The polymer diallyldimethylammonium chloride-acrylamide-glyoxal/montmorillonite nanocomposites (PDM-AM-GL/MMT) were prepared by using polymer diallyldimethylammonium chloride-acrylamide/montmorillonite nanocomposites (PDM-AM/MMT) and glyoxal. The PDM-AM/MMT nanocomposites were synthesized via in situ polymerization method. The PDM-AM/MMT nanocomposites and PDM-AM-GL/MMT nanocomposites were studied by using percent conversion, characteristic viscosity of the polymer, and system rotational viscosity of nanocomposites, respectively. Increasing dose of MMT, percent conversion in nanocomposites system rotational viscosity of nanocomposites is increasing. When MMT dose is increasing up to 3% or 4%, they are decreasing. The characters of the PDM-AM/MMT and PDM-AM-GL/MMT were determined by FT-IR and XRD. FT-IR results show that MMT and polymer could separate successfully by centrifugal method. XRD results indicate that the laminar distance of MMT in nanomaterial was reached the biggest when the dosage of MMT was used 4%. Nanocomposites were applied in leather making and physics mechanical of performance of the resultant leather was measured.