Bench-scale preparation of Cu3(BTC)2 by ethanol reflux: Synthesis optimization and adsorption/catalytic applications

A metal organic framework, Cu-3(BTC)(2) was prepared in a 1 L-capacity Pyrex reactor by ethanol reflux method. H3BTC (1,3,5-benzenetricarboxylic acid) ligand concentration of 1.01 M with Cu salt/H3BTC mole ratio of 9:5 led to a product with excellent textural properties (>1700 m(2)/g) in yield in the range of 40-76% - depending on the stirring rate - after 24 h synthesis. Structural integrity was maintained after pelletizing the powder with a PVA binder, but textural properties deteriorated to some extent. The Cu-3(BTC)(2) powder was highly hydrophilic and water-sorption capacity decreased after pelletization. CO2 adsorption using the ground/sieved Cu-3(BTC)(2) pellets produced an improved breakthrough pattern despite a small reduction in saturation capacity compared with that of the powders. Tetralin oxidation reaction was then carried out for the Cu-3(BTC)(2) powder catalysts using TBHP as an oxidant. Tetralin conversions for three repeated runs remained almost constant and the heterogeneity of the Cu-3(BTC)(2) catalyst in the liquid phase oxidation was examined by hot-filtering experiment. Due to increased pore diffusion resistance, the pellets and its ground/sieved form showed lower catalytic properties than did the powder form of Cu-3(BTC)(2). (C) 2012 Elsevier Inc. All rights reserved.