CN102001709B - Preparation method of basic manganese oxide nanorods - Google Patents
Preparation method of basic manganese oxide nanorods Download PDFInfo
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- CN102001709B CN102001709B CN201010603528XA CN201010603528A CN102001709B CN 102001709 B CN102001709 B CN 102001709B CN 201010603528X A CN201010603528X A CN 201010603528XA CN 201010603528 A CN201010603528 A CN 201010603528A CN 102001709 B CN102001709 B CN 102001709B
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Abstract
The invention discloses a preparation method of basic manganese oxide nanorods which are prepared by hydrothermally reacting potassium permanganate and polyvinyl pyrrolidone. The preparation method comprises the following steps: dissolving the polyvinyl pyrrolidone and the potassium permanganate in a weight ratio of 5:1 to 1:10 in water; hydrothermally reacting at the temperature of 100 DEG C-200DEG C for 2h-24h; then, carrying out solid-liquid separation on the product after reaction; sequentially washing the separated solid with distilled water, absolute ethyl alcohol or acetone; and finally drying the solid at the temperature of 30 DEG C-100 DEG C to obtain the basic manganese oxide nanorods. The method of the invention has no need of a template, high purity of products, even particlesize distribution, simple process, simple operation, mild condition, and no pollution, and is green and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of alkali formula manganese oxide nanometer rod.
Background technology
Alkali formula manganese oxide (MnOOH) is a kind of very important material, and it has crucial purposes in fields such as electrochemistry, battery, electrochromism.MnOOH can be used as the presoma of preparation Li-Mn-O spinel structure, Manganse Dioxide and other manganese and oxygen compound.Tradition upper body phase MnOOH generally can pass through electrochemical production.In recent years, also some bibliographical informations are arranged hydrothermal method, reverse micelle method prepare MnOOH.
Chinese patent document CN101428860A discloses a kind of method for preparing high purity MnOOH, and this method is hydrothermal method, and it is to use MnO
2And Mn
3O
4As the reaction precursor body, earlier with MnO
2And Mn
3O
4After the mixing, add entry, a ℃ following reaction promptly got in 0.5～60 hour in room temperature～100.The deficiency of this method is: MnO
2And Mn
3O
4Solubleness is smaller in water, and solid state reaction is not too even, sneaks into impurity in the product easily, and has used 2 kinds of manganese sources, and its product does not have specific pattern yet.
2004 the 62nd the 24th phases of volume of chemistry journal disclose the document of a piece " reverse micelle method preparation and sign of MnOOH nanometer rod ", and the method in the document is to adopt the aqueous solution/CTAB/ propyl carbinol/heptane four components to form reversed phase micelle system and MnCl
2Making diameter is the MnOOH nanometer rod that 10nm, length are about 200nm.The deficiency of this method is: need reversed phase micelle as template, and need to adopt tensio-active agent.
Chinese patent document CN101851008 A discloses a kind of method of the MnOOH of preparation nanometer rod, and it is with potassium permanganate and N, and dinethylformamide carries out solvent thermal reaction and obtains the MnOOH nanometer rod.The deficiency of this method is: used organic reagent N, dinethylformamide has pollution as solvent and reductive agent to environment.
Summary of the invention
The object of the present invention is to provide a kind of template that need not, product purity is high, size distribution is even, and technology is simple, and is easy and simple to handle, mild condition, and green non-pollution is suitable for the preparation method of the alkali formula manganese oxide nanometer rod of suitability for industrialized production.
The technical scheme that realizes the object of the invention is: a kind of preparation method of alkali formula manganese oxide nanometer rod, it is to carry out hydro-thermal reaction with potassium permanganate and Vinylpyrrolidone polymer to obtain alkali formula manganese oxide nanometer rod.
What have says so: according to 5: 1～1: 10 weight ratio Vinylpyrrolidone polymer and potassium permanganate are dissolved in the water; Under 100 ℃～200 ℃ temperature, carry out hydro-thermal reaction 2h～24h; Then reacted product is carried out solid-liquid separation; Solid after separating with zero(ppm) water, absolute ethyl alcohol or washing with acetone successively, drying solid obtains alkali formula manganese oxide nanometer rod under 30 ℃～100 ℃ temperature at last.
The temperature of above-mentioned hydro-thermal reaction is 140 ℃～160 ℃.
The temperature of above-mentioned drying solid is 50 ℃～90 ℃.
The K value of described Vinylpyrrolidone polymer is 15～90.
The positively effect that the present invention has: (1) method of the present invention does not need the effect of template, but directly carries out hydro-thermal reaction with potassium permanganate and Vinylpyrrolidone polymer, finally obtains the alkali formula manganese oxide nanometer rod that size distribution is even, purity is high.(2) method mild condition of the present invention does not adopt organic reagent, but adopt toxicity very low not only as reductive agent but also as the Vinylpyrrolidone polymer of tensio-active agent, green non-pollution belongs to green synthesis process.(3) technology of the present invention is simple, and is easy and simple to handle, is suitable for suitability for industrialized production.(4) the alkali formula manganese oxide that makes of the present invention is applied to fields such as catalysis, environmental improvement, electrode materials, capacitance material especially.
Embodiment
(embodiment 1)
Take by weighing the potassium permanganate of 0.2g; It is dissolved in the zero(ppm) water of 15mL; The powdered K value that under agitation condition, adds 0.4g is 30 Vinylpyrrolidone polymer, changes mixed solution over to hydrothermal reaction kettle then, in confined conditions; Make the temperature of reaction system rise to 160 ℃, under 160 ℃ temperature, carry out hydro-thermal reaction 16h through temperature controlling system control reaction system.This reaction also is a redox reaction, and principal product wherein is alkali formula manganese oxide (an alkali formula manganese oxide), and alkali formula manganese oxide is solid, and all the other products are dissolved in the liquid system.With the post reaction mixture naturally cooling; Carry out solid-liquid separation through the mode or the filtering mode of spinning then; Use zero(ppm) water and absolute ethanol washing solid more successively, the solid after vacuum-drying washing under 80 ℃ the temperature is 2～3 hours at last, and the air pressure in the loft drier is 0.01～0.03MPa; Obtaining diameter is 100nm～400nm, and length is 10 μ m～15 μ m alkali formula manganese oxide nanometer rod powders.
(embodiment 2～embodiment 5)
Each embodiment and embodiment 1 are basic identical, and difference is seen table 1.
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Vinylpyrrolidone polymer | 0.4g | 0.2g | 0.4g | 0.4g | 0.1g |
| Potassium permanganate | 0.2g | 0.2g | 0.2g | 0.2g | 0.2g |
| Temperature of reaction | 160℃ | 160℃ | 140℃ | 160℃ | 160℃ |
| Reaction times | 16h | 16h | 16h | 12h | 16h |
| Drying temperature | 80℃ | 60℃ | 70℃ | 90℃ | 50℃ |
Claims (3)
1. the preparation method of an alkali formula manganese oxide nanometer rod; It is characterized in that: Vinylpyrrolidone polymer and potassium permanganate are dissolved in the water according to 5: 1～1: 10 weight ratio; Under 100 ℃～200 ℃ temperature, carry out hydro-thermal reaction 2h～24h; Then reacted product is carried out solid-liquid separation, the solid after separating with zero(ppm) water, absolute ethyl alcohol or washing with acetone successively, drying solid obtains alkali formula manganese oxide nanometer rod under 30 ℃～100 ℃ temperature at last; The K value of described Vinylpyrrolidone polymer is 15～90.
2. the preparation method of alkali formula manganese oxide nanometer rod according to claim 1 is characterized in that: the temperature of hydro-thermal reaction is 140 ℃～160 ℃.
3. the preparation method of alkali formula manganese oxide nanometer rod according to claim 1 is characterized in that: the temperature of drying solid is 50 ℃～90 ℃.
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| CN106914234B (en) * | 2017-02-23 | 2020-11-06 | 广西大学 | 'Almond-shaped' Mn2O3Preparation method of/C particles |
| CN111187599B (en) * | 2020-02-25 | 2021-03-23 | 桂林电子科技大学 | Three-dimensional basic manganese oxide nanorod foam composite phase change material and preparation method and application thereof |
| CN114516660B (en) * | 2022-01-27 | 2023-09-08 | 淮北师范大学 | CTAB induced delta-MnO 2 Preparation method of nano-flower supercapacitor anode material, product and application thereof |
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| JP2006248857A (en) * | 2005-03-11 | 2006-09-21 | Tosoh Corp | METHOD OF MANUFACTURING beta-MnOOH |
| CN101851008B (en) * | 2010-07-06 | 2011-11-23 | 江苏技术师范学院 | Method for preparing MnOOH nano rods |
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Effective date of registration: 20130805 Address after: 226600 Nantong, Haian, east of the town of East China Sea Road (East), No. 18, No. Patentee after: Jiangsu Tianheng Nanometer Technology Co., Ltd. Patentee after: Jiangsu University of Technology Address before: 213000 Changzhou Province in the Clock Tower District, Jiangsu, Wu Road, No. 1801 Patentee before: Jiangsu Teachers University of Technology |