Abstract: Amide-t-butylcalix8 arene/polyacrylonitrile nanofiber was prepared by electrospinning technique using dimethylformamide as solvent. When the acidity of the Cu²⁺ containing solution was pH 4.7, and the temperature of the solution was 35℃, the nanofiber showed its best adsorption capacity for Cu²⁺. The adsorption behavior of the nanofiber toward Cu²⁺ was found to comply with both the Langmuir adsorption isothermal model and the Freundlich adsorption isothermal model.