CN102070196A - Method for preparing manganese dioxide nano rod at low temperature - Google Patents
Method for preparing manganese dioxide nano rod at low temperature Download PDFInfo
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- CN102070196A CN102070196A CN 201110021914 CN201110021914A CN102070196A CN 102070196 A CN102070196 A CN 102070196A CN 201110021914 CN201110021914 CN 201110021914 CN 201110021914 A CN201110021914 A CN 201110021914A CN 102070196 A CN102070196 A CN 102070196A
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- manganese dioxide
- nano rod
- dioxide nano
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Abstract
The invention relates to a method for preparing an inorganic material, in particular to a method for preparing a manganese dioxide (MnO2) nano rod. The method comprises the following steps of: mixing manganese chloride tetrahydrate and potassium permanganate uniformly, and dissolving the mixture into distilled water till full dissolution; adding HCl solution to react, putting the mixed reaction solution into a thermostatic water bath, preserving the heat for over 24 hours, and cooling to room temperature to obtain sediment; and finally, centrifugally cleaning the sediment for multiple times by using deionized water till the pH value is neutral, and drying the sediment at room temperature to obtain the high-purity manganese dioxide nano rod. The method has the advantages that: the reagents are commercial products, fussy preparation is not needed, the process is simple and easy to operate, the cost is low, and the prepared product has high purity and can be produced in large batch.
Description
Technical field
The present invention relates to the preparation method of inorganic materials, specifically be meant a kind of Manganse Dioxide (MnO
2) preparation method of nanometer rod.
Background technology
As everyone knows, Manganse Dioxide (MnO
2) be intermediate oxide highly stable under a kind of normal temperature.Manganse Dioxide is used for steel-making in a large number, and is used to make glass, pottery, enamel and drying battery.In recent years, discover that Manganse Dioxide has fabulous catalysis and electrochemical properties.Manganse Dioxide is widely used in toxic organic compound catalysis and electrical condenser process industry now.Because the manganese dioxide nano rod has higher specific surface area, more passage has better properties in its Application Areas.Be used to prepare MnO so far
2The method of nanometer rod mainly contains thermal decomposition method, Gu gas/reaction method, sol-gel method, hydrothermal synthesis method and electrochemical process.These methods need higher temperature, and the cost height, complex process.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, the method for preparing the manganese dioxide nano rod that temperature of reaction is low.The method for preparing the manganese dioxide nano rod of the present invention adopts the water bath with thermostatic control heating method, and step is as follows:
(1) earlier tetrahydrate manganese chloride and potassium permanganate are mixed, wherein tetrahydrate manganese chloride is 2～4: 1 with the mol ratio of mole potassium permanganate, is dissolved in the distilled water, until dissolving fully again; At this mixture being dissolved in the distilled water is that general dissolving gets final product,
(2) continuing under the condition of stirring, adding concentration is that the HCl solution of 1M (mol/L) reacts again, and adding the amount of HCl solution and the mole ratio of tetrahydrate manganese chloride and potassium permanganate mixture is 1～2: 1;
(3) at last mixed reaction solution is positioned in 50～90 ℃ the constant water bath box, insulation was cooled to room temperature again and gets throw out more than 24 hours;
(4) with deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains high-purity manganese dioxide nano rod.
As preferably, the temperature of constant water bath box is 60～80 ℃ in the above-mentioned method for preparing the manganese dioxide nano rod.
As preferably, reactant mixes reactant with ball mill before dissolving in water in the above-mentioned method for preparing the manganese dioxide nano rod.
For example: earlier with certain tetrahydrate manganese chloride (MnCl
24H
2O) and certain potassium permanganate (KMnO
4) mix after, be dissolved into again in 200 milliliters the distilled water.MnCl
24H
2O and KMnO
4Mol ratio be preparation according to the above ratio.In dissolution process, need to continue to stir the dissolution rate of accelerated reaction thing.Reactant fully after the dissolving, is continuing under the condition of stirring in water again, slowly adds 100 ml concns and be the speed of response that the HCl solution of 1M (mol/L) comes the accelerated reaction thing.At last mixing solutions is positioned in 50～90 ℃ the constant water bath box, is incubated after at least 24 hours, be cooled to room temperature.With deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains high-purity manganese dioxide nano rod.
Beneficial effect: in the preparation process of the present invention, agents useful for same is commerical prod, need not loaded down with trivial details preparation, and technology is simple to operation, and cost is low, and the product purity height that makes can be mass-produced.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of the manganese dioxide nano rod that makes with the inventive method;
Fig. 2 is manganese dioxide nano rod Electronic Speculum power spectrum (EDX) spectrogram that makes with the inventive method;
Fig. 3 is transmission electron microscope (TEM) photo of the manganese dioxide nano rod that makes with the inventive method;
Fig. 4 is high-resolution-ration transmission electric-lens (HRTEM) photo of the manganese dioxide nano rod that makes with the inventive method
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
With 0.06 mole of tetrahydrate manganese chloride (MnCl
24H
2O), 0.03 mole of potassium permanganate (KMnO
4) mix after, be dissolved into again in 200 milliliters the distilled water.In dissolution process, need to continue to stir the dissolution rate of accelerated reaction thing.Reactant fully after the dissolving, is continuing under the condition of stirring in water again, slowly adds 100 ml concns and be the speed of response that the HCl solution of 1M comes the accelerated reaction thing.At last mixing solutions is positioned in 60 ℃ the constant water bath box, is incubated after 36 hours, be cooled to room temperature.With deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains black powder shape product.The XRD diffraction spectrogram (shown in Figure 1) of sample confirms that product is the γ-MnO of rhombic system
2, the XRD figure spectrum of gained and the MnO of reference
2Standard diffraction card (14-644) conforms to.The EDX analysis revealed product of Fig. 2 is elementary composition by Mn and O.Wherein the atomic ratio of Mn and O is 1: 1.96, with the MnO of standard
2In Mn and the atomic ratio of O approaching.Wherein the C element derives from and makees the used conductive carbon adhesive tape of scanning electron microscope EDX analysis, and is irrelevant with sample composition.Sample observed under transmission electron microscope as Fig. 3 can find that sample is made up of a large amount of nanometer rod.What Fig. 4 showed is the high-resolution-ration transmission electric-lens photo of individual nanorod.This nanometer rod is that diameter is about 8 nanometers, and length is about 20 nanometers.In conjunction with Fig. 1, Fig. 2, Fig. 3 and Fig. 4, this product is defined as MnO
2Nanometer rod.
Embodiment 2
With 0.06 mole of tetrahydrate manganese chloride (MnCl
24H
2O), 0.02 mole of potassium permanganate (KMnO
4) mix after, be dissolved into again in 200 milliliters the distilled water.In dissolution process, need to continue to stir the dissolution rate of accelerated reaction thing.Reactant fully after the dissolving, is continuing under the condition of stirring in water again, slowly adds 100 ml concns and be the speed of response that the HCl solution of 1M comes the accelerated reaction thing.At last mixing solutions is positioned in 80 ℃ the constant water bath box, is incubated after 24 hours, be cooled to room temperature.With deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains black powder shape product.The pattern of product, structure etc. are all similar to embodiment 1.
Embodiment 3
With 0.06 mole of tetrahydrate manganese chloride (MnCl
24H
2O), 0.015 mole of potassium permanganate (KMnO
4) mix after, be dissolved into again in 200 milliliters the distilled water.In dissolution process, need to continue to stir the dissolution rate of accelerated reaction thing.Reactant fully after the dissolving, is continuing under the condition of stirring in water again, slowly adds 100 ml concns and be the speed of response that the HCl solution of 1M comes the accelerated reaction thing.At last mixing solutions is positioned in 70 ℃ the constant water bath box, is incubated after 36 hours, be cooled to room temperature.With deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains black powder shape product.The pattern of product, structure etc. are all similar to embodiment 1.
Embodiment 4
With 0.06 mole of tetrahydrate manganese chloride (MnCl
24H
2O), 0.02 mole of potassium permanganate (KMnO
4) mix after, be dissolved into again in 200 milliliters the distilled water.In dissolution process, need to continue to stir the dissolution rate of accelerated reaction thing.Reactant fully after the dissolving, is continuing under the condition of stirring in water again, slowly adds 100 ml concns and be the speed of response that the HCl solution of 1M comes the accelerated reaction thing.At last mixing solutions is positioned in 80 ℃ the constant water bath box, is incubated after 48 hours, be cooled to room temperature.With deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains black powder shape product.The pattern of product, structure etc. are all similar to embodiment 1.
Claims (3)
1. a low temperature prepares the method for manganese dioxide nano rod, it is characterized in that step is as follows:
(1) earlier tetrahydrate manganese chloride and potassium permanganate are mixed, wherein tetrahydrate manganese chloride is 2～4: 1 with the mol ratio of mole potassium permanganate, is dissolved in the distilled water, until dissolving fully again;
(2) continuing under the condition of stirring, adding concentration is that the HCl solution of 1M reacts again, and adding the amount of HCl solution and the mole ratio of tetrahydrate manganese chloride and potassium permanganate mixture is 1～2: 1;
(3) at last mixed reaction solution is positioned in 50～90 ℃ the constant water bath box, insulation was cooled to room temperature again and gets throw out more than 24 hours;
(4) with deionized water repeatedly eccentric cleaning throw out to pH value be neutral, drying at room temperature obtains high-purity manganese dioxide nano rod.
2. the method for preparing the manganese dioxide nano rod according to claim 1, the temperature that it is characterized in that constant water bath box is 60～80 ℃.
3. the method for preparing the manganese dioxide nano rod according to claim 1 is characterized in that reactant mixes reactant with ball mill before dissolving in water.
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| CN 201110021914 CN102070196A (en) | 2011-01-18 | 2011-01-18 | Method for preparing manganese dioxide nano rod at low temperature |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583561A (en) * | 2012-01-12 | 2012-07-18 | 大连民族学院 | Alpha-phase manganese dioxide nano-rod, and preparation method and application thereof |
| WO2013057535A1 (en) * | 2011-10-19 | 2013-04-25 | Indian Institute Of Technology Madras | Nanofluid coolant |
| CN108017091A (en) * | 2017-11-07 | 2018-05-11 | 深圳市晶特智造科技有限公司 | A kind of rod-like nano α-MnO2And its preparation method and application |
| CN109674670A (en) * | 2019-01-23 | 2019-04-26 | 复旦大学 | A kind of manganese oxide nanocluster and its preparation method and application |
| CN112266023A (en) * | 2020-11-17 | 2021-01-26 | 河南大学 | Manganese dioxide nanostructure with controllable morphology, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597086A (en) * | 2009-06-26 | 2009-12-09 | 海南大学 | Method for preparing nano manganese dioxide with different crystal forms in low-temperature acid solution |
-
2011
- 2011-01-18 CN CN 201110021914 patent/CN102070196A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597086A (en) * | 2009-06-26 | 2009-12-09 | 海南大学 | Method for preparing nano manganese dioxide with different crystal forms in low-temperature acid solution |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Alloys and Compounds》 20050304 Yong Chen et al. Preparation of single-crystal alpha-MnO2 nanorods and nanoneedles from aqueous solution 282-285 1-3 第397卷, 2 * |
| 《硅酸盐学报》 20050331 冯杨柳 等 无机盐水溶液反应合成MnO2纳米粉体及其电容特性 318-322 1-3 第33卷, 第3期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013057535A1 (en) * | 2011-10-19 | 2013-04-25 | Indian Institute Of Technology Madras | Nanofluid coolant |
| US9464220B2 (en) | 2011-10-19 | 2016-10-11 | Indian Institute Of Technology Madras | Nanofluid coolant |
| CN102583561A (en) * | 2012-01-12 | 2012-07-18 | 大连民族学院 | Alpha-phase manganese dioxide nano-rod, and preparation method and application thereof |
| CN108017091A (en) * | 2017-11-07 | 2018-05-11 | 深圳市晶特智造科技有限公司 | A kind of rod-like nano α-MnO2And its preparation method and application |
| CN109674670A (en) * | 2019-01-23 | 2019-04-26 | 复旦大学 | A kind of manganese oxide nanocluster and its preparation method and application |
| CN112266023A (en) * | 2020-11-17 | 2021-01-26 | 河南大学 | Manganese dioxide nanostructure with controllable morphology, preparation method and application thereof |
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Application publication date: 20110525 |