Abstract: Pervaporation (PV) process is a membrane-based separation technology that provides low-cost, environmentally friendly, and efficient characteristics in the separation of azeotropic mixtures. In this work, we provided a preparation method of a composite membrane based on molybdenum disulfide (MoS₂) two-dimensional material used to dehydrate isopropanol aqueous solution. A ceramic hollow fiber (CHF) membrane was used as a substrate to prepare the MoS₂ composite membrane. In order to reduce the macropores on the surface of the CHF membrane, a TiO₂ intermediate layer was introduced on the outer surface of the CHF substrate. Polyvinyl alcohol (PVA) was used as a binder in the preparation of the MoS₂/PVA separation layer. A MoS₂/PVA separation layer was constructed on the surface of the TiO₂-CHF membrane by vacuum filtration, and then crosslinked with glutaraldehyde solution to reduce the swelling degree of the MoS₂/PVA separation layer in aqueous solution. The morphology and physico-chemical properties of the obtained membranes were studied by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), atomic force microscopy (AFM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and water contact angle (WCA) measurements. The MoS₂/PVA composite membrane showed 486 g/(m²·h) of permeation flux and 445 of separation factor in a 90% IPA aqueous solution at 50 ℃.