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Procedures for the preparation of methyl cellulose/montmorillonite (MC/MMT) nanocomposite films were optimized by testing 30 procedures including differences in type of mixing, speed of mixing and time of mixing. The characterization of films by XRD and TEM indicated that a procedure involving mixing by a homogenizator was the most suitable nanocomposite film preparation method. The effect of MMT concentration on some properties of MC/MMT nanocomposite films was also investigated. It was found that the increase in the MMT concentration caused an increase in the film thickness and opacity values of MC/MMT nanocomposite films, whereas the increase in MMT concentration led to a decrease in their water adsorption and water solubility.