Investigation of layered double hydroxides intercalated by oxomolybdenum catecholate complexes

Inorganic Chemistry
Bernardo MonteiroMartyn Pillinger

Abstract

Oxomolybdenum(VI) complexes of 3,4-dihydroxybenzoic acid (3,4-H 2dhb) have been incorporated into layered double hydroxides (LDHs) by treatment of the LDH-nitrate (Zn-Al, Mg-Al) or LDH-chloride (Li-Al) precursors with aqueous or water/ethanol solutions of the complex (NMe 4) 2[MoO 2(3,4-dhb) 2].2H 2O at 50 or 100 degrees C. The texture and chemical composition of the products were investigated by elemental analysis and scanning electron microscopy (SEM) with coupled energy dispersive spectroscopy (EDS). Microanalysis for N and EDS analysis for Cl showed that at least 90% of nitrate or chloride ions were replaced during the ion exchange reactions. The final Mo content in the materials varied between 6.5 and 11.6 wt %. Mo K-edge EXAFS analysis, supported by IR, Raman, UV-vis, and (13)C{ (1)H} CP/MAS NMR spectroscopic studies, showed the presence of cointercalated [MoO 2(3,4-dhb) 2] ( m- ) and [Mo 2O 5(3,4-dhb) 2] ( m- ) complexes in proportions that depend on the type of LDH support and the reaction conditions. The binuclear bis(catecholate) complex, with a Mo...Mo separation of 3.16 A, was the major species intercalated in the Zn-Al and Li-Al products prepared using only water as solvent. The X-ray powder diffraction (XRPD) patt...Continue Reading

References

Apr 18, 1973·Journal of the American Chemical Society·K Kustin, S T Liu
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Jan 1, 2004·Journal of Research of the National Institute of Standards and Technology·A N Fitch

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Citations

Mar 8, 2016·Chemical Communications : Chem Comm·Mingwan LiXue Duan

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