HT) with different Ni/Zn ratios have been prepared by a coprecipitation method. The properties and microstructure of Ni/Zn/Al-HT precursors and derived catalysts were characterized by X-ray diffraction (XRD), H 2 -temperature programmed reduction (TPR), N 2 physical adsorption analysis (BET), scanning electron microscopy (SEM) and particle size distribution. The results exhibited that the as-prepared samples consisted of a hydrotalcite phase and a ZnO phase, and Zn 2+ was introduced into the layers. At the ratio of Ni/Zn ¼ 1, the ZnAl 2 O 4 phase emerged after calcination; Ni still remained in its original state after reaction, and ZnO always existed during the whole process. In aqueous-phase reforming (APR) of ethylene glycol, the H 2 production rate over Ni/Zn/Al-HT was high, and the selectivity of H 2 can almost reach 100% with a high conversion rate exceeding 99%.