[Display omitted] • MoS 2 -MCA superlattice is prepared. • Bi-layered 2D-MoS 2 precursor can be obtained by MoS 2 -MCA via thermal shock. • Monodisperse bi-layers 2D-MoS 2 solution can be prepared within few minutes by using the 2D-MoS 2 precursor. To investigate thermal shock properties of melamine cyanurate (MCA) for molybdenum disulfide (MoS 2) exfoliation, the MoS 2 -MCA superlattice is prepared through self-assembly of pristine MoS 2 , cyanuric acid (CA) and melamine (MA) in water solution. The prepared MoS 2 -MCA is heated in tubular furnace with controlled temperature to obtain two-dimensional (2D)-MoS 2 precursor. Their morphologies are characterized by using Fourier transform infrared (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The obtained 2D-MoS 2 precursor shows a high specific surface area at 336.90 m2/g due to bi-layer MoS 2. TEM and atomic force microscope (AFM) images of 2D-MoS 2 N-methyl-2-pyrrolidone (NMP) solution further confirm the bi-layer MoS 2 exfoliation. The above results prove that MCA is a good thermal shock agent for MoS 2 exfoliation. And the prepared 2D-MoS 2 precursor could also be a good solid reservoir. [ABSTRACT FROM AUTHOR]