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The correlation of the rheological and optical properties of solutions of cellulose acetate in acetone with the morphological characteristics of ultrafiltration membranes designed for removal of caprolactam from industrial sewage was investigated. It is shown that addition of dioxane, urea, and water to solutions of cotton cellulose acetate (cCA) and wood cellulose acetate (wCA) in acetone decreases the viscosity of the solution and dimensions and increases the number of microgel particles and yields more homogeneous membranes.