Polystyrene/poly(butyl acrylate) dispersion with N‐methylol groups were prepared through two ‐ steps semi continuous emulsion polymerization, where N‐methylol acrylamide (NMA) was used as a functional monomer. A high content of insoluble portions depending on the NMA dosing during polymerization was found in films casted from such dispersions. The crosslinking reactions between methylol groups during polymerization were assumed. Attenuated total reflectance Fourier transform infrared spectroscopy was used to study changes in films prepared from the functionalized and unfunctionalized dispersions. Comparison of the spectra of as‐dried films and heat‐ treated films suggests the occurrence of post‐polymerization crosslinking.
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