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Firstly, hydrotalcite (HT) was synthesized by the urea method. Then, sodium methyl allyl sulfonate (SMAS) was used as intercalation agent to prepare intercalated HT (SMAS–HT). Finally, a novel poly(acrylic-co-acrylamide)/HT nanocomposite superabsorbent was prepared by inverse suspension polymerization, using N,N′-methylenebisacrylamide (NMBA) as a cross-linking agent and potassium persulfate (KPS) as an initiator. The morphology of the superabsorbents was characterized by FT-IR, XRD, SEM and TEM. The influences of the amount of SMAS–HT on the water (salt) absorbency were investigated. Results showed that the intercalation was successful and the intercalated SMAS–HT incorporated into the superabsorbent was completely exfoliated. The superabsorbent particles approach a spherical shape and the average size is 200–300 nm. The particle sizes of the superabsorbents decrease with increasing the content of SMAS–HT. In addition, the superabsorbent acquired its highest water (salt) absorbency when the content of SMAS–HT is 3 wt%. The highest absorbencies of the superabsorbent for deionized water and 0.9% NaCl(aq) were 900 g/g and 140 g/g, respectively. [ABSTRACT FROM AUTHOR]