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Ammoniation of montmorillonites pillared with polyhydroxo-complexes of Al was performed in flow conditions at 773–1073 K and monitored by IR spectroscopy. Interaction of the clay with ammonia revealed exchange of terminal and bridging -OH groups by NH2-, NH- and N- species depending on the reaction temperature. Amination begins at 773 K while formation of NH groups starts at 873 K. Transformation of NH- into N-species occurs at 973 K. A mechanism for the ammoniation reaction is proposed and the series of the relative reactivity of OH groups was established: Si–OH > Mg–OH–Mg > Al–OH–Mg > Al–OH–Al. This series was rationalized in terms of accessibility of the OH groups.
Different types of heterogeneity were shown in F/OH/A1 pillared fluorohectorite by combined use of X-ray and selected area electron diffraction, high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray (EDX) methods: interlayer distances heterogeneity (layer stacking order imperfections); domain structure heterogeneity; and phase heterogeneity (formation of secondary phases from pillaring solutions). The role of ageing of pillaring solutions and pillared smectites was revealed and discussed.
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