ABSTRACT:Wool fibres are treated with titanate tetrabutyl in the presence of C. I. Reactive Blue 69 dye in one-pot process under hydrothermal conditions. The structural changes of wool fibres before and after treatments as well as the remaining particles are characterized by small-spot Micro X-ray fluorescence (µ-XRF), field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC) techniques. The properties of percentage of exhaustion, K/S value, colour fastness to light, tension, photocatalytic activity, and diffuse reflectance spectrum (DRS) are also investigated. The experimental results indicate that after treatment with titanate tetrabutyl and C. I. Reactive Blue 69, wool fibres are evenly immobilized with a thin layer of anatase phase TiO 2 nanoparticles with an average grain size of less than 10 nm. The TiO 2 nanocrystals are synthesized and simultaneously grafted onto wool fibres via the C-Ti 4+ , S-Ti 4+ (Ti 2+ ), and N-Ti 4+ bonds. The thermal stability of wool fibres changes a little. The capability of wool fibres to protect against ultraviolet radiation is improved. The tensile properties decrease to some degree. The photocatalytic activity to decolourize methylene blue dye is endowed. A high degree of percentage of exhaustion and K/S value are obtained by adding a certain amount of acetic acid in the precursor solution, which can well be matched with the custom dip dyeing technique.