Layered double hydroxides (LDHs) were synthesized and modified with different methods and also with different functional molecules. An easy and successful one-pot anion-exchange intercalation procedure was introduced and the influencing parameters of the modification were investigated in comparison to other modification methods. LDH based polymer nanocomposites were prepared with a microcompounder using melt-mixing method. The exfoliation behavior of organomodified LDHs was investigated with two different rheological models and visualized with electron microscopy techniques. Some of the relations between modification of LDH and the extent of exfoliation were identified. Highly exfoliated nanocomposites were successfully prepared after intercalation even with a small molecule like hexanesulfonic acid by performing the introduced anion exchange method. (C) 2014 Elsevier B.V. All rights reserved.