02438nas a2200241 4500008004100000022001400041245017000055210006900225260009500294300001200389490000800401520147800409653001401887653003201901653002101933653001301954100001901967700001301986700002201999700001702021700002802038856013002066 2005 eng d a0021-951700aFormation of nanosized zirconia-supported 12-tungstophosphoric acid in mesoporous silica SBA-15: a stable and versatile solid acid catalyst for benzylation of phenol0 aFormation of nanosized zirconiasupported 12tungstophosphoric aci a525 B ST, STE 1900, SAN DIEGO, CA 92101-4495 USAbACADEMIC PRESS INC ELSEVIER SCIENCEcOCT a341-3520 v2353 a
A nanosized zirconia-supported 12-tungstophosphoric acid (TPA) in SBA-15 composite was prepared by wet impregnation of TPA/ZrO2 nanoparticles inside the mesoporous channels of SBA-15. The resulting composite material was calcined at 1123 K and characterized by elemental analysis, powder X-ray diffraction, nitrogen adsorption isotherms, transmission electron microscopy (TEM), scanning electron microscopy (SEM), solid-state P-31 CP-MAS NMR, Si-29 MAS NMR, UV-vis diffuse reflectance spectra, FTIR, TPD of ammonia, FTIR pyridine adsorption, and thermogravimetric analysis (TG-DTG). The synthesized TPA/ZrO2/SBA-15 showed a well-ordered hexagonal inesoporous structure and mesoporous support SBA-15 stabilized ZrO2-t (tetragonal) phase with crystal size in the range of 3-4 nm. SBA-15 was a better support than MCM-41 and MCM-48 because it retained its mesostructure even after high TPA loading and high calcination temperatures. Mesoporous silica support plays an important role in stabilizing the catalytically active tetragonal phase of zirconia, which gave the most active catalysts. The catalysts were examined for their catalytic activities in the liquid phase benzylation of phenol with benzyl alcohol and the catalyst 15 wt% TPA/ 22.4 wt% ZrO2/SBA-15 calcined at 1123 K was found to have high acidity and to be 10 times more active than neat TPA/ZrO2 Under the reaction conditions studied in benzylation of phenol. (c) 2005 Elsevier Inc. All rights reserved.
10ananosized10aphenol benzylation reaction10aterragonal phase10aTPA/ZrO21 aSawant, D., P.1 aVinu, A.1 aJacob, Nalini, E.1 aLefebvre, F.1 aHalligudi, Shivappa, B. uhttp://library.ncl.res.in/content/formation-nanosized-zirconia-supported-12-tungstophosphoric-acid-mesoporous-silica-sba-15-0