Lignin is the main polymers in woody biomass aside cellulose and hemicelluloses Recently, nano-lignin is gaining importance due to the increasing demand for bio-based and bio-active nanomaterial fillers for many applications such as in composite and textile industries. Palm oil mill effluent (POME) is the main wastewater produce by palm oil mills. Anaerobically treated (AT-POME) contains high soluble lignin due to the anaerobic digestion of cellulosic material in POME. Nano-lignin was precipitated by adjusting the initial pH of AT-POME during the sonication process. Sulfuric acid (H2SO4), nitric acid (HNO3), hydrochloric acid (HCl) and phosphoric acid (H3PO4) were used to adjust the initial pH of AT-POME. Result shows that sulfuric acid was the most suitable acid to be used as it could recovered 96% of the soluble lignin in AT-POME. The presence of ultrasonic during the precipitation process had reduced the size to 383.4 nm. The optimum operating parameter for lignin recovery is at pH 4 using sulfuric acid and sonicated at 80 watts for 15 minutes. This study shows that sonication could reduce the size of precipitated lignin from AT-POME. In addition, removal of lignin from AT-POME also reduced the COD content of AT-POME.