A titanium-containing redox material with disordered wormhole-like mesoporous structure was prepared using microwave heating. Substantially accelerated crystallization was achieved using microwave heating compared with the conventional oven heating. Development of the mesopore structure was confirmed by XRD, TEM, and N-2 physisorption. Incorporation of titanium into the mesopore structure was confirmed by UV-vis spectroscopy. A laser light particle size analyzer showed that smaller particle size and narrower particle size distribution were obtained with microwave heating than with oven-heated hydrothermal synthesis. These mesoporous titanosilicates were equally active as catalysts for liquid-phase oxidation of 2,6-di-tert-butylphenol with hydrogen peroxide as an oxidant.