CN102219263B - Method for preparing Gamma-MnOOH nanometer rod - Google Patents
Method for preparing Gamma-MnOOH nanometer rod Download PDFInfo
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- CN102219263B CN102219263B CN 201110131857 CN201110131857A CN102219263B CN 102219263 B CN102219263 B CN 102219263B CN 201110131857 CN201110131857 CN 201110131857 CN 201110131857 A CN201110131857 A CN 201110131857A CN 102219263 B CN102219263 B CN 102219263B
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- nanometer rod
- mnooh
- mnooh nanometer
- gamma
- mixing solutions
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Abstract
The invention discloses a method for preparing a Gamma-MnOOH nanometer rod, comprising the following steps: firstly, taking LiOH/H2O and Mn(CH3COO)2/4H2O according to the mole ratio of LiOH/H2O to Mn(CH3COO)2/4H2O being 0.2-1, and dissolving the LiOH/H2O and Mn(CH3COO)2/4H2O by deionized water to obtain mixed solution; and secondly, stirring the mixed solution in the first step for 10-36h, then obtaining solution containing brown sediment, filtering and drying the solution so as to obtain the Gamma-MnOOH nanometer rod. In the method, the Gamma-MnOOH nanometer rod is prepared under low temperature, has the advantages of simple process, low cost, short period, low energy consumption, no pollution and the like, and is suitable for industrial production; and the prepared Gamma-MnOOH nanometer rod is more uniform in size distribution and does not contain any impurity.
Description
Technical field
The present invention relates to the preparation field of metallic compound, be specifically related to the method for a kind of γ of preparation-MnOOH nanometer rod.
Background technology
The oxyhydroxide of manganese all has crucial application at aspects such as catalyzer, molecular sieve, IX, molecular adsorption, electrochemistry, biosensor, electrochromic display devices, and especially its catalytic performance receives extensive attention.In the compound of numerous manganese, γ-MnOOH has higher catalytic activity because of there is more active site on its surface; And in the γ-MnOOH of different-shape, the concern that monodimension nanometer material such as nanometer rod, nano wire etc. receive is more.This is because the electricity of monodimension nanometer material transports performance and becomes with the variation of its residing environment, adsorbent; The ratio of the surface-area of monodimension nanometer material and volume is very high, and has extremely strong surface effects and quantum effect, and is comparatively sensitive to the gas response; In addition, monodimension nanometer material has anisotropy, shows peculiar physics, chemical feature.Under many situation; The material of one dimension Nano structure is much more superior than other corresponding body phase materials, and the controlled one-dimensional nano structure material of size, composition and percent crystallinity has become the relation of research structure and performance and the system that haves a great attraction of related application.
In the prior art, preparation γ-MnOOH nanometer rod generally adopts hydrothermal method, as reduce potassium permanganate etc. with reductive agent; Disclose a kind of method of the MnOOH of preparation nanometer rod among the one Chinese patent application CN201010218620.4, it is with potassium permanganate and N, and dinethylformamide carries out solvent thermal reaction and obtains the MnOOH nanometer rod.Hydrothermal method γ-MnOOH nanometer rod preparation need be used reductive agent, and this makes and produce the impurity phase in the resultant, and some water-heat process often need add tensio-active agent to obtain one-dimentional structure, and this can introduce impurity equally, and the removing of impurity makes the preparation process complicated.In addition, water-heat process need need to increase extra heating unit in the temperature heating that is higher than more than 120 ℃.
Summary of the invention
The invention provides the method that a kind of low temperature prepares γ-MnOOH nanometer rod, do not need any tensio-active agent in this method, raw material can recycling, has that technology is simple, cost is low, the cycle is short, a less energy-consumption, advantage such as pollution-free, is fit to suitability for industrialized production.
A kind of method for preparing γ-MnOOH nanometer rod may further comprise the steps:
1) presses LiOHH
2O and Mn (CH
3COO)
24H
2The O mol ratio is 0.2～1 to get LiOHH
2O and Mn (CH
3COO)
24H
2O obtains mixing solutions with deionized water dissolving;
2) mixing solutions in the step 1) is stirred the solution that obtains containing brown precipitate after 10 hours～36 hours,, obtain γ-MnOOH nanometer rod through suction filtration and drying.
In order to reach better invention effect, preferably:
The concentration of described mixing solutions counts 1%～10% with the weight percent of manganese acetate.
Described exsiccant temperature is 40 ℃～70 ℃.
Described stirring can be adopted conventional whipping appts, considers preferred magnetic agitation from the angle of being convenient to operate.
The present invention has the following advantages:
1, the present invention need not heating in low temperature such as envrionment temperature (room temperature etc.) preparation γ-MnOOH nanometer rod down, has that technology is simple, cost is low, the cycle is short, a less energy-consumption, advantage such as pollution-free, suitable suitability for industrialized production.
2, the γ-MnOOH nanometer rod distribution of sizes of the present invention's preparation is more even, does not have any impurity.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of embodiment 1 gained γ-MnOOH nanometer rod.
Fig. 2 is the stereoscan photograph of embodiment 1 gained γ-MnOOH nanometer rod.
Embodiment
Embodiment 1
With LiOHH
2O and Mn (CH
3COO)
24H
2O presses LiOHH
2O and Mn (CH
3COO)
24H
2The O mol ratio is that 4:5 places beaker, and adds the proper amount of deionized water dissolving and obtain mixing solutions, and the concentration of mixing solutions counts 1% with the weight percent of manganese acetate.Above-mentioned mixing solutions magnetic agitation is obtained containing the solution of brown precipitate after 10 hours, the above-mentioned solution that contains brown precipitate is carried out abundant suction filtration, the solid product of suction filtration is obtained final product through baking oven after 40 ℃ of dryings.
Products therefrom is characterized through XRD, see Fig. 1, comparing with the standard diffraction spectra (PDF#88-0649) of γ-MnOOH shows: product is single-phase γ-MnOOH.To the scanning electron microscopic observation of product show final product be length at 1 micron～2 microns, diameter is at the club of 10 nanometers～50 nanometers, and even size distribution, sees Fig. 2.
Embodiment 2
With LiOHH
2O and Mn (CH
3COO)
24H
2O presses LiOHH
2O and Mn (CH
3COO)
24H
2O mol ratio 1:5 places beaker, and adds the proper amount of deionized water dissolving and obtain mixing solutions, and the concentration of mixing solutions counts 5% with the weight percent of manganese acetate.Above-mentioned mixing solutions magnetic agitation is obtained containing the solution of brown precipitate after 24 hours, contain sedimentary solution and carry out abundant suction filtration, the suction filtration product is obtained final product through baking oven after 60 ℃ of dryings above-mentioned.
Final product is shown through XRD product is single-phase γ-MnOOH.Scanning electron microscopic observation to final product shows, final product be length at 2 microns～3 microns, diameter is at the club of 20 nanometers～60 nanometers, and even size distribution.
Embodiment 3
With LiOHH
2O and Mn (CH
3COO)
24H
2O presses LiOHH
2O and Mn (CH
3COO)
24H
2O mol ratio 1:1 places beaker, and adds the proper amount of deionized water dissolving and obtain mixing solutions, and the concentration of mixing solutions counts 10% with the weight percent of manganese acetate.Above-mentioned mixing solutions magnetic agitation is obtained containing the solution of brown precipitate after 36 hours, contain sedimentary solution and carry out abundant suction filtration, the suction filtration product is obtained final product through baking oven after 70 ℃ of dryings above-mentioned.
Final product is shown through XRD product is single-phase γ-MnOOH.Scanning electron microscopic observation to final product shows, final product be length at 2 microns～3 microns, diameter is at the club of 20 nanometers～60 nanometers, and even size distribution.
Claims (3)
1. method for preparing γ-MnOOH nanometer rod may further comprise the steps:
1) presses LiOHH
2O and Mn (CH
3COO)
24H
2The O mol ratio is 0.2～1 to get LiOHH
2O and Mn (CH
3COO)
24H
2O obtains mixing solutions with deionized water dissolving;
2) mixing solutions in the step 1) is stirred the solution that obtains containing brown precipitate after 10 hours～36 hours,, obtain γ-MnOOH nanometer rod through suction filtration and drying.
2. the method for preparing γ-MnOOH nanometer rod according to claim 1 is characterized in that the concentration of described mixing solutions counts 1%～10% with the weight percent of manganese acetate.
3. the method for preparing γ-MnOOH nanometer rod according to claim 1 is characterized in that, described exsiccant temperature is 40 ℃～70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110131857 CN102219263B (en) | 2011-05-20 | 2011-05-20 | Method for preparing Gamma-MnOOH nanometer rod |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110131857 CN102219263B (en) | 2011-05-20 | 2011-05-20 | Method for preparing Gamma-MnOOH nanometer rod |
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|---|---|
| CN102219263A CN102219263A (en) | 2011-10-19 |
| CN102219263B true CN102219263B (en) | 2012-12-12 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103367737A (en) * | 2012-04-09 | 2013-10-23 | 江苏国泰锂宝新材料有限公司 | Preparation method of high-density lithium battery anode material spinel lithium manganate |
| CN103232070A (en) * | 2013-05-07 | 2013-08-07 | 许昌学院 | Method for preparing rod-like basic type manganese oxide nanometer material |
| CN103831096B (en) * | 2014-03-13 | 2015-12-30 | 重庆大学 | A kind of MnOOH nanometer rods denitrating catalyst and preparation method thereof |
| CN104386756B (en) * | 2014-10-20 | 2015-10-21 | 中国科学院海洋研究所 | A kind of analogue enztme material and Synthesis and applications |
| CN114853073A (en) * | 2022-05-30 | 2022-08-05 | 荆门市格林美新材料有限公司 | Preparation method of linear MnOOH, negative electrode material and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060333A (en) * | 2011-02-18 | 2011-05-18 | 中山火炬职业技术学院 | Method for preparing manganese oxide nano-material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060333A (en) * | 2011-02-18 | 2011-05-18 | 中山火炬职业技术学院 | Method for preparing manganese oxide nano-material |
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