The liming/unhairing operation is among the important processes of the leather industry. It generates large amounts of effluent that are highly loaded with organic hazard wastes. Such effluent is considered one of the most obnoxious materials in the leather industry, causing serious environmental pollution and health risks. The effluent is characterized by high concentrations of the pollution parameters. Conventional chemical and/or biological treatment of such wastewater is inefficient to meet the required limits of standard specifications, due to the presence of resistant and toxic compounds. The present investigation deals with an effective treatment approach for the lime/unhair effluent using the Fenton reaction followed by membrane filtration. The experiment was extended to a laboratory pilot-scale in a continuous treatment study. In this study the raw wastewater was treated with the predetermined Fenton's optimum dose followed by membrane filtration. The wastewater was efficiently treated and the final effluent met the standards for unrestricted water reuse.