A Zn/Al LDH with fluorescein intercalated as counterion with fluorescent properties was prepared. Fluorescein was prepared by the reaction between resorcinol and phthalic anhydride using the mixed oxide obtained after the thermal treatment of the LDH as catalyst. The material thus obtained, i.e. fluorescein adsorbed onto the mixed oxide from the calcined LDH, was treated with a mixture of water and pentanol in order to reconstitute the LDH and intercalate the fluorescein in the material. Three mixtures of water/pentanol with volume percent ratios of 100/0, 50/50, 20/80, were used to obtain the LDH with fluorescein intercalated. The best treatment could be determined according to the degree reconstruction and fluorescein intercalated into the LDH.