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

A metal organic framework, Cu3(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 m2/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 Cu3(BTC)2 powder was highly hydrophilic and water-sorption capacity decreased after pelletization. CO2 adsorption using the ground/sieved Cu3(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 Cu3(BTC)2 powder catalysts using TBHP as an oxidant. Tetralin conversions for three repeated runs remained almost constant and the heterogeneity of the Cu3(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 Cu3(BTC)2.

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► Cu3(BTC)2 synthesis in a 1 L-capacity reactor by ethanol reflux method is optimized.
► Cu3(BTC)2 pellets were obtained using PVA binder and with compression only.
► Water and CO2 sorption property of the prepared Cu3(BTC)2 samples were studied.
► Cu3(BTC)2 samples were tested as a catalyst for liquid phase tetralin oxidation.