In this work, we aim to introduce a novel type of PMMA/Fe 2 O 3 hollow nanospheres composite, covering both its synthesis by a microemulsion method that can be grouped into a soft templating category and its niche application. PMMA/Fe 2 O 3 hollow nanospheres composite was fabricated by using a cmbination of O/W microemulsion to prepare polypyrrole (PPy) core and W/O microemulsion to decorate a PMMA shell containing Fe 2 O 3 nanoparticles. At the end, the PPy core was removed with several washing to produce hollow nanospheres composite. The prepared PMMA/ Fe 2 O 3 nanocomposite was characterized with Fourier transform infrared spectrometer (FT-IR), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), transmission electron microscope (TEM), high resolution TEM (HR-TEM), Brunauer−Emmett−Teller (BET), and vibrating sample magnetometer (VSM) analysis. The removal of benzothiophene from an oil model by using the prepared nanocomposite as an absorbent was studied. The obtained results showed that the nanocomposite has good adsorption capacity and also enough magnetic property for simple magnetic recovery with stability after several runs.