Abstract

Intercalation of a range of phosphonic acids into [LiAl2(OH)6]Cl·H2O at pH 8 leads to co-intercalation of both mono- and dianionic guest anions. Solid-state 31P NMR data can be used to show that these materials exhibit a 31P chemical shift that is intermediate between the values for the monoanionic and dianionic forms of the respective acids, suggesting that rapid proton exchange occurs between the intercalated anions. It is possible to calculate the relative amounts of mono- and dianionic species present using the observed averaged chemical shift of the intercalate phase. In the case of methylphosphonic acid, the ratio of mono- and dianionic species (MePO3H-/MePO32-) is estimated to be 2.1. The intercalation of methyl-, ethyl-, phenyl-, and benzylphosphonic acids into [LiAl2(OH)6]Cl·H2O was studied using time-resolved, in situ energy-dispersive synchrotron X-ray diffraction. The rates of intercalation are significantly greater for methylphosphonic acid (MPA), ethylphosphonic acid (EPA), and benzylphospho...

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