Nd_2Zr_2O_7–ZrO_2 nanocomposites were prepared via a facile process with propylene glycol as novel connecting agent and benzene tricarboxylic acid as a new complexing agent. The as-obtained Nd_2Zr_2O_7–ZrO_2 nanocomposites were characterized by transmission electron microscopy(TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis(EDX), Fourier transform infrared(FT-IR)spectroscopy, field emission scanning electron microscopy(FESEM), and X-ray diffraction(XRD). According to the morphological studies of the as-synthesized nanocomposites, it was found that the shape and particle size of Nd_2Zr_2O_7–ZrO_2 nanocomposites depended on the space-filling template type, dosage of space-filling template and tricarboxylic acid as complexing agent. Nd_2Zr_2O_7–ZrO_2 nanocomposites with different shapes and grain sizes have been synthesized. The photocatalytic behavior of as-produced Nd_2Zr_2O_7–ZrO_2 nanocomposites was also investigated through photodegradation of methylene blue dye and 2-naphthol as water pollutants. Nd 2 Zr 2 O 7-ZrO 2 nanocomposites were prepared by a facile process with propylene glycol as novel coupling agent and benzene tricarboxylic acid as a new complexing agent. The as-obtained Nd 2 Zr 2 O 7 -ZrO 2 nanocomposites were characterized by transmission electron microscopy (TEM), UV-vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and X-ray diffraction nanocomposites, it was found that the shape and particle size of Nd_2Zr_2O_7-ZrO_2 nanocomposites depended on the space-filling template type, dosage of space-filling template and tricarboxylic acid as complexing agent. Nd_2Zr_2O_7-ZrO_2 nanocomposites with different shapes and grain sizes have been synthesized. The photocatalytic behavior of as-produced Nd 2 Zr 2 O 7-ZrO 2 nanocomposites was also investigated through photodegrad ation of methylene blue dye and 2-naphthol as water pollutants.