The present work proposes the synthesis of robust biochar from Gracilaria Rhodophyta red weeds for sequential removal of Al(III) and fluoride from wastewater. The sorption experiments have been modeled by preliminary optimization of operational parameters using 24 factorial statistical modeling. The model has estimated an optimum sequential synergetic removal of 44.5 mg/g of Al(III) and 2.1 mg/g of fluoride onto the biochar. FESEM, BET, XRD, EDX, and FTIR established the potentiality of biochar toward synergetic sorption of Al(III) and fluoride. The thermodynamic analysis projected that the adsorption is physisorption in nature. The adsorption of Al(III) and fluoride follows the Langmuir and Freundlich isotherm models, respectively, and the kinetic analysis established the pseudo-second-order deposition of Al(III) and fluoride ions. The synthesized adsorbent is regenerative enough and could achieve synergetic removal of Al(III) and fluoride ions from industrial- and groundwater-contaminated water bodies. Practitioner points: Biochar from seaweeds is explored in the sequential removal of Al(III) and F− ions. Statistical model is developed for % adsorption and tested for reliability by ANOVA. GRBC sorbed 44.5 and 2.1 mg/g of Al(III) and F− ions, respectively, at optimum levels. FESEM, EDX, XRD, and FTIR characterization confirm the potentiality of the GRBC. GRBC sorbed ⁓90% of Al(III) and F− ions from wastewater and is regenerative. © 2019 Water Environment Federation