@hkhavasi

Synthesis, characterization and single crystal structure determination of aluminum alkoxydisilanolates: precursors for silica-alumina composite

, , , and . APPLIED ORGANOMETALLIC CHEMISTRY, 24 (6): 431-438 (June 2010)
DOI: {10.1002/aoc.1634}

Abstract

Several novel aluminum alkoxydisilanolate complexes were prepared by reaction of triphenylsilanol with aluminum 2-methoxyethoxide, aluminum 2-ethoxyethoxide, aluminum sec-butoxide and aluminum iso-propoxide. All new complexes, (Ph(3)SiO)(2)Al(OR)(2) where R = CH(2)CH(2)OCH(3) (1), CH(2)CH(2)OC(2)H(5) (2), CH(CH(3))CH(2)CH(3) (3) and CH(CH(3))(2) (4) were characterized by elemental analysis, mass spectrometry and infrared spectroscopy (IR), as well as (1)H, (13)C, (29)Si and (27)Al NMR spectroscopies. The solid-state structures of the representative compound 2 and 4 were also verified by single-crystal X-ray analyses. Complexes 2 and 4 are dimers having distorted trigonal bipyramidal and tetrahedral coordination at the aluminum center, respectively. The (27)Al NMR spectrum of compound 2 showed that the solid-state structure of the complex was not retained in solution, and tetracoordinated aluminum was found in solution in contrast to the pentacoordinated geometry in the solid state. The hydrothermal treatment of 1 and 4 at 200 degrees C and the subsequent calcination at 1000 degrees C resulted in the formation of alumina-silica composite (4SiO(2)center dot Al(2)O(3)) with gamma-alumina in the silica matrix. Copyright (C) 2010 John Wiley & Sons, Ltd.

Links and resources

Tags