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Carboxymethylcellulose (CMC) acts as a coating material for a magnesium-layered hydroxide-3-(4-methoxyphenyl)propionate (MLH-MPP) nanocomposite via spontaneous self-assembly. The resulting product is called a magnesium-layered hydroxide-3-(4-methoxyphenyl)propionate/carboxymethylcellulose (MLH-MPP/CMC) nanocomposite. The XRD pattern of the MLH-MPP/CMC nanocomposite showed that MPP was maintained in the interlayers of the MLH, thus confirming that CMC is only deposited on the surface of the MLH-MPP nanocomposite. These findings were also supported by FTIR spectra, SEM and TEM. TGA data showed that the thermal stability of the intercalated MPP was significantly enhanced compared to pure MPP and uncoated nanocomposite. The release of MPP from the interlayers of MLH-MPP/CMC nanocomposite showed slower release than did uncoated nanocomposite and followed pseudo–second-order kinetics. Since the herbicide, MPP was released from the synthesised nanocomposite in a sustained manner, thus, it has excellent potential to be used as a controlled-release herbicide formulation. Keywords: Magnesium-layered hydroxide, 3-(4-Methoxyphenyl)propionic acid, Carboxymethylcellulose, Direct reaction method, Controlled release