A simple and rapid process has been developed for the preparation of mesoporous anatase TiO 2 crystalline particles coupled by homogeneously dispersed Na 4W 10 O 32 at a lower temperature ( 200 ℃ ) by combining sol-gel and programmed temperature hydrothermal methods. The composite,Na 4W 10 O 32 /TiO 2,has a uniform mesopore distribution with the average pore diameter of 3.8 nm,and its BET surface area is 178.4 m 2/g. The average size of the composite is below 10 nm. This new photocatalyst exhibited a visible-light photocatalytic activity to decompose para -thion-methyl.