Aluminum titanate (Al2TiO5) powder has been synthesized at low temperature via nonhydrolytic sol-gel method by using aluminum powder as aluminum source, titanium tetrachloride as titanium source, anhydrous ethanol as oxygen donor with different catalysts. The phase transformation of aluminum titanate xerogel powder during heat treatment and the influence of the mixing orders of raw materials, catalyst kinds on the synthesis of aluminum titanate were investigated by means of differential-thermal analysis (DTA-TG), X-ray diffraction (XRD), transmission electron microscope (TEM). The results indicated that aluminum titanate powder was easily synthesized at 750 °C by using AlCl3 as catalyst with a mixing order of adding TiCl4 before AlCl3 into aluminum alcohol mixture. The catalytic order of the different catalysts in the preparation process of aluminum titanate is: FeCl3> AlCl3> MgCl2. The catalyst promoted the activation of metal aluminum powder and played a major role in the synthesis of aluminum titanate powder at low temperature via nonhydrolytic sol-gel method.