Zirconia (ZrO 2)-modified graphitic carbon nitride (g-C 3 N 4) nanocomposite was used for effective photodegradation of 4-nitrophenol (4-NP) in water. The ZrO 2 nanoparticles, g-C 3 N 4 nanosheets, and ZrO 2 /g-C 3 N 4 nanocomposite were well characterized by including N 2 adsorption, X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, UV-Vis diffuse reflectance spectroscopy, photoelectrochemical measurements, and photoluminescence spectroscopy methods. ZrO 2 /g-C 3 N 4 nanocomposites were formed at room temperature using sonication and used for effective for photodegradation of 4-NP under irradiation with visible light. The nanocomposite samples resulted in a significant increase in photocatalytic activity compared with single-component samples of g-C 3 N 4. In particular, the ZrO 2 /g-C 3 N 4 nanocomposite exhibited the significant increase in the photocatalytic activity. The ZrO 2 /g-C 3 N 4 nanocomposite showed an excellent catalytic activity toward the reduction of 4-NP in aqueous medium. Further, ZrO 2 /g-C 3 N 4 nanocomposite can be reused several times for photocatalytic degradation as well as for 4-NP adsorption.