W.N.P. van der Graaff, G. Li, B. Mezari, E.A. Pidko, E.J.M. Hensen
“Synthesis of Sn-Beta with Exclusive and High Framework Sn Content”, ChemCatChem 2015, DOI:10.1002/cctc.201403050 (TU/e)
Sn-Beta zeolite was prepared by acid dealumination of Beta zeolite, followed by dehydration and impregnation with anhydrous SnCl4. The formation of extraframework Sn (EFSn) species was prevented by the removal of unreacted SnCl4 in a methanol washing step prior to calcination. The resulting Sn-Beta zeolites were characterized by X-ray diffraction, Ar physisorption, NMR, UV/Vis, and FTIR spectroscopy. These well-defined Lewis acid zeolites exhibit good catalytic activity and selectivity in the conversion of 1,3-dihydroxyacetone to methyl lactate. Their performance is similar to a reference Sn-Beta zeolite prepared by hydrothermal synthesis. Sn-BEA zeolites that contain EFSn species exhibit lower catalytic activity; the EFSn species also catalyze formation of byproducts. DFT calculations show that partially hydrolyzed framework Sn-OH species (open sites), rather than the tetrahedral framework Sn sites (closed sites), are the most likely candidate active sites for methyl lactate formation.