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Nanocomposites of polystyrene (PS) with modified CoAl-layered double hydroxide (CoAl–LDH) were preparedviasimple solvent blending method and the effect of CoAl–LDH content on the structural and thermal properties was investigated. The structural and thermal properties of the nanocomposites were characterised by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The nano-scale dispersion of the CoAl–LDH layers in the PS matrix is verified by the (0 0 3) XRD reflection of the modified CoAl–LDH. The XRD data show that the exfoliated PS/CoAl–LDH nanocomposites can be obtained by controlling the LDH loading of about 5 wt%. TEM analysis also confirms the formation of exfoliated PS nanocomposites with 3 wt% and 5 wt% LDH loading. The thermal degradation temperature of the PS nanocomposite containing 5 wt% CoAl–LDH is found to be 12°C higher than that of pure PS when 50% weight loss is selected as a point of comparison. The glass transition temperature (Tg) of PS nanocomposites is about 14°C higher than that of pure PS. [ABSTRACT FROM AUTHOR]