Sodium dodecyl sulfate (SDS) intercalated Mg3Al layered double hydroxide (LDH), denoted as DS-LDH, nanohybrids were synthesized via mechano-hydrothermal (MHT) route. The intercalation amount (A(in)) of dodecyl sulfate (DS) anions into LDHs could be easily quantitatively controlled by the molar ratio of SDS to Al(OH)(3) in the starting materials. The removal efficiency (ER) of the DS-LDHs for 2,4-dichlorophenoxyacetic acid (2,4-D) from aqueous solutions was determined. With increasing Ain, the ER increased. An obvious sorbent concentration effect (C-s-effect) was observed: the saturation sorption capacity of 2,4-D on the DS-LDHs decreased as C-s increased. The sorption isotherms of 2,4-D on the DS-LDHs for any given Cs values can be described with the Langmuir and Freundlich isotherms. The C-s-effect can be described with the surface component activity (SCA) model, namely, Langmuir-SCA and Freundlich-SCA isotherms. The nanohybrids are promising sorbents for treating 2,4-D-containing wastewater, and the MHT method can be used to synthesize DS-LDH sorbents. (C) 2014 Elsevier B.V. All rights reserved.