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[Display omitted] • Hollow carbon nanoalloy catalysts were applied to water–oil biphasic systems for phenol hydrogenation. • The formation of NiCo alloys reduces the electron cloud density of Ni species and promotes intermetallic interactions. • The bent structure of the carriers induces metal-carrier interactions that lead to the transfer of electrons from the inner concave surface to the outer convex surface. • The NiCo NPs on the inner surface are in an electron deficient state, which contributes to the planar adsorption of phenol and the rapid generation of active H. Metal hollow carbon nanocatalysts have attracted much attention in the field of catalytic hydrogenation due to their unique hollow structures. In this paper, 5%Ni15%Co@HCS with hollow structure was constructed by soft-template method, which achieved efficient hydrogenation of phenol in biphasic solvent within 1 h and has good potential for industrial application. Both alloying effects and metal-carrier interactions affected the electronic structure of Ni and Co. The formation of Ni-Co alloys was promoted by adjusting the appropriate metal ratios, which reduced the electron cloud density of Ni species and promoted metal–metal interactions. Meanwhile, the bending structure of the carbon spheres induced the metal-carrier interaction, which led to the transfer of electrons from the inner concave surface to the outer convex surface, leaving the Ni-Co NPs on the inner surface in an electron-deficient state and promoting the planar adsorption of phenol and the rapid generation of reactive H. [ABSTRACT FROM AUTHOR]