Organo-bentonites were prepared using a bentonite and an aqueous cetyltrimethylammonium hydroxide solution. The ratio of the surfactant (in mmoles) to the cation exchange capacity varied from 0.5 to 20, with 20 being the highest ratio ever reported in the literature. At high surfactant to cation exchange capacity ratios, the interlayer spacing increased to 3.75 nm due to the formation of a paraffin-type bilayer of surfactant cations, which was shown to be mainly in gauche conformations using solid state 13C CP/NMR. When the exchange reaction was carried out in a methanol-water mixture, the expansion of the organo-bentonites depended on the concentration of methanol (% by volume). The decomposition temperatures of the organic cations depended on the basal spacing of the organo-bentonites, and in situ X-ray diffraction revealed that the basal spacing of our organo-bentonites was stable up to 210°C. Above this temperature, the basal spacing shrunk to 1.47 nm due to decomposition of the surfactants.

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