AbstractBackgroundMetal−organic frameworks (MOFs) are energy‐efficient adsorbents for separating industrial chemical feedstocks. A type of MOF containing an extended porous network of γ‐cyclodextrin (γ‐CD) and alkali metal salts, CD‐MOF, has potential applications in adsorption separation processes in the petrochemical industry. This study aims to present the adsorption efficiency of CD‐MOF‐1 in separating xylene regioisomers.ResultsThe adsorption separation of xylene regioisomers on layered CD‐MOF‐1 microcrystals was studied using batch vapor‐phase adsorption and liquid‐phase breakthrough adsorption. CD‐MOF‐1 showed preferable adsorption of o‐xylene over the other two isomers, with adsorption strength in the order o‐xylene (oX) > m‐xylene (mX) > p‐xylene (pX). With increased temperature, high adsorption capacities of oX and mX over pX were detected. However, this also resulted in a decrease of the separation factors of oX/pX and mX/pX.ConclusionThe high resolution and large separation factors for oX/pX and mX/pX make CD‐MOF‐1 an efficient and reliable alternative adsorbent to the isolation protocols for xylene isomers currently used in the petrochemical industry. © 2018 Society of Chemical Industry