Microwave synthesis of hybrid inorganic–organic materials including porous Cu3(BTC)2 from Cu(II)-trimesate mixture

Using a single, improved synthetic process, three different compounds comprising two known phases such as [Cu3(BTC)2(H2O)3] (1), [Cu2(OH)(BTC)(H2O)] · 2nH2O (2) and a new phase [Cu(BTC–H2)2-(H2O)2] · 3H2O (3) have been prepared by microwave-irradiation (MW) of identical reaction mixture of Cu(II) salt and trimesic acid, benzene-1,3,5-tricarboxylic acid (BTC–H3) at different temperatures. The microwave synthesis of (1) has been compared to its conventional hydrothermal synthesis. It has been found that by using MW synthesis (1) can be obtained in a much shorter synthesis time with improved yield and physical properties. The effect of other synthetic parameters such as solvent, concentration of reactant mixtures and reaction time on the product (1) has been also studied. At high temperature, the compound (2) was obtained in the same solution. The new phase (3) has been characterized by elemental analysis, thermogravimetric analysis, IR spectroscopy, scanning electron microscopy and powder XRD analysis.