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Issue 32, 2007
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Staging during anion-exchange intercalation into [LiAl2(OH)6]Cl·yH2O: structural and mechanistic insights

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Abstract

A series of experiments has been performed to seek more insight into the staging process that occurs during anion-exchange intercalation of some organic carboxylates and phosphonates into the layered double hydroxide [LiAl2(OH)6]Cl·yH2O. High resolution transmission electron microscopy has been employed to gain additional insight into the second-stage intermediates, providing strong evidence that the Rüdorff model of staging is applicable. Small-angle X-ray scattering was used to study the very early stages of the intercalation of succinate into [LiAl2(OH)6]Cl·yH2O: it was observed that the only species present during the reaction were the host, a second-stage intermediate and the first-stage product. The influence of temperature and solvent on the reaction mechanism was investigated. Staging was observed only at low temperatures (T < 60 °C), and found to be confined largely to aqueous systems. Reactions performed in a 95 : 5 (v/v) mixture of water and a second non-aqueous solvent such as ethanol, acetone, THF or formamide proceeded via a second-stage intermediate, whereas for those undertaken in 50 : 50 (v/v) mixtures a direct transformation from host to product was usually observed.

Graphical abstract: Staging during anion-exchange intercalation into [LiAl2(OH)6]Cl·yH2O: structural and mechanistic insights

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Supplementary files

Article information


Submitted
16 Apr 2007
Accepted
24 May 2007
First published
05 Jul 2007

Dalton Trans., 2007, 3499-3506
Article type
Paper

Staging during anion-exchange intercalation into [LiAl2(OH)6]Cl·yH2O: structural and mechanistic insights

G. R. Williams, A. M. Fogg, J. Sloan, C. Taviot-Guého and D. O'Hare, Dalton Trans., 2007, 3499
DOI: 10.1039/B705753A

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