Summary: The first aim of this work was to study the solid‐state copolymerization (SSP) of bis(2‐hydroxyethyl)terephthalate (BHET) with poly(butylene terephthalate) (PBT) by FTIR spectroscopy. The development of the chemical microstructure during the SSP‐reaction was examined as a function of the BHET content, showing the different regimes. The thermal behaviour of the resulting copolymers with different BHET contents was also investigated during cooling using infra‐red dynamic spectra. For low BHET‐concentrations, only crystallization of PBT‐sequences was observed, while for high BHET‐concentrations, only crystallization of PET‐sequences was detectable with a cross‐over behaviour for intermediate concentrations.
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