One of the most challenging emerging pollutants to deal with, particularly in wastewater, is residual surfactants such as nonylphenol ethoxylate-10 (NP10EO). The capacity of advanced oxidation processes, especially Fenton-like reactions, to break down organic pollutants into safer compounds and manageable quantities makes them highly desirable techniques in wastewater treatment research. The purpose of this study was to explore the degradation efficiency of NP10EO using the synthesized iron-impregnated nipa bark biochar (Fe@NBBC) composite catalyst and utilizing sodium percarbonate as an oxidant. SEM, XRF, and FTIR were used to examine the synthesized Fe@NBBC. The Fe@NBBC’s effective synthesis was validated by these analyses. A three-level, two variables (32) full factorial design of experiments was used to determine the effects of Fe@NBBC catalyst loading, and initial NP10EO concentrations on the removal of NP10EO. Higher Fe@NBBC catalyst loadings and lower initial NP10EO concentrations yielded higher NP10EO. A maximum of 85.37% NP10EO degradation can be achieved when 150 mg L−1 Fe@NBBC catalyst loading, 10 mg L−1 initial NP10EO concentration, addition of 1 mmol L−1 SPC, and solution adjusted at pH = 3 are utilized. These results prove that the use of Fe@NBBC catalyst to degrade NP10EO in aqueous solutions through a Fenton-like process is effective.