Hierarchical Microporous/Mesoporous Composite Adsorbent for Deep Dehydration of Tetrahydrofuran.

The presence of residual moisture in tetrahydrofuran (THF) greatly limits its suitability for moisture-sensitive processes, including polymerization, Grignard chemistry, and fine-chemical production, where the allowable water concentration is generally lower than 10 mg/kg. Here, a hierarchical microporous/mesoporous composite adsorbent was prepared via extrusion molding, combining an LTA-type zeolite microporous framework with an amorphous mesoporous matrix. Characterization by XRD, FTIR, SEM, and pore analysis confirmed that the LTA crystal structure was retained while mesopores provided channels for mass transport. Static dehydration tests showed that the composite reduced THF water content from 70 mg/kg to 8.3 mg/kg, compared to 23.4 mg/kg for commercial 3A molecular sieves. The enhanced performance arises from micropores supplying uniform adsorption sites for deep dehydration and mesopores accelerating diffusion. Water vapor adsorption, kinetic and isotherm analyzes, regeneration, and competitive adsorption experiments indicated improved water accessibility and high selectivity, with kinetics described by a double-exponential model. The adsorbent remained stable over six adsorption-regeneration cycles. These results demonstrate that hierarchical microporous/mesoporous structures effectively achieve deep THF dehydration.