Collect. Czech. Chem. Commun. 1997, 62, 1763-1775
https://doi.org/10.1135/cccc19971763

Deactivation of Polymer-Supported Palladium Catalystsin the Hydrogenation of 4-Nitrotoluene

Roman Fišeraa, Milan Králika, Julius Annusa, Vieroslav Krátkya, Marco Zeccab and Milan Hroneca

a Department of Organic Technology, Slovak Technical University, 812 37 Bratislava, Slovak Republic
b Dipartimento di Chimica Inorganica, Metallorganica e Analitica, via Marzolo 1, 35131 Padova, Italy

Abstract

The deactivation of palladium catalysts supported on commercially available sulfonated polystyrene-divinylbenzene resins (DOWEX) in the hydrogenation of 4-nitrotoluene was studied. Catalysts were prepared from 4 and 8 mole % crosslinked polymers, with particle size between 0.04 and 0.80 mm and palladium contents ranging from 0.25 to 1 wt.% (dry state). The catalytic tests were carried out in a batch reactor vigorously shaken, at 30-50 °C, and 0.25 and 0.5 MPa. The analysis of the conversion curves showed that three factors are mainly responsible for the relatively high deactivation rates: (i) the concentration of hydrogen in the neighbourhood of palladium crystallites, (ii) temperature, (iii) the nanomorphology of the support. Some practical advice concerning the employment of polymeric hydrogenation catalysts and relevant operational conditions can be achieved from the results presented herein.

Keywords: Hydrogenation; 4-Nitrotoluene; Ion-exchange polymers; Polymer-supported palladium catalysts; Catalyst deactivation.