Abstract: Nitric acid-modified titanium ore (NATO) sorbents were prepared by high energy ball milling process. The adsorption properties of NATO sorbents were evaluated by the decoloration efficiency of methyl orange (MO) under dark-state absorption. In the adsorption stage, L9(3⁴) orthogonal experiments of different factors, for example, doping ratio, calcination temperature, soaking time and heating rate were performed. Based on the orthogonal experiments, the optimal operating parameters, 2.0wt% nitric acid, 300°C calcination temperature, 3 h soaking time, and 10°C/min heating rate, are obtained. In this optimal condition, the decoloration efficiency of MO reaches 96.8%, which is significantly better than the undoped samples. Thus, it is feasible to treat dye wastewater by these NATO sorbents.