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Cellulose nanofibrils (CNFs) were exposed to the same levels of potassium chloride (KCl) and sodium chloride (NaCl) before being subjected to spray drying. The effect of NaCl and KCl on the size of atomized droplets and the hydrogen bond retardation between CNFs was investigated by characterizing product morphology, particle size distribution, dispersion stability in aqueous system, and surface chemistry. The results showed that the CNF suspensions treated with KCl could be atomized into smaller droplets during spray drying, and then CNF powder with smaller sizes could be obtained. As the agglomeration was less, and the CNF with KCl addition had good dispersion stability after redispersion compared with CNF treated by NaCl. Therefore, KCl treatment was an effective method to reduce the agglomeration of CNF during spray drying.