Amberlite XAD-4 resin was functionalized by coupling through the –N=N- group (azo spacer arm) with p-toludine. Resulting intermediate products were characterized by FTIR method. The functionalized resin was characterized by elemental analysis and FTIR. Thermokinetic parameters were determined by Freeman-Carroll (FC) and Sharp- Wentworth (SW) methods. Activation energies of the degradation were found to be 27.28 kJ (FC method) and 25.60 kJ (SW method). Free energy change (ΔG) and entropy change (ΔS) of the degradation was calculated by both of these methods were found to be in good agreement. The order of degradation obtained by FC method was found to be zero which was further confirmed by SW method.