Two novel ferrocene derivatives (oxalylferrocene and oxalyl(ethylferrocene)) were synthesized by using acylchoride as acylating agent, anhydrous aluminum chloride as catalyst and 1,2-dichloroethane as solvent. The structures of the titled compounds were characterized by ¹HNMR, FT-IR, MS and elemental analysis techniques, and the thermal decomposition properties of AP with 5%(weight) titled compounds were investigated by differential thermal analysis (DTA) and thermogravimetry(TG). Results show that the maximum weight loss rate peak temperature of AP is reduced by about 100 ℃ when adding 5%(weight) ferrocene derivatives.