AbstractIn this research work, multi-responsive poly(N-isopropylacrylamide-co-methacrylic acid) copolymer microgels were synthesized via emulsion polymerization in aqueous medium. Then, nickel and cobalt nanoparticles were fabricated within these microgels by in situ reduction of metal ions using sodium borohydride (NaBH₄) as a reducing agent. Fourier transform infrared spectroscopy was used to characterize these microgels. The pH sensitivity of these copolymer microgels was studied using dynamic light scattering technique (DLS). DLS studies revealed that the hydrodynamic radius of these microgels increased with the increase in pH of the medium at 25°C. The catalytic activity of hybrid microgels for the reduction of p-nitrophenol (4-NP) to p-aminophenol (4-AP) was investigated by UV-visible spectrophotometery. The value of apparent rate constant of reaction was found to change linearly with catalyst dosage. The nickel-based hybrid system was found to be five times more efficient as a catalyst compared to the cobalt-based hybrid system for the reduction of 4-NP to 4-AP in aqueous medium.