Intercalation chemistry is of great importance in solid‐state physics and chemistry for the ability to modulate electronic structures for constructing new materials with exotic properties. This ancient and versatile discipline has recently become prevailing in the synthesis and regulation of 2D transition metal dichalcogenides (TMDs) with atomic thickness due to diverse host–guest configurations and their impact on layered frameworks, which bring in extensive applications in electronics, optoelectronics, and other energy‐based devices. In order to prepare 2D TMD materials with desired structure and properties, it is essential to gain in‐depth understanding of the key role the intercalation chemistry plays in the preparation process. A focused review on recent advances regarding 2D TMD materials through intercalation exfoliation from the view of host, guest, and solvent interactions is provided. The effect of intercalation chemistry on TMD nanosheets synthesis and modification is comprehensively reviewed. The interactions between host and guest from the aspects of lattice strain, interlayer distance, and carrier density are considered. Finally, a prospectus of the future research opportunities for the intercalation chemistry of 2D materials is provided.