Textile wastewater contains large quantities of azo dyes mixed with various contaminants especially heavy metal ions. The discharge of effluents containing methyl orange (MO) dye and Cu2+ ions into water is harmful because they have severe toxic effects to humans and the aquatic ecosystem. The dried algal biomass was used as a sustainable, cost-effective and eco-friendly for the treatment of the textile wastewater. Box-Behnken design (BBD) was used to identify the most significant factors for achieving maximum biosorption of Cu2+ and MO from aqueous solutions using marine alga Fucus vesiculosus biomass. The experimental results indicated that 3 g/L of F. vesiculosus biomass was capable of removing 92.76% of copper and 50.27% of MO simultaneously from aqueous solution using MO (60 mg/L), copper (200 mg/L) at pH 7 within 60 min with agitation at 200 rpm. The dry biomass was also investigated using SEM, EDS, and FTIR before and after MO and copper biosorption. FTIR, EDS and SEM analyses revealed obvious changes in the characteristics of the algal biomass as a result of the biosorption process. The dry biomass of F. vesiculosus can eliminate MO and copper ions from aquatic effluents in a feasible and efficient method.