Diamond@ graphene oxide@ gold nanoparticle (D@GO@AuNP) nanocomposite materials were synthesized by a modified Hummers method using diamond@ graphite composites that were obtained by the spark plasma sintering treatment of diamond, and gold nanoparticles that were prepared from a solution of HAuCl4 via reduction by NaBH4. The obtained diamond@ graphene oxide utilized as a catalytic carrier has great advantages, such as high specific surface area and a porous structure, which provide more opportunities for the gold nanoparticles to access the catalytic carrier. In addition, the prepared hierarchical diamond-based D@GO@AuNP nanocomposites are beneficial to improve the catalytic capacity of gold nanoparticles with higher dispersion on the GO surface. Catalytic experiments with 4-nitrophenol and 2-nitroaniline were carried out using the synthesized D@GO@AuNP material. The obtained nanocomposites demonstrated excellent catalytic activity and high recyclability, without any decrease in the weight of gold nanoparticles after eight cycles of catalytic reduction, indicating the potential applications of the composite catalytic materials.