD, SEM,
TEM tests).Effect is basically identical with embodiment 1.
Claims (5)
1. the preparation method of a nano-manganese dioxide line, it is characterised in that comprise the steps:
(1) add the material containing manganese weighing, reactant and additive in beaker, be subsequently adding deionized water and stir；
(2) solution stirring is proceeded to carry out in polytetrafluoroethylene (PTFE) reactor hydro-thermal reaction, control reaction temperature and time,
It is cooled to room temperature with furnace temperature again, through washing, drying to nano-manganese dioxide line.
2. preparation method according to claim 1, it is characterised in that described material containing manganese be potassium permanganate, manganese acetate,
One or several mixture in manganese sulfate.
3. preparation method according to claim 1, it is characterised in that described reactant is urea, ammonium carbonate, bicarbonate
One or several mixture in ammonium, ammoniacal liquor.
4. preparation method according to claim 1, it is characterised in that described additive is polyvinylpyrrolidone or poly-
Ethylene glycol.
5. preparation method according to claim 1, it is characterised in that described reaction temperature is 100 ~ 220 DEG C, during reaction
Between be 5 ~ 40h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106992291A (en) * | 2017-04-19 | 2017-07-28 | 扬州大学 | Manganese dioxide modification core shell structure-hollow microporous carbon ball coats the preparation method of nanometer sulfur molecule |
| CN107935048A (en) * | 2018-01-22 | 2018-04-20 | 中北大学 | Porous MnO2The synthetic method of multilevel hierarchy |
| CN110327917A (en) * | 2019-08-08 | 2019-10-15 | 华北电力大学（保定） | The metal-doped manganese dioxide photochemical catalyst preparation method of Treatment of Coking Effluent |
| CN110482610A (en) * | 2019-08-05 | 2019-11-22 | 广东美的白色家电技术创新中心有限公司 | A kind of big table specific area α-MnO of high-purity2Hydrothermal synthesis method |
| CN111547710A (en) * | 2020-04-03 | 2020-08-18 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene-based composite material and preparation method and application thereof |
| CN113471627A (en) * | 2021-05-21 | 2021-10-01 | 惠州锂威新能源科技有限公司 | Modified diaphragm and preparation method and application thereof |
| CN114105205A (en) * | 2021-11-24 | 2022-03-01 | 山东大学 | Small-size manganese dioxide, synthetic method and application in anti-tumor product |
| CN114229903A (en) * | 2021-11-23 | 2022-03-25 | 湖北大学 | MnO (MnO)2Electrode material and preparation method and application thereof |
| CN114759194A (en) * | 2022-03-16 | 2022-07-15 | 东华大学 | Manganese-based ternary integrated dual-functional oxygen electrode and preparation method and application thereof |
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| CN102689929A (en) * | 2012-06-12 | 2012-09-26 | 东华大学 | Method for preparing ultralong MnO2 nanowire supercapacitor material |
| CN104773760A (en) * | 2015-04-14 | 2015-07-15 | 湖南有色金属研究院 | Preparation method and applications of nano-manganese oxide |
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| CN102689929A (en) * | 2012-06-12 | 2012-09-26 | 东华大学 | Method for preparing ultralong MnO2 nanowire supercapacitor material |
| CN104773760A (en) * | 2015-04-14 | 2015-07-15 | 湖南有色金属研究院 | Preparation method and applications of nano-manganese oxide |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106992291A (en) * | 2017-04-19 | 2017-07-28 | 扬州大学 | Manganese dioxide modification core shell structure-hollow microporous carbon ball coats the preparation method of nanometer sulfur molecule |
| CN107935048A (en) * | 2018-01-22 | 2018-04-20 | 中北大学 | Porous MnO2The synthetic method of multilevel hierarchy |
| CN110482610B (en) * | 2019-08-05 | 2022-03-15 | 广东美的白色家电技术创新中心有限公司 | High-purity alpha-MnO with large surface area2Hydrothermal synthesis method |
| CN110482610A (en) * | 2019-08-05 | 2019-11-22 | 广东美的白色家电技术创新中心有限公司 | A kind of big table specific area α-MnO of high-purity2Hydrothermal synthesis method |
| CN110327917A (en) * | 2019-08-08 | 2019-10-15 | 华北电力大学（保定） | The metal-doped manganese dioxide photochemical catalyst preparation method of Treatment of Coking Effluent |
| CN110327917B (en) * | 2019-08-08 | 2022-06-07 | 华北电力大学（保定） | Preparation method of metal-doped manganese dioxide photocatalyst for coking wastewater treatment |
| CN111547710B (en) * | 2020-04-03 | 2022-06-07 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene-based composite material and preparation method and application thereof |
| CN111547710A (en) * | 2020-04-03 | 2020-08-18 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene-based composite material and preparation method and application thereof |
| CN113471627A (en) * | 2021-05-21 | 2021-10-01 | 惠州锂威新能源科技有限公司 | Modified diaphragm and preparation method and application thereof |
| CN114229903A (en) * | 2021-11-23 | 2022-03-25 | 湖北大学 | MnO (MnO)2Electrode material and preparation method and application thereof |
| CN114229903B (en) * | 2021-11-23 | 2023-10-31 | 湖北大学 | MnO (MnO) 2 Electrode material, preparation method and application thereof |
| CN114105205A (en) * | 2021-11-24 | 2022-03-01 | 山东大学 | Small-size manganese dioxide, synthetic method and application in anti-tumor product |
| CN114759194A (en) * | 2022-03-16 | 2022-07-15 | 东华大学 | Manganese-based ternary integrated dual-functional oxygen electrode and preparation method and application thereof |
| CN114759194B (en) * | 2022-03-16 | 2024-01-30 | 东华大学 | Manganese-based ternary integrated difunctional oxygen electrode and preparation method and application thereof |
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