In-situ activation of Pd-TUD-1 during the selective reduction of 1,5-Cyclooctadiene (cas 111-78-4)

Add time:08/20/2019    Source:sciencedirect.com

Here, different loading of palladium (Pd), ranged from 0.5 to 5 wt%, was incorporated into the three dimensional siliceous mesoporous material; TUD-1. The synthesis procedure was carried out without the use of solvents, surfactants, and/or copolymers. Only triethanolamine and water with the precursors of Si and Pd were applied in one-pot synthesis procedure to prepare Pd-TUD-1 materials. The prepared materials were characterized by means of elemental analysis, XRD, Raman spectroscopy, N2 sorption measurements, SEM and TEM. Characterization data confirmed the formation of PdO particles inside the pores of TUD-1 matrix, moreover bulky PdO particles were also detected as an extra-framework separated phase in the high loading samples. The prepared samples were divided into two batches, the first was activated by hydrogenation at 300 °C for 3 h, and the second batch did not activated. The catalytic activity of the two batches was examined in the selective hydrogenation of 1,5-cyclooctadiene (COD) at 80 °C under solvent-free condition to produce cyclooctene (COE). The obtained results showed that the samples of the two batches were able to catalyze the reaction with a very comparable activity. The non-hydrogenated sample with a 0.5% Pd gave 98.5% COD conversion with a COE selectivity of 92.8%, while the same sample which pre-hydrogenated gave 96.8% of COD conversion and 93.5% selectivity towards COE. The characterization of the used catalysts confirmed that PdO was in-situ reduced to Pd nanoparticles during the reaction.

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