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In this paper, the photocatalytic effect of Nb(x)/TiO₂ nanocomposites on the degradation of phenol red (PR) was studied. Nb(x)/TiO₂ nanocomposites are fabricated by a simple sol-gel route with new experimental conditions. The structural and optical properties were determined using high transmission electron microscopy (HRTEM), X-ray diffraction, Raman spectroscopy, photoluminescence, and UV-vis absorbance spectroscopy. Compared to pure anatase TiO₂, the recently fabricated Nb(x)/TiO₂ nanocomposite has a shift in the optical band edge to the visible wavelength. Consequently, it has high performance in adsorption capacity and photocatalytic activities. A time of 160 min has been observed to be suitable for mostly degradable 20 mgL⁻¹ of phenol red on Nb(2.0)/TiO₂ composite. The kinetic results were in good agreement with the first-order kinetic model at different concentrations. In addition, the results showed that the addition of Nb led to a significant degradation process. The decomposition of phenol red pollutants showed a synergistic effect of the Nb(2.0)/TiO₂ nanocomposites on wastewater treatment.