In order to synthesize nanocomposite hybrid material clay-calixarene by solid-solid reaction, calixarenic derivative (dicalixarenic amide derivative) has been synthesized, and the complexing properties have been studied. This calixarene has shown a high efficacity as a specific ionophore following the study of these complexing properties with respect to different metal cations with various toxicities. Results show a significant selectivity toward mercury. Natural Tunisian clay was purified and characterized by various methods such as X-ray diffraction, X-ray fluorescence, infrared spectroscopy, and transmission electron microscope. Intercalation of the calixarene in the interlayer space of the clay was confirmed by the increase of the basal space after reaction. Also, the comparison of the infrared spectra shows that the reaction has indeed taken place. Prepared nanocomposite has developed a high specific surface. This is the first synthesis of clay-calixarenic hybrid obtained by solid reaction, with the aim of respecting the environment as much as possible. Taking into account the calixarenic structure, it is assumed that the Ar-Cx hybrid is classed among the class I hybrids.