S. Sener et al., Synthesis of some new sol-gel derived metal-organic compounds and their hydrolysis-condensation reactions, B CHEM S J, 73(6), 2000, pp. 1419-1423
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.