Summary: The hydrotalcite‐catalyzed synthesis of PET was studied to clarify the effect of hydrotalcite properties on its catalytic activity. Hydrotalcite was modified by various treatments to tune its activity as a polycondensation catalyst. Hydrotalcite activity was found to decrease upon calcination. However, rehydration of the calcinated hydrotalcite resumed the catalytic activity. The hydrotalcite activity depends on the ratio of magnesium to aluminum cations in its composition, and highest activity occurs at a molar ratio of 2:1. Replacement of the carbonate anions of hydrotalcite by more nucleophilic ones like hydroxide and alkoxide groups resulted in improved catalytic activity. Hydrotalcite has two assembly orders: primary lamination of sheets into plates and secondary agglomeration of plates into particles. Hydrotalcite with larger sheet size showed lower activity. On the other hand, milling of hydrotalcite particles did not affect its activity as it probably enters the reaction on a plate level, which is not affected by milling. Polycondensation resulted in expansion of the hydrotalcite sheets under the effect of formed polymer. Reuse of hydrotalcite after polycondensation followed by depolycondensation resulted in a large activity enhancement.High‐resolution SEM micrograph of calcinated HT after rehydration.magnified imageHigh‐resolution SEM micrograph of calcinated HT after rehydration.
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