Polyaniline (PANI)/MoS2 composites with porous microspheres were prepared by a hydrothermal and in situ polymerization method. The structural, optical, and morphological properties were characterized by X-ray powder diffraction, FTIR, scanning electron microscope, transmission electron microscope. The XRD results confirmed that the PANI/MoS2 composite was formed. Morphological characterization reveals that the successful formation of few to multilayered MoS2 nanosheet intercalated with the PANI nanoparticles.