Publisher: Bachudo Science Co. Ltd

Hydrothermal Synthesis and Characterisation of Amine-Templated Metal Phosphate Framework

Joseph G. Atai, Samuel S. Etuk, Ayi A. Ayi
KEYWORDS: Hydrothermal synthesis, metal phosphates, p-aminobenzoic acid, ethylacetoacetate, ethylammonium-4-aminobenzoate.

ABSTRACT:

Two coordination polymers [CH 3CH 2NH 3]2M3(NH 3C6H4CO 2)2(HPO 4)4 (H 2O) 2 (M = Ni for compound I and M = Zn for compound II ) incorporating ethylammonium-4-aminobenzoate, were hydrothermally synthesized (autogeneous pressure for 5 days) at 105 0C. The Scanning Electron Micrographs revealed a greenish rectangular block for the Ni(II) complex and a colourless square plate for the Zn(II) complex. The complexes were characterised by IR-spectroscopy and the Infrared spectra of the two compounds exhibited similar essential features. The Spectra clearly showed the presence of co-ordinated water and terminal –NH3+. The broad band at 3914cm -1 (I) and 3926 – 3760cm -1 (II ) is due to the presence of water molecule in the structure. The bands at 3542 - 3401cm -1 (I) and 3434cm -1 are associated with stretching vibration of ν(-NH 2). The strong absorption bands at 1108 - 1014cm -1 (I) and 1108 – 1018cm -1 (II ) are associated with the asymmetric stretching vibration of ν(PO 4) groups, whereas those at 936 - 629cm -1 (I) and 934 – 718cm -1 (II ) correspond to its bending mode. The complexes were thermally stable up to 300 0C, after which the organic components starts decomposing. The solubility test in a wide spectrum of solvents (at room temperature) showed that the complexes were insoluble in water, ethanol, DMF and DMSO.


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