The technique of foam fractionation has already been well received in the field of isolation of proteins using a suitable surfactant. The lower operating cost also makes this technique eligible for treating various wastewater streams. In view of this, methylene blue dye was separated and recovered from its solution by employing sodium dodecyl benzene sulfonate as a collector in a foam fractionator operated in a semi-continuous manner. The separation characteristics were accessed at varying aeration rates, dye concentrations and liquid loadings. Prior to this, the values of other operating variables such as operation time, concentration of the surfactant and solution initial pH were fixed. Subsequently, in order to attain maximum removal fraction and enrichment ratio, individually, Taguchi methodology yielded the optimum values of operating variables, which are crucial for the optimal operation of any foam fractionator. The results revealed implementation of foam fractionation technique in isolating methylene blue dye from dyeing wastewater to be fairly good.