The catalytic synthesis of red pigment power is studied by taking naphthol AS, aniline and sodium nitrite as raw material, sodium dodecyl sulfate (SDS), sodium dodecyl sulfonate (DBS) and sodium dodecyl benzene sulfonate (SDBS) as phase transfer catalysts via diazotization and coupling reaction. The influence of the types of phase transfer catalysts, catalyst dosage and reaction time on the yield of red pigment power is researched. Experiment results show that both reaction products and yield are obviously promoted if the phase transfer catalysts are added, the mixed catalysts (SDS and SDBS) has the best catalytic activity, there is no significantly foaming phenomenon in the reaction, the optimal dosage of phase transfer catalysts is 0.1g, the optimal reaction time is 30min, and the yield can reach 88.1%. This method has the characteristics such as simple operation, fast reaction speed, high product yield, and good product purity and so on.