A novel and inexpensive adsorbent was prepared from sugar scum for the removal of methylene blue as an organic pollutant from aqueous solutions. The response surface methodology was used to study the effects of the calcination temperature and time on the yield and the methylene blue adsorption. In order to determine the optimal conditions of the preparation, the Doehlert design and desirability function were applied. The increase in calcination temperature increases the methylene blue adsorption and induces a reduction in yield. The optimal conditions have been identified to be a calcination temperature of 986°C and calcination time of 61 min. The characteristics of the obtained adsorbent were determined using SEM/EDX, and surface functions were obtained based on FTIR and pH pzc. The produced adsorbent had a porous structure and a pHpzc of 12.5. The results showed that the yield was 49.74% and the adsorption of methylene blue was 24.52 mg·g −1 with a contact time of 10 h determined by kinetic test. The sugar scum was found to be an effective material for the preparation of appropriate adsorbent for dye removal from wastewater.