The preparation of N-phosphonomethylglycine from N-phosphonomethyliminodiacetic acid by catalytic oxidation of hydrogen peroxide had some advantages such as simple post treatment and high yield.The best result was obtained when FeSO4 and A were used as the catalysts in the synthesis of N-phosphonomethylglycine.The optimal conditions were as follows: dropping temperature was 71 ℃ in 2 h,n(N-phosphonomethyliminodiacetic acid)∶n(hydrogen peroxide)=1∶1.4,then reacted at 64 ℃ for 12 h.The overall yield of N-(phosphonomethyl)glycine was 86.3% with 93% purity.The product was characterized by IR and1HNMR.