Hydrothermal Synthesis, Characterization and Catalytic Activities of a Keggin Structure of (4,4′-Bpyh2)3[pw12o40]2•3h2o and a Wells-Dawson Structure of (4,4′-Bpyh2)3(4,4′

Abstract

Two novel polyoxometalates composed of heteropolytungstates, (4,4 '-bpyH2)3[PW12O40]2 center dot 3H2O (1) and (4,4 '- bpyH2)3(4,4 '-bpyH)1.75[Cu(bpy)2]0.25[H2P2W18O62]2 (2) have been synthesized under hydrothermal conditions and characterized by single crystal X-ray diffraction and TGA methods. Compound 1 crystallizes in the cubic space group Ia-3with a = 25.9356(12) angstrom, b = 25.936(3) angstrom, c = 25.936(3) angstrom, alpha = 90.00, (3= 90.00, gamma= 90.00 and Z = 8, and compound 2 crystallizes in the triclinic space group P-1with a = 13.5194(17) angstrom, b = 22.400(3) angstrom, c = 27.374(4) angstrom, alpha = 79.833(3), (3= 77.439(3), gamma= 80.213(4) and Z = 2. In addition to structural characterization, the catalytic activities of 1 and 2 were determined in hydrolysis reactions. In the catalytic study, starch hydrolysis reactions were performed by using hydrothermal synthesis, and starch was hydrolyzed successfully at 150 degrees C, 5 h, based on the results of Lugol's test, which highest conversion yields above 90 wt.% under optimum reaction conditions. FT-IR analysis and catalyst reusability tests were also performed for each compound. No appreciable loss was observed in activity after five reaction cycles.