A metallosurfactant catalyst was developed to address the requirements for the utilization of low-molecular-weight carboxylic acids from dilute effluents. The catalyst Ni­(DBSA)2 combines transition-metal catalysis of nickel ions and surfactant catalysis of 4-dodecylbenzenesulfonic acid (4-DBSA). Requirements for the metallosurfactant catalyst are low water solubility, high catalytic activity in biphasic esterification, and self-assembling properties at the interface. Ni­(DBSA)2 was tested for applicability in the interfacial catalysis of esterification of dilute acetic acid with the solvent 1-octanol and resulted in an octyl acetate yield of 31.3%. Under identical reaction conditions, Ni­(DBSA)2 performed better than sulfuric acid with a yield of 1.7%. The limited catalytic performance of sulfuric acid is caused by the presence of sulfuric acid mainly in the aqueous phase. In contrast, Ni­(DBSA)2 is dissolved in the solvent and assembles at the aqueous/solvent interface where the reaction takes place. Additionally, the metallosurfactant lowers the interfacial tension between 1-octanol and deionized water by up to 75%, thus enhancing mass transfer. Compared to catalysis with 4-DBSA in emulsion, the catalytic performance of Ni­(DBSA)2 dropped by 62%, but this drawback is compensated by the complete suppression of emulsification. With Ni­(DBSA)2, the development of a catalyst was achieved, which self-enhances its catalytic performance in the interfacial catalysis through increased mass transfer area due to its surfactant properties.