Abstract
A new way of modifying aluminum sec-butoxide (Al(OBus)3) is proposed. This synthesis is carried out by reacting Al(OBus)3 dissolved in tetrahydrofuran with an unsaturated acid, viz. acrylic acid.
The structure evolution of Al(OBus)3 with increasing acrylic acid amounts is investigated by infrared, 1H NMR, 13 C NMR, and 27Al NMR spectroscopies and viscosity measurements. Information obtained suggests that the exchange reaction occurring between butoxy groups and acrylate ligands is stopped for an acid/alkoxide molar ratio within the range 1.6–1.7. This value leads us to assume that the dominant trimeric species of precursor is preserved after modification. Moreover, 27Al NMR analysis only reveals the presence of hexacoordinated Al sites in the structure of the modified Al(OBus)3.
Evidence of the acrylic acid reaction with sec-butanol released during the alkoxide modification is also proved by the infrared and 13 C NMR data. However the produced ester amount can be considered as negligible.
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Velez, K., Quinson, J. & Fenet, B. Modification Study of Aluminum sec-Butoxide by Acrylic Acid. Journal of Sol-Gel Science and Technology 16, 201–208 (1999). https://doi.org/10.1023/A:1008767218134
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DOI: https://doi.org/10.1023/A:1008767218134