A two-dimensional molybdenum disulfide (MoS 2 ) nanosheet, as a new type of inorganic material with high hydrophobicity and excellent physicochemical stability, holds great application potential in the preparation of a high separation performance organic− inorganic hybrid membrane. In this work, high hydrophobic MoS 2 was embedded in hydrophobic polyether copolymer block amide (PEBA) to prepare PEBA/MoS 2 organic− inorganic hybrid membranes. The structure, morphology, and hydrophobicity of the hybrid membrane were characterized by scanning electron microscopy, thermogravimetric analysis, contact angle goniometry, X-ray diffraction, infrared spectroscopy analysis, and atomic force microscopy. The effect of embedding of MoS 2 on the swelling degree and pervaporation separation performance of the PEBA/MoS 2 hybrid membrane was studied with a 1.0 wt % pyridine dilute solution. The results indicated that with increasing the MoS 2 content, the separation factor of PEBA/MoS 2 increased first and then decreased, while it showed a downward trend in the permeation flux. When the MoS 2 content in the PEBA/MoS 2 hybrid membrane was 10.0 wt %, the permeation flux was 83.4 g m −2 h −1 (decreased by 21.5% compared with the pure PEBA membrane), and the separation factor reached a maximum value of 11.11 (increased by 37.6% compared with the pure PEBA membrane). Meanwhile, the effects of feed temperature on the pervaporation separation performance of PEBA/MoS 2 hybrid membranes were also studied. In addition, as the PEBA/MoS 2 hybrid membrane has excellent thermal stability, it is expected to be a promising material for recovering pyridine from wastewater.