Concerning the situation of the current industry, and to separate and recycle sulfuric acid and iron, a new method of extracting iron and sulfuric acid simultaneously and separating them in one step was developed, and the optimal conditions for the extraction and separation were investigated. In this method, the sulfuric acid and Fe(III) of the DASE are transferred from the aqueous phase into the organic phase by the solvent extraction, in the mean time, iron and sulfuric acid are separated by mixing the loading organic phase with the WSA. Fe(III) in the organic phase is stripped into the aqueous phase, and Fe(II) in the WSA is remained in the aqueous phase. Sulfuric acid in the WSA is extracted into the organic phase which loads sulfuric acid from the DASE. The organic phase loading sulfuric acid can easily be stripped as Ref. [8], therefore, the study of stripping sulfuric acid from organic solution was omitted. The aqueous phase containing Fe(II) and Fe(III) can be used as raw material to produce a suitable production after further purifi- cation. The raffinate ofthe solvent extraction of DASE can be reused as water in the process by removing the undesirable components. And sulfuric acid with a desired concentration can be obtained by condensation of the stripping solution from the loading organic phase. The process was illustrated in Fig. 1. Obviously, this method is an effective way for the recovery of sulfuric acid and iron from DASE and WSA. Compared to the existing methods, this method can make a comprehensive use of the resources and reduce the cost on the treatment of the waste acid, and comparatively simple technical process for the separation of iron and sulfuric acid. Also, since itis easy to be duplicated and industrialized,the titanium pig ment production industry based on sulfuric acid can be benefited economically and environmentally.