A kind of catalyst for Fcc gasoline's adsorption desulfuration contains in weight percent: 10-85% nano zinc oxide, the atomic diameter of which is 100-500 mu m, 5-80% silica oxide, 5-30% alumina oxide, and 4-45% nickel oxide. The method of preparation is: (1) Mix evenly the nano zinc oxide, silica oxide, alumina oxide, and nickel oxide; dry the particle of step (b); roast the dry particle of step(c); deoxidize the particle of step(d) by proper reductant. The portions of this catalyst remain mixed, and the method adopts the technology of roasting. The catalyst has a good strength, high desulfuration activity, and effective regeneration. Because of the adoption of nano zinc oxide, it causes little to octane number and applies to desulfuration of FCC gasoline. Moreover, the method of preparation is simple and the operation is easy.