Abstract
This Letter reports an experimental study which achieves reproducible oscillations in both pH and heat output (Qr) during a palladium-catalysed phenylacetylene oxidative carbonylation reaction in an homogeneous catalytic system (PdI 2–KI–Air–NaOAc in methanol solution). Experiments were performed in an HEL SIMULAR™ reaction calorimeter with precise control of temperature and gas flow rates. Under certain experimental conditions a second set of oscillations was observed. Oscillations in Qr were exothermic with no corresponding endotherm. Total energy released during oscillations followed a staircase function with a maximum of 600 J/oscillation. Heat release was in phase with pH fall, and decreased as pH increased.
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