The major sources of waste from aquaculture operations emanates from fish or shellfish processing and wastewater generation. A simple technique called coagulation/flocculation utilizes biowaste from aquaculture to produce chitosan coagulant for wastewater treatment. A chemical method was applied in the present study for chitin and chitosan extraction from carapace of Macrobrachium rosenbergii and subsequent application for removal of turbidity and salinity from shrimp aquaculture wastewater. Box-Behnken in RSM was used to determine the optimum operating conditions of chitosan dosage, pH, and settling time, after which quadratic models were developed and validated. Results show that 80 g of raw powder carapace yielded chitin and chitosan of 23.79% and 20.21%, respectively. The low moisture (0.38%) and ash (12.58%) content were an indication of good quality chitosan, while other properties such as water-binding capacity (WBC), fat-binding capacity (FBC), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscope (SEM) confirmed the structure and the α-group, as well as the rough morphology of chitosan. In addition, the high solubility (71.23%) and DDA (85.20%) suggested good coagulant potentials. It was recorded in this study that 87.67% turbidity was successfully removed at 20 mg/L of chitosan dosage and 6.25 pH after 30 min settling time, while 21.43% salinity was removed at 5 mg/L of chitosan dosage, 7.5pH, and 30 min settling time. Therefore, the process conditions adopted in this study yielded chitosan of good quality, suitable as biopolymer coagulant for aquaculture wastewater treatment.