Nanoporous materials have been widely used in many fields. However, their synthesis with uniform particle shapes, pore sizes, pore volumes, and surface areas remains a considerable challenge. Thus, choosing a suitable controllable method for synthesizing nanoporous materials is crucial to obtain appropriate properties. Herein, nanoporous titania particles (NPTPs) were prepared via the hydrothermal method. This study investigated how the synthesis parameters such as the type of chelating agent, the hydrolysis method, and the drying technique affected the properties of NPTPs. The NPTPs were characterized by XRD, FESEM, TEM, and BET. The results demonstrated that when acetylacetone (ACAC, as the chelating agent), the spray‐hydrolysis (SH) method, and the freeze‐drying (FD) technique were used, NPTPs achieved a more uniform particle shape, a smaller particle size, a larger pore size, a larger pore volume, and a higher surface area. Ultimately, the photocatalytic degradation (PCD) of methylene blue (MB) was examined using improved NPTPs.