The environmentally-friendly diacetate cellulose fibers with high specific surface area were prepared by similar procedure to dry spinning, in which diacetate cellulose was dissolved in dichloromethane/acetone blend solvent. The effect of mass fraction and solute ratio on the rheology properties of spinning solution was investigated. The morphology and specific surface area of the as-spun diacetate cellulose fibers were characterized by scanning electron microscope (SEM), 3D field microscope and BET. The experimental results show that the increase in the concentration of the spinning solution will contribute to an increased apparent viscosity, a decreased non-Newtonian index, and also an improved structural viscosity. In the case of blend solution system, when the ratio of dichloromethane is improved, the apparent viscosity as well as the surface tension is also increased. And when the concentration increases and the ratio of dichloromethane decreases, the porous structure is more difficultly formed.