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Organic–Inorganic Hybrid Supermicroporous Iron(III) Phosphonate Nanoparticles as an Efficient Catalyst for the Synthesis of Biofuels
Author(s) -
Pramanik Malay,
Bhaumik Asim
Publication year - 2013
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.201300128
Subject(s) - phosphonate , thermogravimetric analysis , triclinic crystal system , catalysis , nuclear chemistry , materials science , hydrothermal synthesis , bet theory , chemistry , inorganic chemistry , crystal structure , crystallography , chemical engineering , organic chemistry , hydrothermal circulation , engineering
Here we report a novel family of crystalline, supermicroporous iron(III) phosphonate nanomaterials (HFeP‐1‐3, HFeP‐1‐2, and HFeP‐1‐4) with different Fe III ‐to‐organophosphonate ligand mole ratios. The materials were synthesized by using a hydrothermal reaction between benzene‐1,3,5‐triphosphonic acid and iron(III) chloride under acidic conditions (pH≈4.0). Powder X‐ray diffraction, N 2 sorption, transmission and scanning electron microscopy (TEM and SEM) image analysis, thermogravimetric and differential thermal analysis (TGA‐DTA), and FTIR spectroscopic tools were used to characterize the materials. The triclinic crystal phase [ P $\bar 1$ (2) space group] of the hybrid iron phosphonate was established by a Rietveld refinement of the PXRD analysis of HFeP‐1‐3 by using the MAUD program. The unit cell parameters are a =8.749(1), b =8.578(1), c =17.725(3) Å; α =104.47(3), β =97.64(1), γ =113.56(3)°; and V =1013.41 Å 3 . With these crystal parameters, we proposed an 24‐membered‐ring open framework structure for HFeP‐1. Compound HFeP‐1‐3, with an starting Fe/ligand molar ratio of 3.0, shows the highest Brunauer–Emmett–Telller (BET) surface area of 556 m 2 g −1 and uniform supermicropores of approximately 1.1 nm. The acidic surface of the porous iron(III) phosphonate nanoparticles was used in a highly efficient and recyclable catalytic transesterification reaction for the synthesis of biofuels under mild reaction conditions.