Abstract: The disclosure relates to the technical field of functional nanomaterials, in particular to a fluorescent metal-organic framework superstructure compound, a preparation method and application thereof. The present disclosure provides a method for preparing a fluorescent metal-organic framework superstructure compound, comprising the steps of: providing a microfluidic mixing device; injecting a soluble rare earth salt solution from the first feeding pipe 1; injecting an oil phase solution from the second feeding pipe 2; forming droplets of the rare earth salt solution in the mixing channel 4; then subjecting the droplets to a coordination reaction with an organic ligand solution to obtain the fluorescent metal-organic framework superstructure compound. The preparation method provided by the present disclosure can prepare the fluorescent metal-organic framework superstructure compound in the form of a sphere which is self-assembled from MOFs nanorods, and the particle size distribution of the sphere is uniform.