Polyaniline (PANI) and Polyaniline/Nickel oxide (PANI/NiO) composites are prepared to use as a potential catalyst, by Chemical oxidation method using ammonium persulfate (NH4)2S2O8)) as an oxidant. Nickel oxide (NiO) nanopartiles are prepared by Sol-gel method. The synthesized products were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDX), Fourier Transform Infrared Spectroscopy (FTIR) and X-ray Diffraction technique (XRD). The prepared PANI/NiO composites are used as additive with different concentrations in diesel to investigate their efficiency as fuel additive. The catalytic properties are studied by using the synthesized products as catalyst for reduction of dyes in aqueous media. Sodium borohydride (NaBH4) is used as reducing agent. Linear relationships are obtained between time and ln(A0/At) for Methyl orange and Methylene blue. Kapp values were obtained for three catalysts showed the increasing trend of reduction for both dyes as, PANI < NiO < PANI/NiO composites. Experimental data analysis proved PANI/NiO composites to be efficient catalysts and fuel additive as compared to PANI and NiO.