CN101805024A - Preparation method of manganese carbonate nanorod - Google Patents
Preparation method of manganese carbonate nanorod Download PDFInfo
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- CN101805024A CN101805024A CN 201010158824 CN201010158824A CN101805024A CN 101805024 A CN101805024 A CN 101805024A CN 201010158824 CN201010158824 CN 201010158824 CN 201010158824 A CN201010158824 A CN 201010158824A CN 101805024 A CN101805024 A CN 101805024A
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- manganese carbonate
- nanorod
- preparation
- potassium permanganate
- deionized water
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Abstract
The invention relates to a preparation method of a manganese carbonate nanorod, which belongs to the field of nanometer material preparation. The preparation method comprises the following main steps: dissolving manganese chloride and potassium permanganate into deonized water; adding a surfactant, hydrogen peroxide and lithium carbonate; transferring the mixture into a reaction kettle and carrying out a hydrothermal reaction at 180DEG C for 16-24h; and collecting, washing and drying precipitation to obtain a manganese carbonate monocrystal nanorod with regular appearance, the diameter of 50-100nm and the length of 1-2mu m. Mn2O3 and Mn3O4 obtained by carrying out heat treatment on the manganese carbonate nanorod can retain the original appearance and high purity of manganese carbonate and are widely applied to the fields of catalysis and magnetism as well as electrode materials of lithium ion batteries. The invention solves the problem of the manganese carbonate nanorod preparation and has the advantages of simple and feasible operation process, short reaction time, excellent repeatability, low cost and easy industrial implementation.
Description
Technical field
The invention belongs to field of nano material preparation, particularly a kind of preparation method of manganese carbonate nanorod.
Background technology
Nanosecond science and technology are that a coverage rate that grows up the nineties in 20th century is extremely wide, the scientific research and the industrial field of multidisciplinary intersection, it comprises physics, chemistry, biology, materialogy and electronics, comprises with the technological sciences of measuring, analyzing and research is served as theme.Nanoparticle is owing to have many unusual character different with bulk solid, demonstrated application potential widely at aspects such as material, information, the energy, environment, life, military affairs, manufacturings, become countries in the world and seize high-tech and the grand strategy field of global economic competition commanding elevation in this century.
Oxide compound (the Mn of manganese
2O
3, Mn
3O
4) be novel inorganic multifunctional material; on electronic industry; it is the important source material of producing the soft magnetic ferrite soft magnetic materials; on chemical industry; it is cheap eco-friendly catalyzer; can improve a lot of Activity of Chemical Reaction, and effectively reduce the discharging of nitrogen-containing oxide and carbon monoxide, play the effect of protection environment.Aspect new forms of energy, Mn
2O
3, Mn
3O
4Be preparation anode material for lithium-ion batteries LiMn
2O
4Important presoma, simultaneously, also can be directly as the negative material of lithium ion battery because its special status, the oxide compound of manganese enjoys people to pay close attention to.Nano level Mn
2O
3, Mn
3O
4Owing to have surface effects, small-size effect, quantum size effect and macro quanta tunnel effect, with the Mn of routine
2O
3, Mn
3O
4Compare, performance is more excellent.And Mn
2O
3And Mn
3O
4Usually by MnCO
3Obtain under the condition of high-temperature calcination, this method is convenient and swift, and pollution-free, the Mn of preparation
2O
3And Mn
3O
4Granular size remains unchanged substantially, can keep the original pattern of manganous carbonate, the purity height.So people are increasing to the demand of manganous carbonate especially nano level carbonic acid manganese.At present, the domestic mode of production is mainly carried out in the reactor that normal tape stirs by manganese salt and carbonate, and this reaction is rhythmic reaction, the quality product rather unstable, the big and skewness of the manganous carbonate particle that obtains, and long reaction time, required expense is higher.
Summary of the invention
The present invention has considered the problem that occurs in the prior art, and purpose is to provide the preparation method of nano level carbonic acid manganese, preparation pattern rule, the straight slick manganous carbonate monocrystal nano rod in surface.
For achieving the above object, the present invention adopts following technical scheme:
1) be that 1: 4 potassium permanganate and Manganous chloride tetrahydrate is dissolved in the deionized water with mol ratio, the concentration of potassium permanganate is 0.01～0.03mol/L, adds certain amount of surfactant, and the mass ratio of potassium permanganate and tensio-active agent is 1: 1～1.5.
2) the dropping massfraction is 30% hydrogen peroxide, and it is 0.8～1.2L that every mole of potassium permanganate needs the consumption of hydrogen peroxide.
3) Quilonum Retard is joined in the above-mentioned solution, the mol ratio of Quilonum Retard and potassium permanganate is 2～3: 1.
4) said mixture is joined in the autoclave of inner liner polytetrafluoroethylene, in 180 ℃ of constant temperature 16～24h.
5) cooled and filtered is used deionized water and absolute ethanol washing respectively, and the product drying is obtained manganese carbonate nanorod.
Described tensio-active agent is a kind of in polyvinylpyrrolidone, cetyl trimethylammonium bromide, the polyoxyethylene glycol-6000.
The invention solves the difficult problem of manganese carbonate nanorod preparation, operating procedure is simple, and the reaction times is short, good reproducibility, and cost is low, is easy to industrializing implementation.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the manganese carbonate nanorod of the embodiment of the invention 1 preparation, and wherein X-coordinate is diffraction angle (2 θ), unit for degree (°), ordinate zou is a diffracted intensity, unit is cps.
Fig. 3 is field emission scanning electron microscope (FESEM) photo of the manganese carbonate nanorod of the embodiment of the invention 1 preparation.
Fig. 4 is transmission electron microscope (TEM) photo of the manganese carbonate nanorod of the embodiment of the invention 1 preparation, and the upper right corner is selected area electron diffraction (SAED) style of single nanometer rod.
Embodiment
Present embodiment has provided detailed embodiment being to implement under the prerequisite with the technical solution of the present invention, but the invention is not restricted to these embodiment.
Embodiment 1:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, the product drying.By the XRD figure of Fig. 2 product as can be known, sample is a manganous carbonate, and purity is higher.Fig. 3,4 shows that the manganese carbonate nanorod diameter is 50～100nm, and length is 1～2 μ m, and the manganese carbonate nanorod that obtains is a monocrystalline.
Embodiment 2:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyoxyethylene glycol-6000,0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 3:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g cetyl trimethylammonium bromide, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 4:
0.25mmol potassium permanganate and 1mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.05g polyvinylpyrrolidone, 0.25ml 30%.After the 0.625mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 5:
0.75mmol potassium permanganate and 3mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.15g polyvinylpyrrolidone, 0.75ml 30%.After the 1.875mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 6:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.08g polyvinylpyrrolidone, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 7:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.12g polyvinylpyrrolidone, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 8:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.4ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 9:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.6ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 10:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.5ml 30%.After the 1mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 11:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.5ml 30%.After the 1.5mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 18h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 12:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 16h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Embodiment 13:
0.5mmol potassium permanganate and 2mmol Manganous chloride tetrahydrate are dissolved in the 25ml deionized water, add the hydrogen peroxide of 0.1g polyvinylpyrrolidone, 0.5ml 30%.After the 1.25mmol Quilonum Retard joined above-mentioned solution, mixture is changed in the autoclave of inner liner polytetrafluoroethylene, the reactor capacity is 30ml, in 180 ℃ of following constant temperature 24h.After the cooling, filter, use deionized water and absolute ethanol washing respectively, it is 50～100nm that the product drying is obtained diameter, and length is the manganese carbonate nanorod of 1～2 μ m, and manganese carbonate nanorod is a monocrystalline.
Claims (2)
1. the preparation method of a manganese carbonate nanorod is characterized in that, utilizes hydro-thermal reaction to prepare diameter at 50～100nm, and length is the manganese carbonate nanorod of 1～2 μ m, may further comprise the steps:
1) be that 1: 4 potassium permanganate and Manganous chloride tetrahydrate is dissolved in the deionized water with mol ratio, the concentration of potassium permanganate is 0.01～0.03mol/L, adds tensio-active agent, and the mass ratio of potassium permanganate and tensio-active agent is 1: 1～1.5;
2) the dropping massfraction is 30% hydrogen peroxide, and it is 0.8～1.2L that every mole of potassium permanganate needs the consumption of hydrogen peroxide;
3) add Quilonum Retard, the mol ratio of Quilonum Retard and potassium permanganate is 2～3: 1, obtains mixture;
4) said mixture is joined in the autoclave of inner liner polytetrafluoroethylene, in 180 ℃ of constant temperature 16～24h.
5) after the cooling, filter, use deionized water and absolute ethanol washing respectively, will obtain manganese carbonate nanorod after the product drying.
2. according to the preparation method of the described a kind of manganese carbonate nanorod of claim 1, it is characterized in that: used tensio-active agent is a kind of in polyvinylpyrrolidone, cetyl trimethylammonium bromide and the polyoxyethylene glycol-6000.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102456479A (en) * | 2010-10-18 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method for electrode material of super capacitor, application and super capacitor |
| CN103991907A (en) * | 2014-05-08 | 2014-08-20 | 洛阳理工学院 | Preparation method for manganese carbonate nano-fiber ball |
| CN109437309A (en) * | 2018-11-26 | 2019-03-08 | 郝新丽 | A kind of synthetic method of shuttle-type structure manganese carbonate nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080219911A1 (en) * | 2005-03-30 | 2008-09-11 | Yang Kook Sun | Process Of Precipitation for Spheric Manganese Carbonate and the Products Produced Thereby |
| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
| CN101585554A (en) * | 2009-07-06 | 2009-11-25 | 中国科学院广州化学研究所 | Method for preparing manganous carbonate by using waste slag and waste water containing manganese as raw materials |
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2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080219911A1 (en) * | 2005-03-30 | 2008-09-11 | Yang Kook Sun | Process Of Precipitation for Spheric Manganese Carbonate and the Products Produced Thereby |
| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
| CN101585554A (en) * | 2009-07-06 | 2009-11-25 | 中国科学院广州化学研究所 | Method for preparing manganous carbonate by using waste slag and waste water containing manganese as raw materials |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102456479A (en) * | 2010-10-18 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method for electrode material of super capacitor, application and super capacitor |
| CN103991907A (en) * | 2014-05-08 | 2014-08-20 | 洛阳理工学院 | Preparation method for manganese carbonate nano-fiber ball |
| CN103991907B (en) * | 2014-05-08 | 2015-08-19 | 洛阳理工学院 | A kind of preparation method of manganous carbonate nanofiber ball |
| CN109437309A (en) * | 2018-11-26 | 2019-03-08 | 郝新丽 | A kind of synthetic method of shuttle-type structure manganese carbonate nano material |
| CN109437309B (en) * | 2018-11-26 | 2021-04-30 | 河北地质大学 | Synthetic method of shuttle-shaped structure manganese carbonate nano material |
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| CN101805024B (en) | 2012-03-07 |
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