In view of the current situation where the acid resources and valuable components in titanium dioxide waste acid cannot be effectively extracted and are prone to secondary pollution, the research team proposed a new technology of step extraction and comprehensive utilization of titanium dioxide waste acid. In this paper, the preparation of doped iron phosphate from waste acid by selective precipitation was studied. The thermodynamics of selective precipitation, the effect of the reaction temperature, the initial pH value, the molar ratio of P/Fe, and the dispersant on the precipitation process were investigated in detail. The thermodynamics results show that iron(II) in titanium dioxide waste acid is oxidized and is preferentially precipitated with phosphoric acid to form iron(III) phosphate, when compared with other impurity ions. The experimental results show that the optimal precipitation condition is a temperature of 60 °C, an initial pH value of 2.5, an optimal P/Fe molar ratio of 1.1, and a dispersant polyethylene glycol at 5 mL (Per 50 mL of waster acid). After calcination, the precipitate mainly consists of iron phosphate and a small amount of aluminum phosphate. Meanwhile, the utilization ratios of iron and phosphorus were 98.81% and 98.39%, respectively. Moreover, the mass percentage of Fe2O3 and P2O5 and the molar ratio of Fe/P were 99.13% and 1.03, which basically met the requirements of the iron phosphate precursor.