This paper presents a novel immobilization method for the preparation of highly dispersed TiO2 nanoparticles supported on porous glass beads. The method involves an in situ ion exchange process and a calcination process. Mono-dispersed TiO2 nanoparticles exhibiting the anatase phase with different mean diameter and different loading amount have been successfully prepared through the controllable and green way. With the increase of loading amount of Ti from 0.08 wt.% to 4.55 wt.%, the mean diameter of the TiO2 nanoparticles varied from 3.8 to 5.3 nm. And the band gaps of the TiO2 nanoparticles with the highest and lowest loading amount are 3.25 and 3.00 eV, respectively. The prepared TiO2 nanoparticles supported on porous glass beads showed excellent photocatalytic performance for the degradation of methyl orange (MO). For the catalyst with a Ti content of 0.08 wt.%, when the dosage was 1.93e-5 g/mL, 65% of the total MO decomposed after 30 min; for the catalyst with a Ti content of 2.56 wt.%, when the dosage reached 0.81e-3 g/mL, complete degradation was observed. (C) 2012 Elsevier B.V. All rights reserved.