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配合物[Mn(phen)2]2+修饰的MCM-41的合成与表征

郑珊; 高濂; 郭景坤   

  1. 中国科学院上海硅酸盐所高性能陶瓷与超微结构国家重点实验室, 上海 200050
  • 收稿日期:2000-05-10 修回日期:2000-06-02 出版日期:2001-05-20 网络出版日期:2001-05-20

Synthesis and Characterization of Manganese(II)-Phenanthroline Complex Functionalized MCM-41

ZHENG Shan; GAO Lian; GUO Jing-Kun   

  1. State Key Lab of High Performance Ceramics and Superfine Microstructure; Shanghai Institute of Ceramics; Chinese Academy of Sciences; Shanghai; 200050 China
  • Received:2000-05-10 Revised:2000-06-02 Published:2001-05-20 Online:2001-05-20

摘要: 分别以γ-氨丙基和甲基丙烯酸丙酯基修饰介孔分子筛MCM-41内孔壁,将引入的有机官能团与金属配位离子[Mn(phen)Cl]通过配位健成键首次合成了锰(Ⅱ)配位化合物修饰的MCM-41(MCM-ap-Mn(phen),MCM-mp-Mn(Phen)).通过XRD、FTIR、77K氮气吸附-脱附、UV-VIS漫反射光谱和Mn2+电子顺磁共振谱(ESR)表征了复合物MCM-ap-Mn(phen)和MCM-mp-Mn(phen)由于有机基团对MCM-41孔壁的修饰,使复合物的结晶度降低,增加的有机基因和配合物使红外光谱有所改变;BET比表面积,孔容和最可几孔径均下降;γ-氨丙基或甲基丙烯酸丙酯基与Mn2+的配位而使其UV-VIS漫反射吸收光谱在短波长的吸收加强;室温下 Mn2+电子顺磁共振表明 Mn(Ⅱ)配位环境几乎没有变化.

关键词: 介孔分子筛MCM-41, γ-氨丙基修饰的MCM-41, 甲基丙烯酸丙酯基修饰的MCM-41, 邻菲咯啉合锰(Ⅱ)修饰的MCM-41

Abstract: The preparation of manganese(II)-phenanthroline complex functionalized MCM-41 was described. The modification of the internal pore surface of mesoporous MCM-41
with 3-aminopropyl or 3-methacryloyloxypropyl and yielded two different functional groups by using 3-aminopropyltriethoxysilane and (3-methacryloyloxypropyl)trimethoxysilane
as the precursors. Manganese(II) phenanthroline complex was grafted onto the functional MCM-41 via the coordination of the metal ion with the functional group. The metal
ion complex functionalized mesoporous materials were characterized by XRD, FTIR, N2 adsorption/desorption at 77K, solid state diffuse reflectance UV-VIS spectroscopy
as well as electron spin resonance (ESR) at room temperature. After the functionalization, the vibrations such as υC=C, δCH2 from the organic ligands or Mn(II)
complex can be observed clearly. BET surface area, pore volume and most probably diameter decreased correspondingly according to the data of N2 sorption at 77K.
In UV-VIS spectra, the absorption at short wavelength was strengthened because of the introduced organic ligands. And the results of ESR suggested that Mn(II)
coordination in complexes didn’t change remarkably.

Key words: mesoporous MCM-41, 3-aminopropyl functional MCM-41, 3-methacryloyloxypropyl functional MCM-41, manganese(II)-phenanthroline complex functionalized MCM-41

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