Multilayer Ti3C2(MXene) as a carrier was prepared using hydrofluoric acid as an etchant and Ti3AlC2 as raw material, Ni/Ti3C2 with Ni loading (mass fraction of Ni in the catalyst, same as the whole text) of 5%~20% was prepared by a KBH4 reduction method. The structural composition, morphological features and surface properties of Ni/Ti3C2 were characterized by XRD, FTIR, SEM, N2 adsorption-desorption, NH3-TPD, etc, and the catalytic performance of Ni/Ti3C2 for selective hydrogenation of cinnamaldehyde with different Ni loadings was investigated. The results showed that 10Ni/Ti3C2 with 10% Ni loading exhibited the best catalytic performance, and its Ni metal particles uniformly loaded on the surface of Ti3C2 with a well-defined layer structure and a specific surface area of 9.6 m2/g, exhibited the smallest average metallic Ni particle size (43.59 nm) and the highest dispersion (0.21%); The specific surface area and acid site strength of Ni/Ti3C2 increased gradually with increasing Ni loading in the range of 5% to 20%, with little change in the types of acid sites on the surface, 10Ni/Ti3C2 exhibited strong Lewis acid sites (NH3 desorption peak at approximately 511 °C) and good thermal stability. 0.5 g of 10Ni/Ti3C2 for selective hydrogenation of cinnamaldehyde reaction for 3 h under the conditions of 1.0 g cinnamaldehyde, reaction H2 pressure of 2.0 MPa, 30 mL of isopropanol as solvent, and reaction temperature of 120 °C, the cinnamaldehyde conversion and hydrocinnamyl alcohol selectivity were 100% and 99.29%, respectively. In five cycles, 10Ni/Ti3C2 showed high catalytic stability, 100% cinnamaldehyde conversion and 99.29%~92.07% hydrocinnamyl alcohol selectivity.