Nesting doll-shaped manganese oxide nanocrystalline grain composite particle and preparation method thereof

A composite technology of manganese oxide and nanocrystals, applied in the direction of nanotechnology, manganese oxide/manganese hydroxide, etc., can solve the problems of increased removal steps, low specific surface area, cumbersome process, etc., and achieve reduced crystal nucleus concentration, high ratio Surface area, effect of improving dispersibility

Inactive Publication Date: 2012-06-13
HUBEI HENGHAO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patents CN1438181A and CN1513767A prepare nano-manganese dioxide based on surfactant control and microemulsion system respectively, but manganese dioxide particles have no mesoporous structure, and the surfactant used in the preparation process requires additional removal steps, which is cumbersome
Chinese patent CN1467159 discloses a porous manganese oxide nanosheet material and its preparation method, but still needs to use a large amount of long-chain alkyl quaternary ammonium salt surfactants, and has poor fluidity
Chinese patent CN101597085B discloses a preparation method of mesoporous manganese oxide nanoparticles and no surfactant, which has obvious mesoporous characteristics, but the specific surface area is low (less than 15m 2 / g), the chemical activity is only suitable for toluene combustion catalysis
The paper Science, 1997, 276, p926 used the soft template method to prepare micron-sized mesoporous manganese oxide, but the shape was irregular and there was no hollow structure inside, which resulted in poor fluidity and reduced activity, and also required additional removal of surfactants. complex
Dalian University of Technology's public master's thesis "Preparation and Electrochemical Properties of Manganese Dioxide Hollow Microspheres" (2010) Manganese dioxide hollow microspheres were prepared by decomposing manganese carbonate crystal particles by thermal oxidation. Although a hollow structure was obtained, there was no mesopore structure, and the reaction temperature is high (400°C) and the reaction time is long (4 hours)

Method used

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  • Nesting doll-shaped manganese oxide nanocrystalline grain composite particle and preparation method thereof
  • Nesting doll-shaped manganese oxide nanocrystalline grain composite particle and preparation method thereof
  • Nesting doll-shaped manganese oxide nanocrystalline grain composite particle and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dissolve 1 mole of anhydrous manganese sulfate in 800g of water, and 1.2 moles of ammonium bicarbonate in 800g of water; then simultaneously add the two liquids into a container with 120 rpm stirring and ultrasonic frequency of 40KHz, and the ultrasonic power is 100 watts / liter of reaction solution, precipitate reaction at normal temperature for 1 hour, separate the material and liquid, collect the solid material and dry it in the air to obtain a beige ultrafine powder; XRD test results show that the beige ultrafine powder is a composite of manganese carbonate nanocrystals Particles, the size of the nanocrystalline particles is about 12nm; SEM photos show that the obtained manganese carbonate nanocrystalline composite particles are particles with a narrow particle size distribution of 0.7-4 μm.

[0022] The obtained spherical manganese carbonate nanocrystalline composite particles were calcined in an air atmosphere at a temperature of 370° C. for 21 minutes to obtain a...

Embodiment 2

[0025] The manganese carbonate nanocrystalline composite particles prepared in Example 1 were calcined in an air atmosphere at a calcining temperature of 780° C. for 5 to 7 minutes to obtain a dark brown-red powder. SEM photos show that the obtained sample maintains a matryoshka-like structure and the particle size is basically unchanged, with irregular mesopores of about 5-30nm; XRD test results show that it is Mn 2 o 3 JCPDS#71-0636 and Mn 3 o 4 The mixture of JCPDS#80-0382, the BET specific surface area is 65m 2 / g, the fluidity angle of repose is 19°.

Embodiment 3

[0027] The manganese carbonate nanocrystalline composite particles prepared in Example 1 were calcined in an air atmosphere at a calcining temperature of 960° C. for 7 to 12 minutes to obtain a dark brown-red powder. The SEM photos show that the obtained sample maintains a matryoshka-like structure and the particle size is basically unchanged, with irregular mesopores of about 5-50 nm and a small amount of macropores of 70-120 nm; XRD test results show that it is Mn 3 o 4 JCPDS#80-0382 nanocrystalline, the grain size is about 45nm, and the BET specific surface area is 33m 2 / g, the fluidity angle of repose is

[0028] 22°.

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Abstract

The invention which belongs to the nanomaterial preparation field concretely relates to a nesting doll-shaped manganese oxide nanocrystalline grain composite particle and a preparation method thereof. The nesting doll-shaped manganese oxide nanocrystalline grain composite particle is characterized in that: the shape of the particle is spherical, the particle size is 0.7-7mum, and the BET specificsurface area is 20-310m<2>/g; and the structure of the particle has a shell-core nesting doll shape, the shell and the core are respectively composed of manganese oxide nanocrystalline grains, and surfaces of the shell and the core are full of mesopores. The nesting doll-shaped manganese oxide nanocrystalline grain composite particle has the advantages of spherical shape, controllable dimension, good fluidity, shell-core nesting doll-shaped structure, realization of a case that surfaces of the shell and the core are full of mesopores, large specific surface area, and no need of a surfactant, convenience and easy implementation, and low cost of the preparation process.

Description

technical field [0001] The invention relates to the field of preparation of nanometer materials, in particular to manganese oxide materials and preparation methods thereof. Background technique [0002] Manganese oxide is a key basic material in many technical fields such as organic pollutant treatment, supercapacitors, high-performance ferrite and electrode materials. Most of the currently reported literature and patents prepare manganese oxide into nanocrystalline or porous structures and their aggregates, in order to improve their reactivity, catalytic activity and fluidity. Chinese patents CN1438181A and CN1513767A prepare nano-manganese dioxide based on surfactant control and microemulsion system respectively, but the manganese dioxide particles have no mesoporous structure, and the surfactant used in the preparation process requires additional removal steps, which is cumbersome. Chinese patent CN1467159 discloses a porous manganese oxide nano-flake material and its p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02B82Y40/00
Inventor 王维吴建恒胡汉煌周光林
Owner HUBEI HENGHAO TECH
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