NiCoAl layered double hydroxide (NiCoAl LDH) and multiwalled carbon nanotubes (CNTs) were successfully self‐assembled to generate a three‐dimensional CNTs‐NiCoAl LDH hybrid by means of a urea‐hydrolysis method. The scanning electron microscopy observations revealed that the hybrid was composed of both “core/shell” and flower‐like nanostructure. Composites of poly(ethylenes‐co‐vinyl acetate) (EVA) with CNTs‐NiCoAl LDH were prepared by melt blending. Their flammability performance and smoke toxicity were evaluated. CNTs‐NiCoAl LDH was found to be an efficient additive to improve the flame retardancy of EVA and reduce the smoke toxicity by suppressing the emission of carbon monoxide (CO). The physical properties of the char were believed to be critical in improving the flame retardancy. The remarkable reduction in smoke toxicity of EVA upon CNTs‐NiCoAl LDH was probably attributed to the combined effects of adsorption and catalysis on the oxidation of CO. POLYM. COMPOS., 39:E835–E841, 2018.
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