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Kaolinite nanoscrolls (NScs) are halloysite-like nanotubular structures of great interest due to their ability to superimpose halloysite’s properties and applicability. Especially attractive is the ability of these NScs to serve as reaction vessels for the uptake and conversion of different chemical species. The synthesis of kaolinite NScs, however, is demanding due to the various processing steps that lead to extended reaction times. Generally, three intercalation stages are involved in the synthesis, where the second step of methylation dominates others in terms of duration. The present research shows that introducing microwave processing throughout the various steps can simplify the procedure overall and reduce the synthesis period to less than a day (14 h). The kaolinite nanoscrolls were obtained using two final intercalating agents, aminopropyl trimethoxy silane (APTMS) and cetyltrimethylammonium chloride (CTAC). Both produce abundant NScs, as corroborated by microscopy measurements as well as the surface area of the final products; APTMS intercalated NScs were 63.34 m2/g, and CTAC intercalated NScs were 73.14 m2/g. The nanoscrolls averaged about 1 μm in length with outer diameters of APTMS and CTAC intercalated samples of 37.3 ± 8.8 nm and 24.9 ± 6.1 nm, respectively. The availability of methods for the rapid production of kaolinite nanoscrolls will lead to greater utility of these materials in technologically significant applications.