The Wastewater from the weight reduction process of polyester is more difficult to be treated biologically than the general wastewater from dyeing and finishing processes in textile industries. Above wastewater shows high pH, high organic strength and wide variation of organic loading. These characteristics are due to TPA and EG resulting from alkaline weight-reduction process and make trouble in the operation of activated sludge process. Therefore, the objective of this study is to develop the pretreatment method for the successful operation of treatment process. For the successful pretreatment process, the wastewater from weight-reduction process should be segregated from other wastewater stream and then acidified with concentrated sulfuric acid to precipitate out TPA from DST solution. At the optimum pH of 2. 2, the initial $COD_{cr}$ 60,000mg/l is reduced to 11,500mg/l and the removal efficiency of $COD_{cr}$ is 81.1%. The required amount of sulfuric acid for pretreatment is not greater than the amount for the the existing neutralization process. Moreover, the supernatant of pretreatment process can be reused in acidification of wastewater.