Rice starch was used as an adsorbent to adsorb the dyeing wastewater simulated by methylene blue in mini-hydrocyclone. The single experiments were used to explore the effect of starch concentration, split ratio and feed flow rate on the efficiency of adsorption and separation. Moreover, the response surface analysis method was used to optimize process parameters. The results showed that the starch concentration, split ratio and feed flow rate all influenced the efficiency of adsorption and separation. The order of effect on adsorption efficiency was as followed: starch concentration > split ratio > feed flow rate, and the order of effect on separation efficiency was as followed: split ratio > Feed flow rate > starch concentration. The optimal parameters condition obtained by response surface method was as followed: starch concentration was 1.0%, split ratio was 19%, and feed flow rate was 1 080 kg/h. Under the control of these conditions, the efficiency of adsorption and separation was 69.2% and 74.3%, respectively.