In the present study, ferrihydrite-chitosan nanocomposite (FCN) was successfully produced by co-precipitation method and used for the first time as a recyclable flocculant for pre-treatment of palm oil mill effluent (POME). The physicochemical properties of FCN were studied using Raman spectrometer, Scanning Electron Microscope (SEM) and Thermogravimetric Analyser (TGA). The feasibility of FCN to remove total suspended solids (TSS), turbidity, chemical oxygen demand (COD), and, oil and grease (O&G) from POME was investigated using a jar test method. The optimum conditions for contaminant removal from POME were determined by varying the experimental parameters such as flocculant dosage, solution pH and settling time. The results obtained showed that FCN, at a dosage of 1.5 g/L, a contact time of 60 min and pH of 5.0 gave a highest reduction of turbidity, TSS, COD and O&G levels by 72.38%, 77.32%, 71.60% and 53.40%, respectively. Besides that, FCN exhibited a better flocculation performance as compared to alum and chitosan. After three cycles of flocculation/deflocculation process, FCN retained satisfying flocculation efficiency and flocculants recovery in the range of 80-83% and 43.2-78.6%, respectively. Combination of charge neutralisation and polymer bridging was the main key mechanism of interaction between FCN and POME contaminants. The synergy effect between iron oxide/oxyhydroxide nanoparticle and chitosan has increased the physicochemical properties and flocculation performance of the FCN nanocomposite. Overall, FCN nanocomposite can be used an alternative flocculant for POME treatment.