LDH-phases become increasingly interesting due to their broad ability to
be able to incorporate many different cations and anions. The intercalation of methanesulfonate
and ethanesulfonate into a Li-LDH as well as the behavior of the interlayer
structure as a function of the temperature is presented. A hexagonal P63/m
[LiAl2(OH)6][Cl?1.5H2O] (Li-Al-Cl) precursor LDH was
synthesized by hydrothermal treating of a LiCl solution with γ-Al(OH)3. This precursor was
used to intercalate methanesulfonate (CH3O3S?)
and ethanesulfonate (C2H5O3S?)
through anion exchange by stirring Li-Al-Cl in a solution of the respective
organic Li-salt (90?C, 12 h). X-ray diffraction pattern showed an
increase of the interlayer space c' (d001) of Li-Al-methanesulfonate
(Li-Al-MS) with 1.2886 nm and Li-Al-ethanesulfonate (Li-Al-ES) with 1.3816 nm
compared to the precursor with 0.7630 nm. Further investigations with
Fourier-transform infrared spectroscopy and scanning electron microscopy
confirmed a complete anion exchange of the organic molecules with the precursor
Cl?. Both synthesized LDH compounds [LiAl2(OH)6]CH3SO3?nH2O
(n = 2.24-3.72 (Li-Al-MS) and [LiAl2(OH)6]C2H5SO3}?nH2O
(n = 1.5) (Li-Al-ES) showed a monomolecular interlayer structure with
additional interlayer water at room temperature. By increasing the temperature,
the interlayer water was removed and the interlayer space c' of Li-Al-MS decreased to 0.87735 nm (at 55?C).
Calculations showed that a slight displacement of the organic molecules is
necessary to achieve this interlayer space. Different behavior of Li-Al-ES
could be observed during thermal treatment. Two phases coexisted at 75?C - 85?C, one with a
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