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Synthesis and Temperature‐Induced Morphological Control in a Hybrid Porous Iron–Phosphonate Nanomaterial and Its Excellent Catalytic Activity in the Synthesis of Benzimidazoles
Author(s) -
Dutta Arghya,
Mondal John,
Patra Astam K.,
Bhaumik Asim
Publication year - 2012
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201201350
Subject(s) - materials science , chemical engineering , phosphonate , catalysis , mesoporous material , nanomaterials , hydrothermal synthesis , morphology (biology) , phase (matter) , porosity , hybrid material , particle (ecology) , tetragonal crystal system , particle size , fourier transform infrared spectroscopy , hydrothermal circulation , chemistry , organic chemistry , nanotechnology , composite material , oceanography , biology , geology , engineering , genetics
A new organic–inorganic hybrid porous iron–phosphonate material, HPFP‐1, has been synthesized under hydrothermal conditions by using hexamethylenediamine‐ N , N , N ′, N ′‐tetrakis‐(methylphosphonic acid) (HDTMP) as the organophosphorus precursor. The morphology of this material was found to be different at three different temperatures. The material that was synthesized at 453 K showed a flake‐like particle morphology and the material was highly crystalline. Whereas, the materials that were synthesized at 443 K and 423 K were semi‐crystalline and showed rod‐like‐ and spherical morphological features, respectively. SEM and TEM were employed to understand this change in particle morphology depending on the reaction temperature. Powder XRD analysis suggested the formation of a new tetragonal phase in HPFP‐1 ( a =11.313, c =15.825 Å; V =2025.659 Å 3 ). N 2 ‐sorption analysis suggested the existence of supermicropores and interparticle mesopores in these materials. Elemental‐ and thermal analyses, as well as FTIR spectroscopy, were employed to verify the composition and framework bonding of the material. The HPFP‐1 material showed excellent catalytic activity for the synthesis of benzimidazole derivatives under mild liquid‐phase reaction conditions.