SnO 2 /TiO 2 nanocomposite photocatalysts were prepared from TiCl 4 and SnCl 4 ·5H 2 O by supercritical fluid combination technique (SCFCT). This novel SCFCT is a combination of supercritical fluid drying method and sol-gel method. The XRD, TEM and FTIR results show that a new kind of active particle (Ti, Sn)O 2 has formed and there is no sign of SnO 2 crystals observed in the range of the doping concentration studied. The samples' photocatalytic activity was evaluated by the degradation of acrylic acid. The results indicate that the SnO 2 /TiO 2 nanocomposite photocatalysts prepared through SCFCT show significant improvement in catalytic activity as compared to pure TiO 2 or SnO 2 /TiO 2 catalysts prepared by traditional drying (TD). The effect of H 2 O 2 (0.167 v%) on the photodegradation was also investigated. After the addition of H 2 O 2 , the chemical oxygen demand (COD) of acrylic acid, which had been treated with (15.1 mol%) SnO 2 /TiO 2 nanocomposite photocatalysts for 3 h, was reduced from 400-500 to 20 mg/L. Keywords: SnO 2 /TiO 2 nanocomposite photocatalysts, supercritical fluid combination technique (SCFCT), acrylic acid, photodegradation.Acrylic acid, acrylic ester and their ramification have developed quickly in recent years. However, their production process produces a mass of waste water, which, when released into the aquatic ecosystem, becomes a source of dramatic disturbance of aquatic life. So how to deal with this problem has attracted much attention of scientists recently. At present, contaminations like acrylic acid are dealt with burning, bio-anaerobic method, which are complicated, hard-handling and high cost.Semiconductor photocatalysis appears as an emerging destructive technology, leading to the total mineralization of most of the organic pollutants [1] because of its nontoxicity, high activity and no-pollution. TiO 2 has become one of the most promising environment friendly catalysts [2] . However, photocatalytic activities of such catalysts are limited by the facts that its forbidden band is wide, and efficient photo-induced charges (electrons and holes) are only generated by near ultraviolet and are susceptible to recombination. The modifications of these catalysts include depositing noble metals on the surface of TiO 2 , doping of transition metal ions, composing of semiconductor and dye sensitization, etc. [3] .In this study, the nanocomposite photocatalysts SnO 2 /TiO 2 were prepared by novel SCFCT and a new crystal of (Ti, Sn)O 2 structure was observed which is different from the reported research [4] that most TiO 2 exists as rutile or anatase type crystal and SnO 2 is amorphous in the TiO 2 /SnO 2 complex. The photocatalytic activity for degradation of the acrylic acid was also studied. These novel catalysts are much better than those reported before, with regard to both the crystal structure and the catalytic activity. The success of the present study should shed light on the feasible application in the waste water treatment.