Al2(1-x)MgxTi1+xO5(x=0.05-0.3) composite powder was prepared by the method of chemical coprecipitation and subsequent sintering using TiCl4, MgCl2 and AlCl3 solution as the raw materials, and ammonia and ammonium carbonate as the solvent. Thermal dynamics and kinetic dynamics analysis of the precursor during the heat treatment were explored in detail, and the reaction process of Al2(1-x)MgxTi1+xO5 (x=0.3) composite powder was confirmed. Results show that, as the temperature increases MgO reacts with TiO2 of anatase phase to form MgTi2O5. At about 650°C, anatase transfers into rutile. Then MgTi2O5 reacts with Al2O3 to produce MgAl2O4 at 900°C. When the temperature is above 1100°C, the desired Al2(1-x)MgxTi1+xO5(x=0.3) composite powder is synthesized by the reaction of MgAl2O4, Al2O3 and TiO2 of rutile phase.