Synthesis of Some New Sol-Gel Derived Metal-Organic Compounds and Their Hydrolysis-Condensation Reactions

Abstract This work comprised the following parts: a) hydrolysis of Ti(OEt)4 and Zr(OPr)4 with different amounts of water, b) complexation of the same alkoxides with varying amounts of 2-methylbutanoic and 3-methylbutanoic acids, and c) hydrolysis of complexation products with varying amounts of water. All reactions were carried out at room temperature. The complex products were [Ti(OEt)3.2(2-MBA)0.8], [Ti(OEt)3.2(3-MBA)0.8], [Zr(OPr)2.5(2-MBA)1.5], and [Zr(OPr)3.3(3-MBA)0.7] (2-MBA: 2-methylbutanoate, 3-MBA: 3-methylbutanoate). The products were characterized by 1H NMR, FT-IR, and elemental analysis. While Ti(OEt)4, [Ti(OEt)3.2(2-MBA)0.8], and [Ti(OEt)3.2(3-MBA)0.8] were hydrolyzed with 1.30, 1.28, and 1.30 mol of water, Zr(OPr)4, [Zr(OPr)2.5(2-MBA)1.5], and [Zr(OPr)3.3(3-MBA)0.7] were hydrolyzed with 2.0, 0.96, and 1.10 mol of water, respectively. These products were characterized by gas chromatography (GC), Karl-Fischer coulometric titrations, and thermal analysis.