CO 3 2− -intercalated Cu–Al layered double hydroxide (CO 3 ·Cu–Al LDH) was calcined to yield Cu–Al oxide, and then ethylenediaminetetraacetate-intercalated Cu–Al LDH (edta·Cu–Al LDH) was prepared by reconstructing Cu–Al oxide in edta solution. Decomposition of CO 3 ·Cu–Al LDH occurred in four stages. The production of Cu–Al oxide was caused by the thermal decomposition of CO 3 ·Cu–Al LDH until the third stage. The first stage was the elimination of adsorbed surface water and interlayer water in CO 3 ·Cu–Al LDH. The second and third stages were the dehydroxylation of the brucite-like octahedral layers and the elimination of CO 3 2− intercalated in the interlayers. The edta·Cu–Al LDH was found to take up Y 3+ in aqueous solution. The uptake of Y 3+ was caused not only by the chelating function of Hedta 3− in the interlayer but also by the chemical behavior of Cu–Al LDH itself. The edta·Cu–Al LDH was found to selectively take up rare earth ions from a mixed solution. The degree of uptake was high, in the order Sc 3+ >Y 3+ >La 3+ for all time durations, which was attributable to differences among the stabilities of Sc(edta) − , Y(edta) − and La(edta) − .