Abstract: Antistatic agents of alkyl phosphate were synthesized with aliphatic alcohol and P2O5 as main materials. Firstly, the synthesis conditions were discussed by orthogonal experiments. The results showed that stable products with high conversion rate can be obtained when esterified under 80℃ for 5h, hydrolyzesdat 70℃ for 2h, with diethanolamine as neutralization agent. The effect of n（dodecyl alcohol）: n（octadecanol）on the yield under given conditions was small, but the product’s moisture absorption increased and heat resistance decreased as octadecanol increased, while the product’s antistatic property was best when n（dodecyl alcohol）: n（octadecanol）was 2:1.