Toluene was nitrated effectively in fluorous phase in the presence of ytterbium(Ⅲ) perfluorooctanesulfonate（Yb（OSO₂C₈F₁₇）₃） catalyst. Perfluorodecalin(C₁₀F₁₈) was used as a fluorous solvent for this reaction. By simple separation,the fluorous phase containing catalyst has been recovered and reused for a number of times,p/o ( ratio of p-isomer to o- isomer) of the nitration product was increased to 0.92. Effects of reaction temperature,the ratio of V_PFC/V_{organic solvent} and the water in the reaction system on the nitration were investigated. It was observed that the optimum temperature for fluorous biphasic nitration of toluene was 80 ℃. Simultaneously,increasing the ratio of V_PFC/V_{organic solvent} can enhance p/o ratio.