The new low‐cost clean pre‐desulfation technology is very important in pyrometallurgy and hydrometallurgy. However, traditional reactors have low space‐time yield and desulfation rate, resulting in high energy consumption and SO2 emissions in the industrial desulfation processes. Herein, dual rotating liquid film reactors (RLFRs) and lime are proposed to construct a recyclable, ultra‐fast, and value‐added desulfation method. Parameter optimization and kinetic calculations prove that the above reactions are controlled by internal diffusion, revealing that RLFR promotes the mass transfer and reaction rate. The new process greatly shortens the desulfation time of lead paste from 40 min to 10 s with a high desulfation rate of 99.7%, and the sulfation time of lime from 30 min to 30 s with a sulfation rate of 98.6% with a net profit of 55.99 ¥/ton by cost accounting. Moreover, ten batches of continuous scale‐up experiments demonstrate the stability of processes, the desulfation and sulfation rates are kept at 99.7% and 98.2%, which greatly reduces the emissions of waste desulfate liquor. This work provides a new universal strategy for a sustainable, low‐cost, and clean desulfation method of waste resources to achieve technical and economic feasibility.