This work investigates removing the anionic azo dye from wastewater using Fe3O4 magnetic nanoparticle adsorbents in a batch system. The effects of adsorbent dosage (0.1–0.5 g/L), pH (2−10), dye concentration (5–45 mg/L), contact duration (0–140 min), and shaking speed (100–180 rpm) on the removal (adsorption) efficiency at 23 °C were investigated. Besides the kinetic and isothermal studies were applied as well to improve commercial adsorbents’ performance in removing anionic dyes. Fe3O4 magnetic nanoparticles achieve a maximum azo dye removal (adsorption) efficiency of 99.99% at the optimum values of the investigated parameters: 3 g/L of adsorbent dose, 5 mg/L dye concentration, pH 2, and 180 rpm in 120 min at 23 °C. Langmuir adsorption isotherm has the highest correlation coefficient (R2 = 0.977) compared to Freundlich, and Temkin isotherms; the maximum absorption of azo dye is estimated to be 0.4158 mg/g. The values of the equilibrium parameter (RL) in the Langmuir isotherm model are between 0 and 1, indicating the Langmuir isotherm's favorability. The Fe3O4 magnetic nanoparticle adsorption rates follow pseudo-first-order adsorption kinetics, with R2 = 0.973.