The paper covers the synthesis and characterization of cellulose derivatives from waste cellulose, namely, towel wastes. For this purpose, the cellulose acetate derivatives were synthesized from towel waste by applying the conventional chemical synthesis process. To clarify the structure of synthesized materials, some spectroscopic methods (FT-IR, XRD, 1 H-NMR, 13 C-NMR) were used. Furthermore, thermal behavior and surface morphology of prepared materials were investigated by DTG-TG and SEM, respectively. It was found that the degree of substitution values decreased as the duration of hydrolysis increased in cellulose diacetate synthesis. It was also understood that cellulose diacetate was dissolved in acetone differently from cellulose triacetate. Degree of substitution values of cellulose diacetate were compared by using 1 H-NMR and titrimetric method. These helped elucidate the expected reaction. The proposed method was easy compared with the conventional method.