The invention discloses a preparation method of a sulfide heterojunction material capable of resisting photocorrosion in a photo-Fenton reaction, and belongs to the fields of photochemical energy conversion and photocatalytic degradation. The preparation method aims at solving the technical problem that the corrosion to a sulfide is possibly exacerbated in a strongly oxidative photo-Fenton reaction induced by hydrogen peroxide. The method provided by the invention comprises the following steps of I, adding an alpha-Fe2O3 nano particle into deionized water, agitating, then adding Na2MoO4.2H2O and CH4N2S in sequence, ultrasonically oscillating, heating and then carrying out heat preservation, washing with absolute ethyl alcohol for 3 times, then washing with ionized water for 3 times, and drying, so as to obtain Fe2O3/MoS2; and II, dispersing the Fe2O3/MoS2 obtained in step I in a mixed solution, ultrasonically oscillating, then agitating at a room temperature to completely hydrolyze TEOS (Tetraethyl Orthosilicate), taking a deposit, and carrying out vacuum drying, so as to obtain the sulfide heterojunction material. The preparation method is used in the fields of the photochemical energy conversion and the photocatalytic degradation.