In the work reported, we utilized a facile flash nanoprecipitation process to generate Ag nanoparticles@nanospheres polymer composites. Ag nanoparticles can be loaded onto the polymeric polystyrene (PS) nanosphere surface using a simple and inexpensive method through in situ growth; the amount of loaded Ag nanoparticles and the size of holes on the PS surface prepared by flash nanoprecipitation can be fine‐tuned by changing the pH of the water medium and the PS nanoparticles should have a greater specific area. The as‐synthesized Ag@PS composite nanoparticles obtained via the one‐step and continuous preparation route show high catalytic activity in the reduction reaction of 4‐nitrophenol. Importantly, the nanoparticles show no loss of catalytic performance over five cycles.
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