Catalysts of aluminum dihydrogen tripolyphosphate supported by activated carbon ((ATP-AC) were prepared by using activated carbon oxidized by Na2S2O8, H2O2 and HNO3, respectively, and characterized by Brunauer-Emmett-Teller (BET), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscope (FE-SEM) and X-ray diffraction (XRD). The orthogonal design experiment was used to obtain the best condition of the three kinds of catalysts. The results show that the three kinds of ATP-AC catalyst disply higher activity and selectivity. The optimal conditions are: for preparation conditions of catalyst ATP-AC-1: oxidant concentration c (Na2S2O8) = 0.75 mol/L, bonding temperature t = 603 K, mass ratio W% (ATP) = 60%; for catalyst ATP-AC-2: oxidant concentration c(H2O2) = 1.0 mol/L, bonding temperature t = 603 K mass ratio W% (ATP) = 60%; for catalyst ATP-AC-3: oxidant concentration (HNO3) = 0.5 mol/L, bonding temperature t = 603 K, mass ratio W% (ATP) = 60%. The yield of tributyl citrate is over 90%. Three kinds of oxidants increase the carbon-oxygen functional groups of activated carbon and improve its hydrophilicity. The pore structure of oxidated AC is more regular, and the quantity of microporous and larger pores is increased. All these changes promote the chemical bonding between activated carbon and ATP.