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New layered double hydroxides (LDHs) CoNiFe, ZnNiFe and CoZnFe with MII/MIII molar ratio of 3, with acetate ions in the interlayer region have been prepared by forced  hydrolysis in polyol medium.The physico-chemical properties of all products were characterized by the methods of powder X-ray Diffraction, Infrared Spectroscopy, UV-Spectroscopy, Elemental analysis, Thermal analysis, Transmission Electron Microscopy and Scanning Electron Microscopy.It was found that all compounds present the typical features of hydrotalcite-like structure and exhibit a turbostratic character.The insertion of acetate anions into LDHs was confirmed and the interlayer spacing values were respectively 12.47, 13.64 and 14.69 Å for CoNiFe, ZnNiFe and CoZnFe.We notice that there is a difference between the interlayer spacing for all synthesized phases with and without zinc. This can be explained by a structural modification on the level of the layers and/ or different arrangement from the inserted species (anions + water) in the interlayer space for zinc materials.57Fe Mössbauer spectrometry allows concluding the presence of Fe3+ cations which occupy octahedral sites and confirming the absence of Fe2+ in the as-prepared compounds.

New acetate-intercalated CoNiFe, ZnNiFe and CoZnFe layered double hydroxides: Synthesis by hydrolysis in polyol medium and characterization