A combination of delamination and ion exchange allowed us to obtain new solids consisting of nanolayers of double hydroxides containing hydroxyl as charge balancing ion (i.e., meixnerite monolayers). The solids were prepared from Mg/Al HLCs containing dodecylbenzenesulphonate (DBS) anion in the interlayer region, using a procedure involving sonication and swelling of the interlayer region in the presence of 1-butanol as solvent. This treatment converts the initial, milky dispersion, into a translucent dispersion suggesting that the solid is completely exfoliated. Then, the translucent dispersion is treated with an NaOH solution in 1-butanol in order to exchange DBS- ions with OH- ions and simultaneously precipitate the DBS sodium salt while offsetting charge deficiencies in the solid layers. The exchange process results in no relamination of the structure, which allows a new material consisting of individual nanolayers of meixnerite to be prepared.