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A two-stage method of hydrothermal carbonization and chemical activation technology was applied to prepare a novel, large surface area and rich-pore structure activation-hydrochar from sludge sewage and coconut shell due to its mild, low-cost, and well-developed merits. The pore-making mechanism of activation-hydrochar was discussed by FT-IR, XPS, SEM, TG, TG-MS, XRD, and BET characterization. These results illustrated that the first stage of hydrothermal carbonization achieved the rich-pore structure hydrochar via dehydration, decarboxy