Zn-Al-CO3 layer double hydroxides (LDHs) are synthesized by a simple hydrothermal method, followed by the anion-exchange processes to intercalate dodecyl sulfate (DS) anions into LDHs interlayer. The structures and morphologies of the as-prepared samples are characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results illustrate all samples have typical layer structure of LDHs, and the LDHs intercalated with dodecyl sulfate (LDH-DS) has better crystallization and smoother surface compares to conventional LDHs. Subsequently, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), Tafel and galvanostatic charge/discharge tests on LDH-DS electrode are performed. The results demonstrate that the exchanged sample has superior electrochemical performances in comparison with LDH-CO3, such as superior cycle stability, higher specific discharge capacity and utilization ratio of the active material. The specific discharge capacity of the LDH-DS electrode reaches 375mAhg−1 and exhibits excellent stability after 150 cycles.