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https://doi.org/10.5562/cca3426

Multinuclear Magnetic Resonance Study on Aluminium Sec-butoxide Chelated with Ethyl Acetoacetate in Various Amounts

Stanislav Kurajica orcid.org/0000-0002-7066-1213 ; Univeristy of Zagreb, Faculty of Chemical Engineering and Technology, Marulićev trg 19, HR-10000 Zagreb, Croatia
Tatjana Gazivoda Kraljević ; Univeristy of Zagreb, Faculty of Chemical Engineering and Technology, Marulićev trg 19, HR-10000 Zagreb, Croatia
Gregor Mali orcid.org/0000-0002-9012-2495 ; National Institute of Chemistry, Hajdrihova 19, SI-1000 Ljubljana, Slovenia
Ivan Simčić ; Pliva Hrvatska d.o.o., Prilaz baruna Filipovića 25, HR-10000 Zagreb, Croatia
Vilko Mandić orcid.org/0000-0002-1036-0603 ; Univeristy of Zagreb, Faculty of Chemical Engineering and Technology, Marulićev trg 19, HR-10000 Zagreb, Croatia
Iva Minga ; Univeristy of Zagreb, Faculty of Chemical Engineering and Technology, Marulićev trg 19, HR-10000 Zagreb, Croatia

Sažetak

Reactive aluminum alkoxide (ASB, aluminium sec-butoxide) was chelated using β-diketone (EAA, ethyl acetoacetate) in order to gain control over rapid hydrolysis in the course of the sol-gel process. Derived chelates were analysed using several NMR spectroscopic techniques: one-dimensional 1H, 13C, 27Al NMR and two-dimensional COSY, HSQC and DOSY. The NMR analysis enabled identification of the formed chelate species, as well as determination of their quantitative relationships. Several complexation products were observed: tris-chelated monomer, Al(EAA)3, bis-chelated dimmer, Al2(OnBu)4(EAA) 2, tris-chelated dimmer, Al2(OnBu)3(EAA)3, tetra-chelated dimmer, Al2(OnBu)2(EAA)4, and monochelated trimer, Al3(OnBu)8(EAA). Of the formed oligomer compounds, this is the first evidence of Al2(OR)3L3 in any alkoxide and β-ketoester or β-diketone combination. Aluminium sec-butoxide and ethyl acetoacetate complexes Al2(OnBu)4(EAA) 2 and Al2(OnBu)2(EAA)4 were also observed for the first time. With the increase of the EAA/ASB ratio the coordination of aluminium shifts towards six, whereas above the EAA/ASB ratio of 2.5 solely six-coordinated aluminium exists.

This work is licensed under a Creative Commons Attribution 4.0 International License.

Ključne riječi

aluminium sec-butoxide; ethyl acetoacetate; NMR spectroscopy; sol-gel processes

Hrčak ID:

216310

URI

https://hrcak.srce.hr/216310

Datum izdavanja:

28.1.2019.

Posjeta: 1.817 *