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Molecular iodine was intercalated from nonaqueous solution into microsized ZnAl-layered double hydroxide (LDH) in the iodide form, generating the I(3)(-)/I(-) redox couple into the interlayer region. Chloroform, ethanol, acetonitrile, or diethyl ether were used as solvents to dissolve the molecular iodine. The intercalation compounds were characterized by thermogravimetric analysis, X-ray powder diffraction, UV-vis spectroscopy, and scanning and transmission electron microscopy. The stability of iodine-solvent adducts and the iodine concentration affected the LDH iodine loading, and samples with I(2)/I(-) molar ratio ranging from 0.14 to 0.82 were prepared. Nanosized, well dispersible LDH, synthesized by the urea method in water-ethylene glycol media, were also prepared and successfully functionalized with the I(3)(-)/I(-) redox couple applying the conditions optimized for the micrometric systems.
Bastianini et al. (Wed,) studied this question.
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