Phosphine free SBA-15-EDTA-Pd highly active recyclable catalyst: synthesis characterization and application for suzuki and sonogashira reaction
Title | Phosphine free SBA-15-EDTA-Pd highly active recyclable catalyst: synthesis characterization and application for suzuki and sonogashira reaction |
Publication Type | Journal Article |
Year of Publication | 2014 |
Authors | Sharma, P, Singh, AP |
Journal | Catalysis Science & Technology |
Volume | 4 |
Issue | 9 |
Pagination | 2978-2989 |
Date Published | AUG |
ISSN | 2044-4753 |
Abstract | Phosphine obstructed highly efficient and reusable SBA-15-EDTA-Pd(11) has been synthesized by anchoring a Pd-EDTA complex over the surface of organo-functionalized SBA-15. The physiochemical properties of the organo-functionalized catalyst were analyzed by elemental analysis, ICP-OES, XRD, N-2 sorption measurement isotherms, TGA and DTA, solid state C-13, Si-29 NMR spectroscopy FT-IR, XPS DRS UV-visible, SEM and TEM. The XRD and N-2 sorption analyses of the synthesized catalyst confirm that the ordered mesoporous channel structure was retained even after the multistep synthetic procedures. The (100), (110) and (200) reflections in SBA-15 provide a good structural stability, an the existence of a long range order and high pore wall thickness. The TGA-DTA results reveal that the thermal stability of the synthesized catalyst SBA-15-EDTA-Pd(11) was maintained at higher temperature. The organic moieties anchored over the surface of the SBA-15 and inside the pore wall were demonstrated by solid state C-13 NMR and FT-IR spectroscopy. Further, solid state Si-29 NMR spectroscopy provides information about the degree of functionalization of the surface silanol groups, of the SBA-15 with organic moieties. The electronic environment and oxidation state of the Pd metal in the SBA-15-EDTA-Pd(11) were monitored by XPS, and DRS UV-visible techniques. Moreover, the morphologies and topographic information of the synthesized catalyst were confirmed by SEM and TEM spectroscopy. The synthesized catalyst SBA-15-EDTA-Pd(11) was screened for the Suzuki and Sonogashira coupling reactions and shows a higher catalytic activity with higher TON (turn over number). The anchored solid catalyst can be recycled efficiently and reused five times, without a major loss in the reactivity. |
DOI | 10.1039/c4cy00144c |
Type of Journal (Indian or Foreign) | Foreign |
Impact Factor (IF) | 5.525 |