This paper reports the synthesis of an Mg/Al double layered hydroxide (LDH) by coprecipitation, and of its dodecylsulphate (DS) and dodecylbenzenesulphonate (DBS) intercalates by rehydration. The resulting LDHs, also known as hydrotalcite-like compounds, were characterized by using various instrumental techniques including X-ray diffraction (XRD), IR spectroscopy and solid-state NMR spectroscopy. The solids obtained were tested as catalysts in the epoxidation of limonene with hydrogen peroxide. Because the presence of a nitrile was found to be indispensable for the reaction to develop to an acceptable extent, the influence of various nitriles on catalytic activity was examined. The epoxidation reaction yielded limonene oxide.