This study presents a new, sustainable, high-pH recirculating batch process for the regeneration of NH4+-laden cation exchange resins, while recovering the ammonia as a pure, reusable, solid salt (NH4Cl). The process efficiently recycles a minimal volume of regeneration solution while reducing NaCl consumption between cycles. The regeneration solution, containing a high concentration of NaCl maintained at high pH (pH > 11) allows Na+ to replace the desorbed NH4+, which, due to the high pH, completely transforms into NH3. Real time pH monitoring of the regeneration solution and the column effluent provided accurate tracking of the regeneration rate and allowed concise endpoint determination. Ammonia was recovered by evaporation of the exhausted regeneration solution followed by sublimation (and thereafter deposition) of NH3 and HCl, which produced pure NH4Cl salt.The optimal working conditions for the cation exchange regeneration were identified as 1 M NaCl, pH 12.0, and regeneration solution volume of 1 bed volume. Single-column application of six adsorption-regeneration cycles (no zeolite replacement) showed that the process conditions do not degrade the resin’s adsorption performance. Cost assessment of two possible ammonia recovery options indicated that while stripping NH3 from the regeneration solution and reabsorbing it in an acidic solution is operationally easier, the sublimation-based approach yields a more valuable product. For an optimized sublimation approach, a low regeneration solution volume, combined with a high resin capacity for NH4+, are essential.This process demonstrates a sustainable solution for ammonia salt recovery from wastewater, offering a circular approach that does not only add an important control to the regeneration step, but also harvests ammonia as a reusable product.
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