A novel and simple method to synthesize supported Ni2P/Na(x)-MCM-41 catalysts (where x is the mass fraction of Na-to-MCM-41 in terms of percentage) at a lower reduction temperature by incorporation of Na was described. The catalysts were characterized by H2 temperature-programmed reduction (H2-TPR), X-ray diffraction (XRD), N2 adsorption–desorption, CO uptake, X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The effect of Na on the structure of catalysts and catalytic properties for the dibenzothiophene (DBT) hydrodesulfurization (HDS) was investigated, which confirmed that a suitable amount of Na can promote highly dispersed Ni2P particles. The Na preferentially interacts with phosphate to generate the sodium phosphate and therefore suppresses the formation of stronger P–O–P bonds, which enables the phosphide catalyst to be easily formed at a lower reduction temperature. Compared with conventional phosphate (973–1273 K), the reduction temperature of Ni2P/Na(x)-MCM-41 catalyst was relatively low (773 K). The Ni2P/Na(x)-MCM-41 catalyst with x = 1.0 showed the maximum DBT conversion of 91.6%, which is higher than that of Ni2P/M41 without Na (80.3%).
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