Taguchi method was applied to optimize process parameters for the removal of Congo red (CR) dye from aqueous solutions by batch adsorption experiments. The L-18 (3(5)) orthogonal array was chosen for carrying out experimental trials. The selected parameters include initial solution pH, adsorbent dose, initial dye concentration, contact time, and adsorbent type. Signal-to-noise ratio and variance analysis were used to determine optimum removal conditions and significant operating parameters, respectively. The results showed that initial dye concentration, adsorbent dose, adsorbent type, and contact time were the significant parameters for CR removing with contribution percentages of 61.72%, 32.99%, 2.25%, and 1.18%, respectively. Under optimal conditions, the adsorption kinetic data fitted well to pseudo-second-order model.