The invention provides a preparation method of dissolving-resistant oil-water separation filter paper, and the preparation method comprises the following steps: obtaining raw materials; adding nano-diatomaceous earth, calcium carbonate, water-soluble phenolic resin, coconut fibers, saw dust, citric acid, zinc nitrate and microcrystalline cellulose into mixed slurry, and heating to 70-80 DEG C; after defibering by a defibering machine, grinding pulp, performing papermaking according to a conventional papermaking process, forming, squeezing and drying; compared with the prior art, the preparation method comprises the following beneficial effects: by selecting natural cotton fibers, gypsum fibers, and polyester fibers to serve as basic raw materials, the characteristics of oil-water resistance and high temperature resistance of the filter paper are provided, by addition of the saw dust, the environment-friendly performance is improved, and the oil-water separation performance of the filter paper material is effectively improved.