The invention discloses a layered fluorine-containing metal-organic framework material for adsorbing and separating acetylene ethylene, the structural general formula is ML2A, M is a metal ion, L is abroken line type organic ligand, A is an inorganic fluorine-containing anion, and the metal ion M is at least one of Cu<2+>, Fe<2+>, Co<2+>, Ni<2+> and Zn<2+>, wherein the broken line type organic ligand L is at least one of 4, 4'-dipyridylsulfoxide and 4, 4'-dipyridylsulfone, and the inorganic fluorine-containing anion A is at least one of SiF6<2->, GeF6<2->, ZrF6<2->, SnF6<2->, TiF6<2->, NbOF52<->, WO2F4<2-> and MoO2F4<2->. The layered fluorine-containing metal-organic framework material can be prepared by adopting an interface diffusion method, a solvothermal method or a room-temperature stirring method. The layered fluorine-containing metal-organic framework material is used as an adsorbent and is in contact adsorption with a gas mixture containing acetylene and ethylene, and efficient separation of acetylene/ethylene can be realized at normal temperature, low acetylene content and low acetylene partial pressure.