TiO2/γ-AlO(OH) nanocomposite powder photocatalysts was synthesized by low-temperature solution method. In the above synthesis process, aluminum nitrate, tetrabutyl titanate, triammonium citrate and polyvinylpyrrolidone (PVP) were used as aluminum source, titanium source, foaming agent and surfactant, correspondingly. The synthesized nanocomposites were further characterized by HRTEM, FESEM, EDS, XRD, UV-Vis DRS and N2adsorption-desorption(BET). In addition, effects of different parameters, including γ-AlO(OH) doping mass fraction and PVP surfactant, on the morphology and photocatalytic activity of TiO2/γ-AlO(OH) composite nanopowders were investigated. Effect of adsorption on catalyst activity was also studied. Experimental results show that the mesoporous structure of γ-AlO(OH) nanospheres (the support material) prevents agglomeration and growth of TiO2 nanocrystals. It is also found that, with adding proper PVP surfactant, agglomeration of composite powders can be slow down and micro-morphology of composite powders can be controlled. Experimental results indicate, with doping 10% mass fraction γ-AlO(OH) and adding 0.1 mmol PVP, TiO2/γ-AlO(OH) composite nano-powder has BET specific surface area of 334.27 m2/g and can exhibit the optimum catalytical performance. After 30 min of illumination, with using the synthesized nanocomposites, degradation efficiency of Rhodamine B can be 94.26%, which is much higher than pure anatase TiO2 and commercial P25 catalyst. © 2020, Editorial Office of Acta Petrolei Sinica(Petroleum Processing Section). All right reserved.