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A mixed diluent composed of γ-butyrolactone (γ-BL) and dioctyl phthalate (DOP) was employed for preparing PVDF microporous membrane via TIPS method. The relation equations expressing the quantitative relationship between interaction parameter and phase separation temperature were deduced based on Flory–Huggins equation and solubility parameter theory. The unknown constants in the relation equations were solved out by fitting the binodal curve with cloud points in phase diagram. The binodal curves of PVDF/mixed diluent systems with different diluent compositions were calculated according to the relation equations. The compositions possible to yield bicontinuous structure inside microporous membrane were predicted in phase diagram. Finally, the hollow fiber membrane with interconnected sponge-like structures was prepared successfully from the predicted system (PVDF 12.74%, DOP 58.44 …