Lead contamination in wastewater causes toxicity to aquatic life, the environment, and water quality, and it causes many human dysfunctions and diseases. Thus, it is necessary to remove lead from wastewater before discharging it into the environment. Orange peel powder (OP) and orange peel powder doped iron (III) oxide-hydroxide (OPF) were synthesized, characterized, and investigated lead removal efficiencies by batch experiments, adsorption isotherms, kinetics, and desorption experiments. The specific surface area of OP and OPF were 0.431 and 0.896 m2/g, and their pore sizes were 4.462 and 2.575 nm, respectively which OPF had a higher surface area than OP, whereas its pore size was smaller than OP. They were semi-crystalline structures that presented the specific cellulose peaks, and OPF also detected the specific iron (III) oxide-hydroxide peaks. The surface morphologies of OP and OPF were irregular and porous surfaces. Carbon (C), oxygen (O), calcium (Ca), O–H, C–H, C=C, C–O, C=O, and –COOH were observed in both materials. The pHpzcof OP and OPF were 3.74 and 4.46. For batch experiments, OPF demonstrated a higher lead removal efficiency than OP because of spending less on material dosage than OP, and OPF demonstrated high lead removal by more than 95% while OP could remove lead at only 67%. Thus, the addition of iron (III) oxide-hydroxide helped to increase material efficiency for lead adsorption. Both materials corresponded to the Freundlich model relating to physiochemical adsorption, and they also corresponded to a pseudo-second-order kinetic model relating to a chemisorption process. Moreover, both materials could be reusable for more than 5 cycles for lead adsorption of more than 55%. Therefore, OPF was potential material to apply for lead removals in industrial applications.