Abstract: The Ni-P amorphous alloy was synthesized by chemical reduction, modified by adding element Co, and characterized by XRD, SEM, XPS and DSC. The hydrodeoxygenation (HDO) performance of the amorphous alloy was investigated by hydrodeoxygenation of vanillin to 2-methoxy-4-methylphenol (MMP). It is shown that the synergy between Ni and Co not only contributes to the reduction of Ni, increases the number of active centers of the catalyst, but also improves the dispersion, disorder and thermal stability of the amorphous alloy. Under the optimized reaction conditions:n_Co/(n_Co + n_Ni)=0.08 (molar ratio), H₂ partial pressure of 2.0 MPa, reaction temperature of 150℃, reaction time of 180 min, catalyst dosage of 0.05 g, vanillin conversion and the MMP selectivity can reach 100% and 82.7%, respectively. After 5 cycles of the catalyst, the conversion of vanillin remains 100% and the selectivity of MMP decreases to 68.7%.