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Continuous flow reduction of 4-nitrophenol by “water soluble” palladium nanoparticles: from batch to continuous flow system

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Abstract

Process intensification research is concentrated on the use of the continuous flow microreactor over the conventional batch reactors due to the various advantages that bring this latter in terms of efficient micromixing and enhanced heat and mass transfer in small residence time. The continuous flow process has been successfully developed for many common reactions in the pharmaceutical and chemical industries. This paper explores the catalytic performance of Pd nanoparticles (NPs) in a continuous flow mode and studies different microreactors configuration, and their applications on the benchmark reaction model of 4-nitrophenol reduction in aqueous media by using sodium borohydride as a reducer. A PTFE Spiral Capillary Microreactor (SCM) was designed and compared to a Continuous Vessel Microreactor (CVM) for the reduction of 4-Nip into 4-Amp. Multiple equations were obtained from different microreactor configurations that can be used for the calculation of theoretical mean conversion and 4-nitrophenol concentration at the outlet of the microreactor. The kinetics studies of this reaction model already determined in batch reactor were confirmed by using pseudo-first order in continuous flow microreactor. The real microreactor (SCM) is acting as a plug flow reactor (PFR). The engineering aspects such as reaction conditions and microreactor model are discussed. This work studies the kinetics of the 4-Nip reduction for the first time with nanoparticles non supported in continuous flow. This work showed that the kinetic study of the reaction can be carried out successfully in SCM and advantageously in particular for short reaction times.

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Authors and Affiliations

  1. Laboratoire TIMR, EA4297, Centre de Recherche de Royallieu, Sorbonne Universités - Université de Technologie de Compiègne, rue du docteur Schweitzer, CS 60319, 60203, Compiègne cedex, France

    A. Iben Ayad, E. Guenin & A. Ould Dris

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  1. A. Iben Ayad
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  2. E. Guenin
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  3. A. Ould Dris
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Contributions

A.I. conceived and designed the experiments; A.I. performed the experiments and analyzed the data; A.I., A.O., and E.G., provided the concept of this research and managed all the experimental and writing process as the corresponding authors; all authors discussed the results and commented on the manuscript.

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Correspondence to A. Ould Dris.

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Highlights

- Kinetics study of nitro-phenol reduction in the presence of Pd nanoparticles can be performed successfully in a PTFE Spiral Capillary Microreactor.

- Since the reduction of nitrophenol is a pseudo first order reaction, this work has confirmed that a reactor close to the plug reactor (PR) is giving a higher conversion than a reactor that is close to a continuously stirred tank reactor (CSTR)

- The experimental results with PTFE Spiral Capillary Microreactor are close to those of plug reactor model in comparison to those of the laminar flow reactor model even if the flow is taking place in the laminar flow regime.

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Iben Ayad, A., Guenin, E. & Ould Dris, A. Continuous flow reduction of 4-nitrophenol by “water soluble” palladium nanoparticles: from batch to continuous flow system. J Flow Chem 12, 101–111 (2022). https://doi.org/10.1007/s41981-021-00194-x

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  • DOI: https://doi.org/10.1007/s41981-021-00194-x

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