The aim of the present work was to prepare microgel nanocomposites based on silver and magnetite to apply as adsorbents and heterogeneous catalysts for removal of methylene blue (MB) cationic dye from aqueous solution. For this, 2-acrylamido-2-methylpropane sulfonic acid (AMPS) and acrylamide (AAm) monomers were used to prepare AMPS/AAm microgel based on the emulsion technique. Ag and Fe 3 O 4 nanoparticles were embedded into the AMPS/AAm microgel using the in situ technique. Their particle sizes, surface charges, crystalline lattice structure, morphology, magnetic properties and thermal stability were investigated. The AMPS/AAm hydrogel nanocomposites were used as an adsorbent to remove MB dye. The AMPS/AAm microgel nanocomposites were tested as catalysts to reduce MB and degrade its chemical structure with heterogeneous Fenton oxidation using Ag and Fe 3 O 4 nanocomposites, respectively. This study presents promising data as the prepared materials used as adsorbents and catalysts show competitive features compared with the data presented in the literature.