We reported on the development of mesoporous zirconium hydroxide (mp-Zr(OH)4) sorbents with high capacity for adsorptive removal of organic pollutants from industrial wastewater. The sorbent was prepared by a one-step chemical precipitation method at room temperature. The adsorption capacity and removal efficiency for the chemical oxygen demand (COD) of the industrial wastewater were studied using an automatic adsorption measurement apparatus. The effects of different parameters (adsorbent dosage, adsorption time, regeneration times, adsorbate's molecular weight and adsorbate solubility), isotherm, thermodynamics, and kinetics were evaluated. By analyzing scanning electron microscopy (SEM) images and powder X-ray diffractograms (XRD) no obvious differences were observed for the sorbents before and after the adsorption of the organics, which indicated a structural stability of the sorbent. The specific surface area was reduced from 450 m2/g to 189 m2/g on adsorption, and after desorption of the organics the specific surface area was 350 m2/g. The adsorption of COD was analyzed in a Langmuir model that described the data better than the empirical Freundlich model. This finding points towards that the adsorption occurred as a monolayer on the mp-Zr(OH)4. The free energy of adsorption (ΔG) is in the range of −20 kJ/mol < ΔG < 0. Entropy changes are ΔS > 0. The kinetics of the adsorption of COD is better described with a Quasi-second-order dynamic model than with a Quasi-first-order dynamic model, which elucidates its primary reliance on porous adsorption surfaces and incorporation of chemical adsorption.