The monodispersed nano-Sb2O3 was prepared from SbCl3 as raw material by alcoholysis,hydrolysis and treatment with surfactants.Various factors and levels in the preparation of monodispersed Sb2O3 nanoparticles were studied with changing factors and orthogonal test. The effects of the type and amount of surfactants as dispersant on the size and morphology were also studied with TEM and sedimentation.The results showed that the optimum conditions of preparing monodispersed Sb2O3 nanoparticles were concentration of SbCl3 in CH3CH2OH 0.17 g8226;ml-1,reaction temperature 318 K and reaction time 1 h.The surfactants,as shown in the experiments,were important to disperse and keep Sb2O3 nanoparticles.The monodispersed nano-Sb2O3 of about 25 nm could be obtained by treating 1 g nano-Sb2O3 with 1.0 ml PEG or 0.3 g CTAB.