is research employed a novel and facile approach called nanoclay aerogel masterbatch.. is innovative technique was conducted by attaching the clay layers directly onto a mobile polymer, for example, polyethylene glycol (PEG), in order to modify the clay layer through PEG-clay intercalation and PEG-hydrogen bonding. is state was maintained with a small amount of the anionic polymer hydrogel, for example, kappa-carrageenan (KC), and turning it into a highly porous and fragile structure by freeze-drying, thus a so-called nanoclay aerogel masterbatch. e facile nanoclay aerogel masterbatch was able to be attained even at high clay loadings (55-67 wt.% of the inorganic clay content) with constant PEG and KC loadings. e interlayer spacing enlargement of the nanoclay galleries was around 17Å with the typical lamellar morphology like a house of cards structure. e density values were within 0.108-0.122 g·cm −3 . e thermal stabilities were up to 270°C, revealing better thermal stability for melt mixing with the commodity plastics at a high melting temperature. e flowability and processability were certified by the melt flow index (MFI) results. e highest nanoclay loading capacity (67 wt.%) of the achieved nanoclay aerogel masterbatch was selected to prepare PS-clay nanocomposites via a melt-mixing process. e comparative nanocomposites were produced by using organoclay. e results of the X-ray diffraction (XRD) and transmission electron microscopy (TEM) exhibited that the exfoliated morphologies were obtained at all clay contents (1-3 wt.%); however, the intercalated structure was gained by using organoclay.e outstanding transparency and brightness were remarked from the specimens prepared by using the nanoclay aerogel masterbatch. e brownish specimens were observed by using organoclay. e significant improvements of tensile properties, glass transition temperature (T g ), and thermal stability were noticed from the nanocomposites prepared using the nanoclay aerogel masterbatch.