Microcapsules of cellulose acetate with Cyanex 923 were prepared and used in this study for phenol removal from water and synthetic textile wastewater. The influence of several factors on the microcapsules extraction efficiency was studied, as well as characterization and phenol adsorption isotherm. Microcapsules characterization demonstrated the extractant reagent encapsulation, while in a batch mode procedure, good adsorption of phenol (ca. 5.5 × 10−3 mol Kg−1) has been reached. A slight decrease in phenol extraction percentage was obtained when synthetic textile wastewater was used (ca. 4.955 × 10−3 mol Kg−1), although a decrease in color was observed due to dye microcapsule extraction. Results indicate that this method is a promising alternative to conventional phenol removal technologies for aqueous samples of low phenol concentrations or in textile effluents.