Six new azopolyamides were synthesized from 2, 2¹–dimethoxy 4, 4¹–diaminoazobenzene [Benzenamine–(3, 3¹– dimethoxy–4, 4¹-azo) bis] condensed with any one of the following diacid chlorides viz. (i) terephthaloyl chloride. (ii) isophthaloyl chloride. (iii) 4, 4¹–azodibenzoyl chloride (iv) 3, 3¹-azo dibenzoyl chloride (v) 4, 4¹–stilbene dicarbonyl chloride and (vi) 4, 4¹–oxydibenzoyl chloride using low temperature solution method. These polyamides were characterized by thermogravimetric analyses (TGA and DTA). Activation energy has been calculated using Murray and white, coats and Redfern, Doyle's, Freeman and Carroll, Ozawa–Flyn–Waal's and modified Coats and Redfern's method.