Fabrication and characterization of highly crystalline mordenite membranes on α-alumina disks via a seeded in situ template-free hydrothermal treatment

Abstract

A template-free seeded short-time in situ hydrothermal treatment was carried out in a brass autoclave to synthesize crystalline mordenite (MOR) membranes on alumina-silicate disk supports with micro-scale pores. According to XRD analysis, MOR was the only zeolitic material present in the membrane layers on the supports. SEM examination of the membranes showed three different layers of the membrane thickness: (i) support sub-layer, (ii) mix penetrated mid-layer, the MOR crystals filling the pores among the support (about 4–5 μm), and (iii) MOR top-layer (about 4–5 μm). The crystalline bonds between MOR crystals of the membrane top-layer and the crystals of the support were clearly observed within the mid-layer. The continuous top-layer of zeolitic membrane was formed by many large and well-shaped crystals. The seeding treatment significantly enhanced the formation of MOR crystals onto the surface of the supports. EDAX analysis showed a Si/Al ratio of 6.8 for the MOR layer of the membrane. Due to their hydrophilic natures, the polycrystalline MOR membranes were found to be selective for continuous dehydration of different EtOH–water mixtures through an adsorption–diffusion–desorption mechanism. Both total permeation flux and separation factor of the membrane were found to increase by increasing temperature and water concentration of feed. The continuity and high crystallinity of the membrane top-layer led to the fairly high dehydration of EtOH. It was found that there was no pinhole within the layer and the morphology of the membrane was almost defect-free.