The invention discloses an ultrathin layered material prepared by a metal-organic coordination polymer and a preparation method of the ultrathin layered material. The ultrathin layered material consists of the following components in parts by mass: 0-30 parts of transition metals, 0-40 parts of organic sulfonic acid and 100-30 parts of a nitrogen-containing ligand. The preparation method of the ultrathin layered material comprises the following steps: preparing metal-organic coordination polymer by taking organic amine as a template agent and using anion of organic sulfonic acid as counter anion; performing solvent thermal treatment on the prepared metal-organic coordination polymer in an organic solvent, and separating the treated metal-organic coordination polymer to prepare the ultrathin layered material. The layered material has strong conductivity, and is a relatively ideal catalyst loading carrier and a graphene-like material. The ultrathin layered material prepared by the process has the advantages of a simple preparation method, easiness for operation, low preparation cost, wide application prospect, and the like.