The intercalation of bicyclic and tricyclic carboxylates into layered double hydroxides

Journal Article · Wed Dec 15 00:00:00 EST 2010 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2010.09.036· OSTI ID:21504030

Khan, Aamir I ^[1]; Hu, Gang; Rees, Nicholas H ^[1]; O'Hare, Dermot ^[1]

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1. Chemistry Research Laboratory, Department of Chemistry, University of Oxford, Mansfield Road, Oxford OX1 3TA (United Kingdom)

Twenty-four nanocomposites built from layered double hydroxides and bicyclic and tricyclic carboxylates have been synthesised for the first time. Eight carboxylates were successfully intercalated into [LiAl{sub 2}(OH){sub 6}]Cl.yH{sub 2}O, [Ca{sub 2}Al(OH){sub 6}]NO{sub 3}.yH{sub 2}O, and [Mg{sub 2}Al(OH){sub 6}]NO{sub 3}.yH{sub 2}O, and the products fully characterised. Guest species incorporated include 1-adamantane carboxylate (1-AC) and 5-norbornene-2-endo-3-exo-dicarboxylate. In some cases, carbonate anions were co-intercalated with the organic guest, and in others poorly crystalline aluminium hydroxides formed as by-products. Sharper resonances were observed in the {sup 13}C solid-state NMR spectra of the 1-AC intercalates than in the spectrum of pure 1-AC, suggesting increased order in the arrangement of the cyclic cages in the intercalates. Where possible, time-resolved in situ X-ray diffraction was employed to study the nanoscopic steps involved in the intercalation reactions. These investigations showed that the reactions are one-step processes, proceeding directly to the fully exchanged intercalate with no intermediate phases. The intercalation processes were found to be nucleation controlled. -- Graphical abstract: Twenty-four novel nanocomposites built from layered double hydroxides and bicyclic and tricyclic carboxylates have been synthesised and fully characterised. In situ X-ray diffraction was used to study reaction mechanisms and kinetics. Display Omitted

• OSTI ID: 21504030
• Journal Information: Journal of Solid State Chemistry, Vol. 183, Issue 12; Other Information: DOI: 10.1016/j.jssc.2010.09.036; PII: S0022-4596(10)00435-4; Copyright (c) 2010 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ALUMINIUM COMPOUNDS
ALUMINIUM HYDROXIDES
BY-PRODUCTS
CALCIUM COMPOUNDS
CARBONATES
CLATHRATES
COMPOSITE MATERIALS
CYCLOALKANES
LITHIUM COMPOUNDS
MAGNESIUM COMPOUNDS
NANOSTRUCTURES
NITRATES
NMR SPECTRA
NUCLEATION
REACTION KINETICS
TIME RESOLUTION
X-RAY DIFFRACTION
ALKALI METAL COMPOUNDS
ALKALINE EARTH METAL COMPOUNDS
ALKANES
CARBON COMPOUNDS
COHERENT SCATTERING
DIFFRACTION
HYDROCARBONS
HYDROGEN COMPOUNDS
HYDROXIDES
KINETICS
MATERIALS
NITROGEN COMPOUNDS
ORGANIC COMPOUNDS
OXYGEN COMPOUNDS
RESOLUTION
SCATTERING
SPECTRA
TIMING PROPERTIES