Hybrid mesoporous silica MCM-41 (O-MCM-41) was prepared using γ-aminopropyltriethoxysilane (APTES) as spacer, tetraethoxysilane as precursor and 2-acetylpyridine as organic moiety. The heterogeneous palladium catalys...Hybrid mesoporous silica MCM-41 (O-MCM-41) was prepared using γ-aminopropyltriethoxysilane (APTES) as spacer, tetraethoxysilane as precursor and 2-acetylpyridine as organic moiety. The heterogeneous palladium catalyst (PdCl2 / O-MCM-41) was then prepared by reaction of the hybrid MCM-41 with PdCl2(PhCN)2. The products were characterized by means of IR, XRD, XPS and N2 adsorption-desorption isotherms. The catalytic properties of the supported catalyst in the oxidative carbonylation of phenol to diphenyl carbonate (DPC) were investigated. The yield of DPC and turnover number (TON) reached 5.8% and 29 mol DPC·mol Pd-1, and Pd loss was only 2.7% at 110 °C, 4.4 MPa for catalytic reaction of 5 h with 4.2wt% Pd loading, and molar ratio of phenol to Pd being 1000 in the presence of Cu2O and terahydrofuran (THF).展开更多
文摘Hybrid mesoporous silica MCM-41 (O-MCM-41) was prepared using γ-aminopropyltriethoxysilane (APTES) as spacer, tetraethoxysilane as precursor and 2-acetylpyridine as organic moiety. The heterogeneous palladium catalyst (PdCl2 / O-MCM-41) was then prepared by reaction of the hybrid MCM-41 with PdCl2(PhCN)2. The products were characterized by means of IR, XRD, XPS and N2 adsorption-desorption isotherms. The catalytic properties of the supported catalyst in the oxidative carbonylation of phenol to diphenyl carbonate (DPC) were investigated. The yield of DPC and turnover number (TON) reached 5.8% and 29 mol DPC·mol Pd-1, and Pd loss was only 2.7% at 110 °C, 4.4 MPa for catalytic reaction of 5 h with 4.2wt% Pd loading, and molar ratio of phenol to Pd being 1000 in the presence of Cu2O and terahydrofuran (THF).