Since the 1990s, due to the increasing demand of high-quality iron oxide powder as raw materials for magnetic material industry, acid regeneration unit is widely used in the production of iron oxide. As the largest application of steel mills process, spray roasting method has been deeply studied. Among these researches, lots of works focus on the optimization of the quality of iron oxide powder, including purification and BET improvement. But reports referred material balance about acid regeneration process can hardly be found. Furthermore, the material balance as a key theory support achieves controlling exhaust emissions in acid regeneration process. Therefore, this paper via material balances to improve iron loss and acid loss occurred during the acid regeneration process. Meanwhile, these calculations as theoretical basis for analyzing exhaust gas treatment equipment were used to strive to accurately identify the causes of excessive waste acid and iron oxide dust, and a new door has been opened to protect the environment and reduce the air pollution.