| Summary: | A new, double hydroxide based on Co and Fe was elaborated on by forced hydrolysis in a polyol medium. Complementary characterization techniques show that this new phase belongs to the layered double hydroxide family (LDH) with Co<sup>2+</sup> and Fe<sup>3+</sup> ions located in the octahedral sites of the bucite‑like structure. The acetate anions occupy interlayer space with an interlamellar distance of 12.70 Å. This large distance likely facilitates the exchange reaction. Acetates were exchanged by carbonates. The as‑obtained compound Co‑Fe‑Ac/<sub>Ex</sub> shows an interlamellar distance of 7.67 Å. The adsorption of direct red 2 by Co‑Fe‑Ac‑LDH has been examined in order to measure the capability of this new LDH to eliminate highly toxic azoic anionic dyes from waste water and was compared with that of Co‑Fe‑Ac/<sub>Ex</sub> and Co‑Fe‑CO<sub>3</sub>/<sub>A</sub> (synthesized in an aqueous medium). The adsorption capacity was found to depend on contact time, pH, initial dye concentration, and heating temperature. Concerning CoFeAc‑LDH, the dye uptake reaches a high level (588 mg/g) due to the occurrence of both adsorption processes: physisorption on the external surface and chemical sorption due to the intercalation of dye by exchange with an acetate anion. The study enables us to quantify the uptake amount of each effect in which the intercalation has the most important amount (418 mg/g).
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