Herein, we demonstrate a simple and cost-effective method to prepare the new hierarchically Nidoped porous CaCO 3 monoliths in a large scale by mineralizing finger citron residue templates with a calcium acetate precursor. The morphology, microstructure, and element composition of as-prepared adsorbents are characterized by Scanning Electron Microscope (SEM), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), and N 2 adsorption, respectively. Adsorption performance of anionic dye Congo red was investigated in a batch experiment. The results showed that pseudo-second-order kinetic model and Langmuir adsorption isotherm matched well for the Congo red adsorption. Compared with previously reported adsorbents, due to positive and negative charge effect between Congo red and Ni, Nidoped porous CaCO 3 monoliths demonstrated a superior Congo red dye adsorption capability. The results of the present study substantiate that Ni-doped porous CaCO 3 monoliths is a promising adsorbent for the removal of the anionic dyes from wastewater.