Synthesis of diaryliodonium salts from aromatics and potassium iodate was investigated by means of orthogonal and single factor methods.Results showed that the yields of diphenyl iodonium hexafluorophosphate,dimethylphenyl iodonium hexafluorophosphate,di-tert-butyl phenyl iodonium hexafluorophosphate and bisdodecylphenyl iodonium hexafluorophosphate reached 52.7%,63.6%,68.7% and 45.9%,respectively.All the products were confirmed with liquid chromatography,LC-MS and NMR.