Abstract: On a composite surfactant template(Brij35 and PEG), ordered mesoporous TiO2 was synthesized successfully. The formation of the ordered mesoporous TiO2 was analyzed by continuously monitoring the conductivity and viscosity during the reaction process, the ordered mesoporous TiO2 formed was characterized by XRD, HRTEM, SEM, FT-IR and N2 adsorption and desorption methods. The results indicated that ordered mesoporous TiO2 was of a hexa nal packed structure, at a temperature below 400 ℃, ordered mesoporous TiO2 has a higher thermal stability and a higher surface area of 252 m2•g－1,the mesoporous pore diameter was uniform with a value of 3.4 nm and the crystal was in anatase phase. After TiO2 was calcined at 500 ℃, ordered mesoporous structure was destroyed somewhat, and the formation of rutile phase appeared. The results also showed that liquid crystal template played a key role for the reaction, especially in a high polar media, in which non-polar carbon-hydrogen chain easily coagulated forming micelle, and TBOT gathered around the micelle formed, when they were acted by acid, reaction took place gradually to generate ordered mesoporous structure TiO2. It was found that taking efficient measures to control the hydrolysis and condensation processes of the reaction was the key of forming ordered mesoporous structure TiO2.