Polystyrene/molybdenum disulfide (PS/MoS_2) nanocomposites were prepared by means of one-step in situ anion polymerization of the intercalated monomers. The nanocomposites were characterized by means of XRD, FT-IR and SEM. The results indicate that the interlayer of MoS_2 has been expanded (0.672) nm by intercalating polystyrene molecules, it shows the nanocomposites are intercalation composites. The oxidation behavior of the intercalation composites prepared by one-step and two-step method were investigated by XPS. The results indicate that the oxidation behavior of the two intercalation composites is different from each other, the former is mainly resulted in Mo~(4+) to Mo~(6+), the later is mainly resulted in S~(-2) to S~(6+) for MoS_2, respectively.