Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating
The reduction of nitroarenes to arylamines is a synthetically important transformation both in the laboratory and in industry. Herein, Palladium (Pd) nanoparticles were synthesized via incorporation with mesoporous fumed silica material by doping technique. Water was used as a solvent and the as-syn...
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MDPI AG
2023-02-01
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| Series: | Catalysts |
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| Online Access: | https://www.mdpi.com/2073-4344/13/2/445 |
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| author | Afaf Y. Khormi Badria M. Al-Shehri Fatimah A. M. Al-Zahrani Mohamed S. Hamdy Amr Fouda Mohamed R. Shaaban |
| author_facet | Afaf Y. Khormi Badria M. Al-Shehri Fatimah A. M. Al-Zahrani Mohamed S. Hamdy Amr Fouda Mohamed R. Shaaban |
| author_sort | Afaf Y. Khormi |
| collection | DOAJ |
| description | The reduction of nitroarenes to arylamines is a synthetically important transformation both in the laboratory and in industry. Herein, Palladium (Pd) nanoparticles were synthesized via incorporation with mesoporous fumed silica material by doping technique. Water was used as a solvent and the as-synthetized material was reduced by using NaBH<sub>4</sub> to ensure the total transformation of PdO into Pd nanoparticles. The synthesized sample was characterized by using inductively coupled plasma (ICP) elemental analysis, X-ray powder diffraction (XRD), N<sub>2</sub> sorption measurement, scanning electron microscope (SEM), energy-dispersive spectroscopy (EDX), and transmission electron microscopy (TEM). Data showed that the Pd nanoparticles were successfully synthesized and supported on the mesoporous silica with an average size in the ranges of 10–20 nm, with an irregular shape. The purity of the synthesized sample was confirmed by EDX analysis which exhibits the presence of Si, O, and Pd. The catalytic activity of the prepared sample was evaluated in the heterogeneous reduction of nitroarenes to aromatic amines. Reduction reaction was monitored by Shimadzu GC-17A gas chromatography (GC, Japan) equipped with flam ionization detector and RTX-5 column, 30 m × 0.25 mm, 1-μm film thickness. Helium was used as carrier gas at flow rate 0.6 mL/min. Interestingly, the green hydrogenation of nitroarenes to primary amine compounds was achieved in an aqueous solution with high efficiency and in a short time; moreover, the reusability of heterogeneous Pd-SiO<sub>2</sub> was performed for four repeated cycles with more than 88% of efficiency at the fourth run. Finally, the heterogeneity of catalysis with high reliability and eco-friendly processes is a super new trend of nitroarenes reduction in the industry and economic scales. |
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| issn | 2073-4344 |
| language | English |
| last_indexed | 2024-03-11T09:00:33Z |
| publishDate | 2023-02-01 |
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| record_format | Article |
| series | Catalysts |
| spelling | doaj.art-0c706bd7f0304524b6a6f3681c9572ef2023-11-16T19:43:17ZengMDPI AGCatalysts2073-43442023-02-0113244510.3390/catal13020445Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave HeatingAfaf Y. Khormi0Badria M. Al-Shehri1Fatimah A. M. Al-Zahrani2Mohamed S. Hamdy3Amr Fouda4Mohamed R. Shaaban5Chemistry Department, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi ArabiaChemistry Department, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi ArabiaChemistry Department, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi ArabiaChemistry Department, Faculty of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi ArabiaDepartment of Botany and Microbiology, Faculty of Science, Al-Azhar University, Nasr City, Cairo 11884, EgyptDepartment of Chemistry, Faculty of Science, Cairo University, Giza 12613, EgyptThe reduction of nitroarenes to arylamines is a synthetically important transformation both in the laboratory and in industry. Herein, Palladium (Pd) nanoparticles were synthesized via incorporation with mesoporous fumed silica material by doping technique. Water was used as a solvent and the as-synthetized material was reduced by using NaBH<sub>4</sub> to ensure the total transformation of PdO into Pd nanoparticles. The synthesized sample was characterized by using inductively coupled plasma (ICP) elemental analysis, X-ray powder diffraction (XRD), N<sub>2</sub> sorption measurement, scanning electron microscope (SEM), energy-dispersive spectroscopy (EDX), and transmission electron microscopy (TEM). Data showed that the Pd nanoparticles were successfully synthesized and supported on the mesoporous silica with an average size in the ranges of 10–20 nm, with an irregular shape. The purity of the synthesized sample was confirmed by EDX analysis which exhibits the presence of Si, O, and Pd. The catalytic activity of the prepared sample was evaluated in the heterogeneous reduction of nitroarenes to aromatic amines. Reduction reaction was monitored by Shimadzu GC-17A gas chromatography (GC, Japan) equipped with flam ionization detector and RTX-5 column, 30 m × 0.25 mm, 1-μm film thickness. Helium was used as carrier gas at flow rate 0.6 mL/min. Interestingly, the green hydrogenation of nitroarenes to primary amine compounds was achieved in an aqueous solution with high efficiency and in a short time; moreover, the reusability of heterogeneous Pd-SiO<sub>2</sub> was performed for four repeated cycles with more than 88% of efficiency at the fourth run. Finally, the heterogeneity of catalysis with high reliability and eco-friendly processes is a super new trend of nitroarenes reduction in the industry and economic scales.https://www.mdpi.com/2073-4344/13/2/445palladiumsilicaheterogeneouscatalysismicrowave |
| spellingShingle | Afaf Y. Khormi Badria M. Al-Shehri Fatimah A. M. Al-Zahrani Mohamed S. Hamdy Amr Fouda Mohamed R. Shaaban Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating Catalysts palladium silica heterogeneous catalysis microwave |
| title | Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating |
| title_full | Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating |
| title_fullStr | Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating |
| title_full_unstemmed | Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating |
| title_short | Palladium Nanoparticles Incorporated Fumed Silica as an Efficient Catalyst for Nitroarenes Reduction via Thermal and Microwave Heating |
| title_sort | palladium nanoparticles incorporated fumed silica as an efficient catalyst for nitroarenes reduction via thermal and microwave heating |
| topic | palladium silica heterogeneous catalysis microwave |
| url | https://www.mdpi.com/2073-4344/13/2/445 |
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