A two-step method combining colloid synthesis and incipient wetness impregnation was developed for the preparation of bimetallic Pd-Cu/γ-Al2O3 catalysts, with the aim of increasing the selectivity to styrene in the selective hydrogenation of phenylacetylene. The structural properties of the catalysts were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), CO-pulse chemisorption, N2 physisorption, and inductively coupled plasma atomic emission spectrometry (ICP-AES). The effects of changing the Cu/Pd molar ratio, the Pd loading, and the order in which the Pd and Cu were introduced into the catalysts on the catalytic activity and selectivity were investigated. The results showed that Pd-Cu/γ-Al2O3 exhibited much higher selectivity toward styrene than Pd/γ-Al2O3. In particular, Pd-Cu/γ-Al2O3 with a Pd loading of 0.3%(w) and a Cu/Pd molar ratio of 0.6 displayed excellent performance at 40 °C under 0.1 MPa H2, with a high selectivity of 95% at a conversion of 90%, and a selectivity of approximately 82%, even at conversions of higher than 99% . The increased selectivity of Pd-Cu/γ-Al2O3 was ascribed mainly to the 2315
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