Nanocrystalline cellulose (NCC) was prepared from Agave tequilana Weber blue variety via acid hydrolysis. The NCC was used in forming acrylic acid/acrylamide hydrogels (AA/AM), (80/20 w/w), crosslinked with N-N-methylene bisacrylamide (MBA) at addition levels of 1, 2, 4, and 8 wt% of the monomeric phase. The NCC was dosed at 0.1, 0.5, and 1.0 wt%. Two synthesis routes were used. In the first route, polymerization was performed immediately after mixing the components. In the second route, the mixture of the components was kept at 2 °C ± 1 °C for 24 h before the polymerization (thermal treatment). All the hydrogels were characterized by nuclear magnetic resonance (NMR), water absorption tests, scanning electron microscope (SEM) analysis, and rheology tests. The NCC particles had a diameter of approximately 75 nm. The hydrogels that were subjected to the thermal treatment reached the equilibrium after approximately 72 h. The un-treated hydrogels reached the equilibrium after approximately 58 h. The thermally treated samples had a lower swelling degree and the swelling degree decreased as the crosslinking degree and the NCC concentration increased. The swelling kinetics followed the Schott´s pseudo-second-order.