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Polypyrrole/molybdenum trioxide (MoO3) composites have been prepared by the in situ polymerization technique. The prepared composites were characterized by Fourier transform infrared spectroscopy and surface morphology by employing scanning electron microscopy. It was observed that the grains are highly agglomerated and its average size is 2–4 mm. Furthermore, the dielectric study was carried out at microwave frequency. It was observed that the variations in MoO3 to polypyrrole cause the interface polarization and multiple scattering, which is useful for the absorption of large number of microwaves. Among all the composites, 50 wt% polypyrrole/MoO3 composites show the lowest real and imaginary permittivity values (i.e., 3.57 and 5.51, respectively), and for other composites, real values vary from 5.51 to 16.57. Therefore, these composites can be used as microwave application.