A laboratory study on the liquid–liquid extraction system has been carried out for the removal and recovery of methyl red from aqueous solutions using xylene as an extractant. The concentration of methyl red has been studied in the range of 1.72×10 −4 to 1.72×10 −3 molL −1 . The efficiency of dye extraction increased with increasing time of extraction. Distribution ratio is reasonably high (D=49) even in the presence of inorganic salts. Extracted dye in the organic phase has been stripped into sodium hydroxide solution. The organic solvent is reused for reextraction of the dye from aqueous solution. The efficiency of reused organic solvent was maintained up to 10 runs. Loading capacity of dye has been found to be 14.32mg. Under optimized conditions, real textile wastewater has been studied and the results are satisfactory.