Experimental model validation for n-propyl propionate synthesis in a reactive distillation column coupled with a liquid–liquid phase separator

In the synthesis of some organic esters, reactive distillation coupled with a liquid–liquid phase separator is often used to increase the product purity or to recover the reactants. In this article, we present a comprehensive experimental and theoretical study on the heterogeneously catalysed synthesis of n-propyl propionate by reactive distillation and a subsequent liquid–liquid phase separator. The experiments were performed in a pilot-scale reactive distillation column. Data-reconciliation tests proved that the experimental results obtained comprise a complete, reliable set of composition and temperature profiles along the pilot-scale reactive distillation column and can be used for further model validation. A nonequilibrium-stage model was applied to predict the experimental results. Simulation studies demonstrated that the composition and temperature profiles in the rectifying section of the column were highly sensitive to the composition of the reflux stream entering the column. Deviations between the experimental and predicted composition profiles in the rectifying section were identified. An explanation for the deviations is given in this article.

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► No side-products, like di-n-propyl ether, were detected in all experiments.
► Conducted experiments provide reliable experimental data for model validation.
► Column profiles are highly sensitive to the composition of the reflux stream.