Intercalation of an oxalatooxoniobate complex into layered double hydroxide and layered zinc hydroxide nitrate

• Published in: Journal of colloid and interface science 2009-02, Vol.330 (2), p.352-358
• Main Authors: Arizaga, Gregorio Guadalupe Carbajal, Gardolinski, José Eduardo Ferreira da Costa, Schreiner, Wido Herwig, Wypych, Fernando
• Format: Article
• Language: English
• Subjects: Chemistry; Colloidal state and disperse state; Exact sciences and technology; General and physical chemistry; Intercalation; Layered double hydroxide; Layered hydroxide salt; Niobium complex; Surface physical chemistry; Zinc hydroxide nitrate
• ISSN: 0021-9797; 1095-7103
• DOI: 10.1016/j.jcis.2008.10.025

A Zn/Al layered double hydroxide with molar ratio of 3 was prepared by coprecipitation in alkaline pH and used as a matrix to intercalate the ionic complex diaquadioxalatooxoniobate(V) (DDON), derived from NH 4[NbO(C 2O 4) 2(H 2O) 2]⋅2H 2O. In a similar way, the layered zinc hydroxide nitrate, Zn 5(OH) 8(NO 3) 2⋅2H 2O, was synthesized, preexpanded with azelate ions ( −OOC(CH 2) 7COO −), and then intercalated with the niobium complex. For both layered matrices, the results from X-ray powder diffractometry, Fourier transform infrared spectroscopy, and thermal analysis (TG/s-DTA) indicate the presence of the oxalate ion. In addition, results from X-ray photoelectron and Raman spectroscopy indicate the presence of the niobium center bonded to oxygen atoms. Finally, diffuse reflectance UV–vis spectroscopy suggests that the niobium centers are coordinated to oxalate ions. This is the first report of the intercalation of niobium into a layered matrix. A Zn/Al layered double hydroxide and a zinc layered hydroxide nitrate were intercalated with the anionic complex diaquadioxalatooxoniobate(V) and the products characterized by different instrumental techniques.