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A method for preparing porous nano or submicron rod-shaped manganese oxide

A submicron rod and nanorod technology, which is applied in the field of preparation of porous nanorod manganese oxide, can solve the problem of no literature reports on the background technology of porous nanorod manganese oxide

Inactive Publication Date: 2011-11-30
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, there is no literature report on the background technology of the preparation of porous nanorod manganese oxide

Method used

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  • A method for preparing porous nano or submicron rod-shaped manganese oxide
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  • A method for preparing porous nano or submicron rod-shaped manganese oxide

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Embodiment 1

[0021] Under the condition of magnetic stirring, 1.25g KMnO 4 and 0.52g MnSO 4 ·H 2 O was dissolved in 80mL of deionized water, stirred for 20 minutes, added 3.17g of glucose, 1mL of ethylenediamine, stirred for 1h, then transferred to a 100mL stainless steel reactor lined with polytetrafluoroethylene (80% volume filling degree) ), then put it in a constant temperature box at 160°C for 12h, then cool it at room temperature, filter the obtained turbid solution, wash, dry (60°C, 12h), and grind it evenly to obtain the target product precursor, which is placed in a muffle furnace In the air atmosphere, the temperature was raised to 400°C at a rate of 1°C / min and kept at 400°C for 6 hours to obtain cubic bixbyite Mn 2 o 3 Black powder, particle shape is relatively uniform porous nano-rod shape, diameter is about 28nm, length is about 600-800nm, its XRD sees figure 1 (a), HRSEM photo see figure 2 (a), TEM photo see image 3 .

Embodiment 2

[0023] Under the condition of magnetic stirring, 1.50g KMnO 4 and 0.27g MnSO 4 ·H 2 O was dissolved in 80mL deionized water, and after stirring for 20 minutes, 1g of polyvinylpyrrolidone (PVP) was added, and after stirring for 1h, it was transferred to a 100mL stainless steel reactor lined with polytetrafluoroethylene (80% volume filling degree). ), then put it in a constant temperature box at 160°C for 24h, then cool it at room temperature, filter the obtained turbid solution, wash, dry (60°C, 12h), and grind it evenly to obtain the target product precursor, which is placed in a muffle furnace In the air atmosphere, the temperature was raised to 400°C at a rate of 1°C / min and kept at 400°C for 4 hours to obtain the tetragonal βMnO 2 Black powder, particle shape is submicron rod shape, diameter is about 400nm, length is about 6μm, its XRD sees figure 1 (b), HRSEM photo see figure 2 (b).

Embodiment 3

[0025] Under the condition of magnetic stirring, 0.64g KMnO 4Dissolve in 80mL deionized water, stir for 20 minutes, add 1.4mL HCl (mass fraction: 37%), 1mL ethylenediamine, after stirring for 1h, transfer it to a 100mL stainless steel reactor lined with polytetrafluoroethylene medium (80% volume filling degree), then put it in a constant temperature box at 120°C for 12h, then cool it at room temperature, filter the obtained turbid solution, wash, dry (60°C, 12h), and grind evenly to obtain the target product precursor placed in a muffle furnace, heated up to 500°C at a rate of 1°C / min in an air atmosphere and kept at 500°C for 4 hours to obtain spinel-type bixbyite Mn 2 o 3 Black powder, particle shape is submicron rod shape, diameter is about 150nm, length is about 1.5μm, its XRD sees figure 1 (c), HRSEM photo see figure 2 (c).

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Abstract

The invention discloses a method for preparing porous nano or submicron rod-like manganese oxide, and belongs to the technical field of functional materials. Ethanediamine, glucose or polyvinylpyrrolidone (PVP) is adopted as an additive, and the porous nano rod-like manganese oxide is prepared. The method mainly comprises the following steps of: dissolving KMnO4 and MnSO4 or KMnO4 and hydrochloric acid in deionized water in a certain molar ratio to obtain a homogeneous solution; adding the ethanediamine, glucose or PVP in a corresponding molar ratio; and fixing the volume of the solution by using deionized water, transferring to a self-pressure reactor, ensuring a liner filling rate is 80 percent, crystallizing at certain temperature for corresponding time, naturally cooling to room temperature, performing suction filtration on the obtained substance, drying at 60DEG C for 12 hours, fully grinding, heating from the room temperature to 400DEG C at a temperature rise rate of 1DEG C / min in the air, keeping the constant temperature for corresponding time to obtain the porous nano rod-like or submicron rod-like manganese oxide, wherein the obtained product contains a small amount of impurity phase.

Description

technical field [0001] The present invention relates to a preparation method of porous nano-rod-shaped manganese oxide, and specifically relates to the preparation of manganese oxide with rod-shaped morphology by using hydrothermal method, using ethylenediamine or PVP as a surfactant, and glucose or hydrochloric acid as an additive. In the technical field of functional materials, it has important applications in ion exchange, molecular adsorption, catalytic materials and electrochemical capacitors. Background technique [0002] In recent years, one-dimensional nanostructures such as nanowires, nanorods, and nanotubes have attracted widespread attention. One-dimensional nanostructured materials are widely used in fields such as conductive connections, nanoelectronics, optoelectronic materials, and functional sensing elements (G. Fasol, et al., Science, 1998, 280: 545-546). So far, a large number of literatures have reported the synthesis and characterization of many nanowire...

Claims

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Application Information

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IPC IPC(8): C01G45/02B82Y40/00
Inventor 戴洪兴王芳白广梅邓积光吉科猛刘雨溪高宝族
Owner BEIJING UNIV OF TECH
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