The invention discloses a general synthesis method of a three-dimensional compound structure based on three-dimensional MXene, and belongs to the field of nano materials. The three-dimensional compound structure is composed of a three-dimensional MXene load inorganic nano structure and is of a flower-like hierarchical porous structure. The method comprises the steps that an ultrasonic atomizer isadopted for atomizing mixed suspension liquid of three-dimensional MXene particles, metal salt and an auxiliary into aerosol micro-droplets, and under inert or reactive atmosphere, high-temperature fast drying is conducted to obtain the three-dimensional compound structure with controllable structure and size; or the three-dimensional MXene particles and metal salt or a nonmetallic compound are evenly mixed in solvent or in a solid-phase mode to obtain a mixture, and high-temperature calcination is conducted under the inert or reactive atmosphere to obtain the three-dimensional compound structure with controllable structure and size. By means of the three-dimensional compound structure based on the three-dimensional MXene, the problems of inorganic nano material particle aggregation, poorconductivity and two-dimensional MXene stacking can be solved, and thus a foundation is laid for preparation, processing and various aspects of application of a MXene-based high-performance functionalmaterial.