Direct hydrothermal synthesis of hierarchically porous siliceous zeolite by using alkoxysilylated nonionic surfactant.
A hierarchically porous siliceous MFI zeolite (silicalite-1) with narrow mesoporosity has been hydrothermally synthesized by using trialkoxysilylated alkyl poly(oxyethylene ether) as mesopore-directing agent. A mesostructured silica-surfactant composite was formed at the early stage of the reaction, and zeolite crystallization proceeded during subsequent hydrothermal treatment. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations of the crystallized products showed that micro- and mesopores were hierarchically assembled in unique particle morphology with rugged surfaces. Solid-state (29)Si and (13)C NMR revealed that the covalent bonds between the zeolite framework and mesopore-directing agent were present in the products before calcination. The use of nonsilylated alkyl poly(oxyethylene ether) or a silylated alkytrimethyl-ammonium-type cationic surfactant for the synthesis of silicalite-1 resulted in a mixture of mesoporous silica and zeolite as the final product, which suggests that the covalent interaction and nonelectrostatic charge matching interaction favor the formation of hierarchically mesoporous siliceous zeolite. This alkoxysilylated nonionic surfactant can also be extended to synthesize aluminosilicate MFI zeolite (ZSM-5).
Mukti
Rino R
RR
Department of Chemical System Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan.
Hirahara
Hirotomo
H
Sugawara
Ayae
A
Shimojima
Atsushi
A
Okubo
Tatsuya
T
D010316:Particle Size; D016062:Porosity; D013499:Surface Properties; D013501:Surface-Active Agents / Q000138:chemical synthesis / Q000737:chemistry*; D013696:Temperature; D017641:Zeolites / Q000138:chemical synthesis* / Q000737:chemistry
D013501:Surface-Active Agents; D017641:Zeolites