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Self‐Assembled Hybrid Molybdenum Phosphonate Porous Nanomaterials and Their Catalytic Activity for the Synthesis of Benzimidazoles
Author(s) -
Pramanik Malay,
Bhaumik Asim
Publication year - 2014
Publication title -
chemcatchem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.497
H-Index - 106
eISSN - 1867-3899
pISSN - 1867-3880
DOI - 10.1002/cctc.201402291
Subject(s) - materials science , chemical engineering , nanomaterials , magic angle spinning , molybdenum , hydrothermal synthesis , catalysis , thermogravimetric analysis , phosphonate , inorganic chemistry , chemistry , organic chemistry , nanotechnology , nuclear magnetic resonance spectroscopy , hydrothermal circulation , engineering
A new porous organic–inorganic hybrid molybdenum phosphonate nanomaterial (HMoP‐1) was synthesized through the reaction of benzene‐1,3,5‐triphosphonic acid and molybdenum(V) chloride under hydrothermal conditions in the absence of any structure‐directing agent. The morphology of the hybrid material was found to be different at different synthesis temperatures. The material synthesized at 423 K (HMoP‐1‐LT) has spherical particle morphology, and the material synthesized at 453 K (HMoP‐1‐HT) has self‐assembled flakelike morphology. Powder XRD, field‐emission SEM, high‐resolution TEM, N 2 sorption, solid‐state 13 C cross‐polarization magic‐angle spinning NMR and 31 P magic‐angle spinning NMR analyses, X‐ray photoelectron spectroscopy, thermogravimetric differential thermal analysis, NH 3 temperature‐programmed adsorption, and FTIR spectroscopic techniques were employed to characterize the samples and understand the morphological diversity. The orthorhombic crystal phase of the material was established through REFLEX and CELSIZ unit cell refinement programs. The calculated unit cell parameters of HMoP‐1‐HT are a =8.001(0.046) Å b =7.029 (0.039) Å, c =6.010 (0.036) Å; whereas HMoP‐1‐LT is amorphous in nature. HMoP‐1‐HT shows outstanding catalytic activity and high recycling efficiency for the green and efficient one‐pot condensation reaction for the synthesis of bioactive 2‐aryl benzimidazoles in excellent yields at room temperature.