1. Enhancement of nitrogen content in fullerene soot via radical decarboxylative coupling under catalytic and noncatalytic conditions.
- Author
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Hosseini, Fatemeh Sadat and Zamani, Mehdi
- Subjects
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TRANSITION metal catalysts , *FIELD emission electron microscopy , *FOURIER transform infrared spectroscopy , *COUPLING reactions (Chemistry) , *DIFFERENTIAL scanning calorimetry , *X-ray emission spectroscopy - Abstract
Herein, a fast and efficient method for enhancement of nitrogen content in fullerene soot up to 21.44 wt.% via catalytic and noncatalytic radical decarboxylative coupling reactions with 4-nitrobenzoic acid under mild microwave irradiation is developed. The experiments are performed in N-methyl-2-pyrrolidone (NMP) or NMP/H2O solution containing an oxidant among K2S2O8, (NH4)2S2O8, Oxone, KMnO4, MnO2, CrO3, K2Cr2O7, ceric ammonium nitrate (CAN) and 2,2,6,6-tetramethylpiperidinyloxy (TEMPO). The several unimetallic and bimetallic salts of Cu, Ag, Mn, Fe, Ni, Co, Pb, Cr, Pd, Cu/Pd, Ag/Cu, Ag/Pb, Ag/Pd, Cr/Ag and Cr/Pd are examined as catalysts. The morphological and textural features as well as thermal behavior of the prepared samples are studied by X-ray diffraction (XRD), scanning electron microscopy/energy-dispersive X-ray spectroscopy and elemental mapping (SEM/EDS-Map), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry analysis differential scanning calorimetry (TGA-DSC). XRD patterns for most samples show a predominantly amorphous structure. The highest nitrogen content belongs to the sample prepared by CrO3. The nitrogen content is enhanced by the presence of Ag and Pd salts. Using NMP/H2O as solvent provides higher performance than NMP for enhancement of nitrogen content. The enhancement of nitrogen content reflects the increase of NO2 groups in the texture of fullerene soot detecting by FT-IR and TGA-DSC. The heat released from thermal decomposition of the prepared samples increases when transition metal catalysts are used in the preparation procedure. [ABSTRACT FROM AUTHOR]
- Published
- 2025
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