Synthesis of some new sol-gel derived metal-organic compounds and their hydrolysis-condensation reactions

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 alkox ides with varying amounts of 2-methylbutanoic and 3-methylbutanoic acids, a nd c) hydrolysis of complexation products with varying amounts of water. All reactions were carried out at room temperature. The complex products we re [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 H-1 NMR, FT-IR, an d elemental analysis. While Ti(OEt)(4), [Ti(OEt)(3.2)(2- MBA)(0.8)], and [T i(OEt)(3.2)(3-MBA)(0.8)] were hydrolyzed with 1.30, 1.28, and 1.30 mol of w ater, 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. Thes e products were characterized by gas chromatography (GC), Karl-Fischer coul ometric titrations, and thermal analysis.