The invention discloses preparation of a water-soluble metal-organic framework composite material and application thereof in detecting the concentration of fluorine ions in water. The preparation comprises the following steps of: preparing a urea solution; adding aluminum trichloride into ultrapure water, carrying out ultrasonic treatment until the aluminum trichloride is completely dissolved, adding 2-aminoterephthalic acid under a stirring condition, and stirring until the 2-aminoterephthalic acid is completely dissolved to obtain a mixed solution; slowly dropwise adding the urea solution into the mixed solution, and stirring to obtain a reaction solution; carrying out heat preservation after the reaction solution is heated, cooling, centrifuging, washing precipitates, and carrying out centrifugal separation to obtain a first product; and dispersing the first product into N, N-dimethylformamide, stirring, carrying out centrifugal separation to obtain a second product, dispersing thesecond product into methanol, stirring, carrying out centrifugal separation, and carrying out vacuum drying to obtain the water-soluble metal organic framework composite material. The composite material is used for detecting the fluorine ion concentration in water. The fluorescent probe prepared by the preparation method has a nanosheet microstructure, is easy to store, and has excellent solubility and good stability in water.