Lead-contaminated wastewater causes toxicity to aquatic life and water quality for water consumption, so it is required to treat wastewater to be below the water quality standard before releasing it into the environment. Duck eggshell powder (DP), duck eggshell powder mixed iron (III) oxide-hydroxide (DPF), calcinated duck eggshell powder (CDP), and calcinated duck eggshell powder mixed iron (III) oxide-hydroxide (CDPF) were synthesized, characterized, and investigated lead removal efficiencies by batch experiments, adsorption isotherms, kinetics, and desorption experiments. CDPF demonstrated the highest specific surface area and pore volume with the smallest pore size than other materials, and they were classified as mesoporous materials. DP and DPF demonstrated semi-crystalline structures with specific calcium carbonate peaks, whereas CDP and CDPF illustrated semi-crystalline structures with specific calcium oxide peaks. In addition, the specific iron (III) oxide-hydroxide peaks were detected in only DPF and CDPF. Their surface structures were rough with irregular shapes. All materials found carbon, oxygen, and calcium, whereas iron, sodium, and chloride were only found in DPF and CDPF. All materials were detected O–H, C=O, and C–O, and DPF and CDPF were also found Fe–O from adding iron (III) oxide-hydroxide. The point of zero charges of DP, DPF, CDP, and CDPF were 4.58, 5.31, 5.96, and 6.75. They could adsorb lead by more than 98%, and CDPF illustrated the highest lead removal efficiency. DP and CDP corresponded to the Langmuir model while DPF and CDPF corresponded to the Freundlich model. All materials corresponded to a pseudo-second-order kinetic model. Moreover, they could be reusable for more than 5 cycles for lead adsorption of more than 73%. Therefore, CDPF was a potential material to apply for lead removal in industrial applications.