This study aims to compare the influence of processing techniques and procedures on the morphology and mechanical properties of polyvinyl chloride (PVC) nanocomposites. PVC nanocomposites with 5 phr montmorillonite (MMT) clay were prepared on a two-roll mill or in a microcompounder, both were either processed once or via a masterbatch containing 20 phr MMT. The MMT was treated with non-ionic surfactants and analysed by thermo gravimetric analysis and X-ray diffraction prior to being added. The final composites were analysed and tested using X-ray diffraction, scanning and transmission electron microscopy (SEM/TEM), tensile test, and Charpy impact test. The dispersion was found to be best in the roll milled samples prepared via the masterbatch and the elongation at break and impact strength was also better for the roll milled samples. E-modulus and tensile strength, on the other hand, were significantly better for the microcompounded samples despite the larger particle size. This can be explained by a higher degree of orientation in these samples. Finally, it must be stated that the change in properties are not satisfactory. Although we see an increase in E-modulus, the decreased impact properties are not acceptable. The main reason for this is the lack of compatibility between the clay particles as observed by high resolution SEM.