The dispersion stability of multi-walled carbon nanotube (MWNTs) with carboxylate and carboxylic anion in aqueous acrylamide solution was studied. The solutions were subsequently used in in situ solution polymerization by adding free-radical initiator to prepare polymerized poly(acrylamide) (PAAm)/CNTs nanocomposites films. The reactor was sonicated for sufficient dispersion of modified MWNTs in the acrylamide aqueous solution, using an ultrasonic generator for 15 mm. After dispersion, the reactor equipped with condenser, thermometer, and a magnetic stirrer was kept at 60 °C and 200 rpm. After 1 h of nitrogen purging, the 0.2 g of KPS was added as a water soluble initiator and the polymerization was carried out at 70° C for 2 h. The result suggests that the surface treated MWNTs, especially MWNTs with carboxylic anion groups, have much improved dispersion stability in aqueous acrylamide solution.