Abstract
The synthesis and characterization of twin monomers [Ti(OCH2-2-MeO-C6H4)4(HOCH2-2-MeO-C6H4)]2 (3) and [Al(OCH2-2-MeO-C6H4)3]4 (5) by reacting HOCH2-2-MeO-C6H4 (1) with Ti(OiPr)4 (2), or 1 with AlMe3 (4) is discussed. Single crystal X-ray structure analysis of 3 shows a dimeric structure with two alkoxide ligands bridging the titanium ions, while the others are terminal bonded. The respective phenolic resin / metal oxide hybrid materials HM_Ti and HM_Al were obtained in moderate (HM_Ti) to excellent (HM_Al) yields using typical base-catalyzed twin polymerization conditions (230 °C, 2 h). Nuclear magnetic resonance and infrared spectroscopy as well as scanning electron microscopy and scanning transmission electron microscopy combined with energ-dispersive X-ray spectroscopy proved the formation of inorganic–organic hybrid materials consisting of resin and MxOy materials (HM_Ti, TiO2; HM_Al, Al2O3) containing interpenetrating phase nano-domains with sizes of < 5 nm, as is charcteristic for twin polymerization processes. Oxidation of HM_Ti and HM_Al yielded the respective oxide materials Ox_Ti (TiO2) and Ox_Al (Al2O3), which possess low surface areas of ABET = 53 m2/g and 76 m2/g, respectively.
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