In the present work, the PANI and PANI/Zr composite powders were synthesized by the method of chemical polymerization in the inorganic acid medium. The morphology of prepared composites demonstrates fiber-like structure revealed by scanning electron microscopy. The value of the specific surface area estimated by the BET technique depends on the type of the composite powder and was found to be 66.8 and 142.05 m 2 /g for PANI and PANI/Zr respectively. UV–Vis spectroscopy was employed to characterize the optical properties of the synthesized powder composites. The incorporation of zirconium gives rise to the red shift of π– π* transition of pristine PANI. The synthesized composite powders were used for preparation of PANI/PVA and PANI/Zr/PVA composites which electrochemical properties were compared in different electrolytes: 0.5 M KOH, 0.5 M NaCl and 0.5 M H2SO4. Excellent electrochemical reversibility was found out for both PANI/PVA and PANI/Zr/PVA composites. Effect of electrolyte type and current value on the specific capacitance of the prepared composites was observed.