In order to concentrate the diluted sulfuric acid from the titanium dioxide (TiO2) production of sulphate process, a new concentration process was proposed by coupling chemical dehydration and multi-effect evaporation. The ferrous sulfate monohydrate (FeSO4·H2O), as the dehydrant, was added to the diluted sulfuric acid to form fer-rous sulfate heptahydrate (FeSO4·7H2O) according to the H2SO4-FeSO4-H2O phase diagrams, which partially removes the water. This process was named as Chemical Dehydration Process. The residual water was further re-moved by two-effect evaporation andfinally 70 wt％sulfuric acid was obtained. The FeSO4·H2O can be regener-ated through drying and dehydration of FeSO4·7H2O. The results show that FeSO4·H2O is the most suitable dehydrant, the optimal reaction time of chemical dehydration process is 30 min, and low temperature is favor-able for the dehydration reaction. 45.17％of the entire removed water can be removed by chemical dehydration from the diluted sulfuric acid. This chemical dehydration process is also energy efficient with 24.76％saving com-pared with the direct evaporation process. Furthermore, 51.21％of the FeSO4 dissolved originally in the diluted sulfuric acid are precipitated out during the chemical dehydration, which greatly reduces the solid precipitation and effectively alleviates the scaling in the subsequent multi-effect evaporation process.