Nano-sized magnetic Fe-0/polyaniline (Fe-0/PANI) nanofibers were used as an effective material for sonocatalytic degradation of organic anionic Congo red (CR) dye. Fe-0/PANI, was synthesized via reductive deposition of nano-Fe-0 onto the PANI nanofibers at room temperature. Prepared catalyst was characterized using HR-TEM, FE-SEM, XRD, FTIR instruments. The efficacy of catalyst in removing CR was assessed colorimetrically using UV-visible spectroscopy under different experimental conditions such as % of Fe-0 loading into the composite material, solution pH, initial concentration of dye, catalyst dosage, temperature and ultrasonic power. The optimum conditions for sonocatalytic degradation of CR were obtained at catalyst concentrations = 500 mg.L-1, concentration of CR = 200 ppm, solution pH = neutral (7.0), temperature = 30 degrees C, % of Fe-0 loading = 30% and 500 W ultrasonic power. The experimental results showed that ultrasonic process could remove 98% of Congo red within 30 min with higher Q(max) value (Q(max) = 446.4 at 25 degrees C). The rate of degradation of CR dye was much faster in this, ultrasonic technique rather than conventional adsorption process. The degradation efficiency declined with the addition of common inorganic salts (NaCI, Na2CO3, Na2SO4 and Na3PO4). The rate of degradation suppressed more with increasing salt concentration. Kinetic and isotherm studies indicated that the degradation of CR provides pseudo-second order rate kinetic and Langmuir isotherm model compared to all other models tested. The excellent high degradation capacity of Fe-0/PANI under ultrasonic irradiation can be explained on the basis of the formation of active hydroxyl radicals ((OH)-O-center dot) and subsequently a series of free radical reactions. (C) 2017 Elsevier B.V. All rights reserved.