Mesoporous organosilicas with Pd(II) complexes in their framework

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• 作者：Noemi Linares^a ; Angel E. Sepú ; lveda^b ; Jesú ; s R. Berenguer^b ; ^{jesus.berenguer@unirioja.es} ; ; Elena Lalinde^b ; Javier Garcia-Martinez^a ; ^{j.garcia@ua.es} ;
• 关键词：Mesoporous organosilicas ; Hybrid materials ; Co-condensation ; Complexes immobilization
• 刊名：Microporous and Mesoporous Materials
• 出版年：2012
• 期刊代码：78_13871811
• 类别：ch
• 出版时间：1 August, 2012
• 卷：158
• 期：Complete
• 页码：300-308
• 文件大小：1130 K

摘要

Incorporation of various Pd(II) complexes into the framework of mesoporous organosilica materials has been achieved by co-condensation, using a facile solvent-free one-pot method. The synthesis of Pd(II) complexes using ligands with triethoxysilyl terminal groups allowed for their homogeneous in situ incorporation into the organosiliceous structure. Organic/inorganic precursor bis(triethoxysilyl)ethane was used both, as silica source and as solvent for the synthesis of the complexes, avoiding the use of any other organic co-solvent and making the synthesis more environmentally friendly. The mild synthetic conditions used such as neutral pH, room temperature and ethanol extraction of the surfactant, allowed for a cleaner route for the preparation of hybrid organic/inorganic mesoporous materials with Pd(II) complexes covalently bounded to the support. The chemical integrity of the metal complexes after the synthesis of the hybrid material, [trans-PdCl₂L₂] (L = 4-C₅H₄N-(CH₂)₂Si(OEt₃) and PPh₂(CH₂)₂Si(OEt)₃), was confirmed by several spectroscopic techniques. A systematic study of the role of the different parameters involved in the synthesis of these materials and their relation with the final morphology of the catalysts is herein described.