The composite anion‐exchange material MOR‐1–HA (metal–organic resin‐1–alginic acid) was investigated as sorbent for the capture of the methyl orange anion (MO−) from aqueous solutions. MOR‐1–HA shows a remarkably high sorption capacity (up to 859 mg g−1) and rapid sorption kinetics, the fastest among the reported metal–organic sorbents. It is capable of absorbing MO− over a wide pH range (1–8) and, in addition, it exhibits significant MO− sorption affinity even in the presence of large excesses of competing anions (e.g., Cl−, NO3−, SO42−). The exceptional MO−‐sorption properties of MOR‐1–HA arise not only from its highly porous structure and easily exchangeable Cl− anions, but also from a multitude of interaction effects, such as electrostatic interactions between MO− and the NH3+ groups of the material, hydration/dehydration, hydrophobicity/hydrophilicity, size and capacity of generating lateral interactions, and intercalation as revealed by theoretical studies. An ion‐exchange column with a stationary phase containing MOR‐1–HA and silica sand showed high efficiency for the removal of MO− from various types of aqueous samples. The column can be readily regenerated and reused for many runs with minimal loss (2.3–9.3 %) of its exchange capacity. The simplicity of the MOR‐1–HA/sand column and its high regeneration capability and reusability make it particularly attractive for application in the remediation of MO−‐contaminated industrial wastewater.