Alkali lignin, a significant waste resource from the pulp and paper industry, is produced in large quantities each year, but its utilization remains limited. This study focuses on the cleavage of −OCH 3 groups attached to the aromatic ring in alkali lignin to obtain demethylated alkali lignin nanospheres (DAL-NPs) enriched with aromatic hydroxyl (Ar−OH) groups. These DAL-NPs are intended for the efficient adsorption of NH 3 . Qualitative and quantitative characterization of alkali lignin, both pre-and post-demethylation, was performed using Fourier transform infrared spectroscopy and 1 H NMR. The analysis revealed a reduction in methoxy groups and an increase in Ar−OH groups in the DAL-NPs. The NH 3 adsorption experiment demonstrated that the DAL-NPs exhibited a rapid and high adsorption capacity, reaching an NH 3 uptake capacity of 10.0 mmol g −1 within 0.42 min at 298 K and 1.0 bar. In addition, the DAL-NPs displayed superior selectivity based on the ideal adsorption solution theory for 10% NH 3 /90% N 2 (3252) and 10% NH 3 /90% CO 2 (175) at 298 K and 1.0 bar. The DAL-NPs also demonstrated reversibility and stability during 10 adsorption−desorption cycles. The DAL-NP adsorbent possesses exceptional properties, such as abundance and low cost, rapid and efficient adsorption, reversibility, and stability, making it a promising solid adsorbent for effective NH 3 adsorption in the ammonia process.