In order to avoid using P2O5 as phosphorylation reagent in phosphorylation reaction, an amphoteric phosphate ester surfactant was synthesized by using polyphosphate acid as phosphorylation reagent. The phosphorylation reaction studies confirmed the best condition was molar ratio of hydroxyl and P2O5 of 3.0:1.0, reaction temperature of 80°C and reaction time of 5.5h. The content of monoalkyl phosphate (MAP) and the conversion rate reached to 89.3% and 97.2%, respectively. The production of MAP product was increased by 15% than that of obtained by P2O5 as phosphorylation reagent. The structure of the phosphate ester surfactant was characterized by FTIR. The surface tension of phosphate ester surfactant was better than that of dodecyl trimethyl ammonium bromide and sodium dodecyl sulfate. The application results indicated the leather oiled by the amphoteric phosphate surfactant was softer and than that treated by L-3 fatliquor.