Laminated Adsorbents with Very Rapid CO₂ Uptake by Freeze-Casting of Zeolites

Structured zeolite 13X monoliths with a laminated structure and hierarchical macro-/microporosity were prepared by freeze-casting aqueous suspensions of zeolite 13X powder, bentonite, and polyethylene glycol. Colloidally stable suspensions with a low viscosity at both room temperature and near freezing could be prepared at alkaline conditions where both the zeolite 13X powder and bentonite carry a negative surface charge. Slow directional freezing of the suspensions led to the formation of well-defined and thin lamellar pores and pore walls while fast freezing resulted in more cylindrical pores. The wall thickness, which varied between 8 and 35 μm, increased with increasing solids loading of the suspension. Thermal treatment at 1053 K of the freeze-cast bodies containing between 9 and 17 wt % bentonite resulted in mechanically stable zeolite 13X monoliths. The monoliths displayed a carbon dioxide uptake capacity of 4-5 mmol/g and an uptake kinetics characterized by a very fast initial uptake where more than 50% of the maximum uptake was reached within 15 s. Freeze-cast laminated zeolite monoliths could be used to improve the volumetric efficiency and reduce the cycle time, of importance in, for example, biogas upgrading and CO2 separation from flue gas.