Zeolite analcime (EMANA) was synthesized through the hydrothermal method by using carbothermal reduction electrolytic manganese residue (CR-EMR). The structural properties of EMANA and CR-EMR were studied using various characterization techniques. After hydrothermal synthesis, the CR-EMR became super-microporous, and the surface area increased by 4.76 times than before. Among the various synthesized zeolites, 6 h-synthesized EMANA was selected as the best adsorbent for macrolide antibiotics in aqueous solution. The adsorption performance of EMANA on the adsorption capacity was examined by using various experimental parameters, such as contact time (0–24 h), initial concentration (50–300 mg/L), temperature (30–50 °C) and pH (3–13). The experimental results were also analyzed by the Langmuir and Freundlich adsorption models, with the latter obtaining better representation. The adsorption process could be described well by the pseudo-second-order model, even under a low concentration (50 mg/L). This result suggests that the adsorption process of macrolide antibiotics is due to chemisorption. According to the Fourier Transform infrared spectroscopy (FT-IR) results, the adsorption of zeolite was mainly due to its hydroxyl group, which played an important role during the adsorption process. Moreover, EMANA is more suitable for treatment of roxithromycin (ROX) than azithromycin (AZM), because ROX has more adsorption sites for the hydroxyl group.