A preparation method of a pervaporation metal organic framework UiO-66 series gasoline desulfurization film includes: introducing a zirconia sol layer firmly combined with a carrier onto the carrier to obtain the carrier with the zirconia sol layer, and performing solvothermal growing to prepare a film layer; in the process of growing, the zirconia sol layer provides a metal source for a Uio-66 series film and serves as a active site and a connection point of film forming to promote forming of the UiO-66 series film which is continuous, uniform and complete. The UiO-66 series film prepared bythe method is a hydrophilic film and can preferentially adsorb thiophene with relatively high polarity; zirconium in a framework of the UiO-66 series film has special adsorption effect on thiophene, so that the UiO-66 series film has excellent performance in pervaporation dulsufurization, enrichment factor is higher than 10, and permeation flux is greater than 1.0kgm-2h-1. In addition, UiO-66 series materials are comparatively stable, so that the obtained film can be operated continuously for a long time (longer than 3d) while maintains stable performance.