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A novel adsorbent lignin-calcium was fabricated by a simple flocculation–sedimentation approach to remove methylene blue. The structure and morphology of the well-prepared sample were analyzed by multiple characterization methods. Lignin-calcium microspheres demonstrated a mesoporous and inserted layer structure with a coarse surface. Methylene blue (MB) adsorption by lignin-calcium complied with the Langmuir model, showing a maximum adsorption amount of 803.9 mg/g, exceeding that reported in the literature by 3–22-fold. The adsorption kinetics matched the pseudo-second-order model well. The pore volume diffusion model was technically applied to evaluate the mass transfer mechanisms. The effective pore volume diffusion coefficient was 6.28 × 10–12 m2/s. Furthermore, lignin-calcium exhibited excellent adsorbability for methylene blue across a pH range from 3 to 11 and could be regenerated by hydrochloric acid with an elution efficiency of 62.44%. Multiple mechanisms may support the adsorption. Altogether, the tailor-made lignin-calcium is promising as an efficient and sustainable adsorbent for scavenging cationic dyes from dyestuff effluent.