The invention discloses a preparation method of a phenazine-connecting two-dimensional covalent organic framework material of a novel structure. The synthesized phenazine-connecting two-dimensional covalent organic framework material of the novel structure has a highly planar rigid structure in a graphene-like single layer, and is also highly conjugated between layers. A synthesis method is a solvothermal method and is easy and safe to operate, the reaction is a molecular level reaction, and the synthesized product is more ordered and more stable. According to the method, triphenylene-2,3,6,7,10,11-hexaaminotriphenylene and hexaketocyclohexane octahydrate serve as raw materials, 1,4-dioxane and 1,3,5-mesitylene serve as organic solvents, and the phenazine-connecting two-dimensional covalent organic framework material of the novel structure is successfully prepared through the solvothermal method under the condition that acetic acid is used for adjusting the acid environment.