介孔MnO2 超结构的合成及其性能

摘要/Abstract

摘要： 为了研制高级氧化水处理中所需的高效稳定催化剂, 采用了一种节能环保、工艺简单、无需模板的界面合成法, 在H₂O/CH₂Cl₂ 界面上制备出了介孔MnO₂, 并探究了其热稳定性. 应用X 射线衍射仪、傅里叶红外光谱仪、扫描电子显微镜、透射电子显微镜、比表面积及孔隙度分析仪对制备的样品进行组分和形貌的分析. 结果表明: 制备的介孔MnO₂ 是由y-MnO₂ 和"e-MnO₂ 组成, 它是由中空的亚微米级的MnO₂ 刺球堆积排列而成, 平均孔径约为5.9 nm, 比表面积为322.5 m²/g, 孔容为0.451 cm³/g. 在热稳定性方面, 这种介孔MnO₂ 经过400 ^oC 以下的煅烧, 物相没有变化, 只有晶型转变, 仍保持刺球形貌; 经过500 C 煅烧后, MnO₂变成了纯相Mn₂O₃, 中空刺球结构发生坍塌. 此外, 对这种独特的介孔MnO₂ 超结构的生长机理进行了初步的探讨. 可见, 界面合成法可以制备出高比表面积的形貌奇特、结构稳定的介孔MnO₂.

关键词: H₂O/CH₂Cl₂界面, 超结构, 介孔MnO₂, 热稳定性, 生长机理

Abstract: Mesoporous manganese dioxide (MnO₂) has been synthesized successfully by means of a facile and environmental friendly method by virtue of a soft interface between CH₂Cl₂ and H₂O without templates. It’s thermostability has also been investigated. X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy analysis, scanning electron microscopy, transmission electron microscopy and an automatic surface area or pore size analyzer were applied to investigate the composition and microstructure of the as-synthesized MnO₂. As a result, the as-prepared MnO₂ was proven to be a mixture of e-MnO₂ and y-MnO₂ using X-ray diffraction techniques. The structure characterizations indicated a unique mesoporous structure of as-prepared MnO₂ composed of hollow MnO₂ sub-microspheres with thorns at surface. Nitrogen sorption analyses show that the as-synthesized MnO₂ has an adsorption average pore diameter of 5.9 nm, mesoporous volume of 0.451 cm³.g−1, and Brunauer Emmett Teller specific surface area of 322.5 m²/g. The as-synthesized MnO₂ which has undergone the heat treatment of temperature lower than 400 ^oC, appears crystal change without change of composition. It would keep the microstructure of hollow MnO₂ sub-microspheres. Howerver, heat treatment of 500 ^oC can turn the MnO₂ to pure Mn₂O₃ along with it’s microstructure’s collapse. Otherwise,the possible growth mechanism of mesoporous MnO₂ has been proposed. In brief, high surface area Mesoporous MnO₂ with a novel and stable superstructure has been obtained by the facile interfacial method.

Key words: growth mechanism, H2O/CH2Cl2 soft interface, mesoporous MnO2, superstructure, theromostability

中图分类号:

TQ 137

刘延雨, 王利军, 侯凌癸, 汪文峰, 陈志文. 介孔MnO₂ 超结构的合成及其性能[J]. 上海大学学报(自然科学版), 2013, 19(4): 405-410.

LIU Yan-yu, WANG Li-jun, HOU Ling-gui, WANG Wen-feng, CHEN Zhi-wen. Superstructures and Properties of Mesoporous MnO₂Synthesized by a Facile Interface Method[J]. Journal of Shanghai University（Natural Science Edition）, 2013, 19(4): 405-410.

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介孔MnO₂ 超结构的合成及其性能

Superstructures and Properties of Mesoporous MnO₂Synthesized by a Facile Interface Method

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