In this study, a synthetic BaSO4·CaSO4 composite was prepared by co-precipitation technique, characterised and examined for REE sorption. The sorption parameters were; pH = 4, equilibrium time = 20 min, temperature = 303 K, and REE liquor volume to composite mass ratio of 0.2:1 L g−1. The sorption reaction was controlled by pseudo 2nd order kinetic mechanism and Langmuir adsorption isotherm with an adsorption capacity of 168.63 mg g−1. 90.14% of REE (III) was desorbed using 1 mol L−1 HNO3. The process was endothermic and spontaneous. Accordingly, 1:1 barite-gypsum (natural ingredient for BaSO4·CaSO4), with 136 mg g−1 loading capacity, was used for REEs extraction.