The invention discloses a preparation method of metal organic framework compound adsorbent particles for extracting rubidium and cesium resources from salt lake brine, seawater and underground water. The adsorbent particles are prepared by taking a water-absorbing polymer as a carrier, adding transition metal ferrous ferrocyanide, potassium cobalt cyanide, potassium nickel ferrocyanide, potassium titanium ferrocyanide, potassium copper ferrocyanide, potassium cadmium ferrocyanide or other metal organic framework compound adsorbents in a high loading amount, and carrying out secondary cross-linking. The preparation process is simple and is suitable for industrial production. The prepared adsorbent particles have the characteristics of high elasticity, porosity, high water absorption, good permeability and the like. A resin matrix is resistant to strong acid, strong alkali and high-salt environments, the polyhydroxy structure on the surface of the matrix can effectively adsorb adsorbent particles, the solution loss rate is effectively reduced, the method can be applied to extraction of rubidium and cesium elements in salt lake raw brine, old brine, seawater and underground water resources, and meanwhile the high-strength corrosion-resistant matrix is suitable for an industrial adsorption column process.