TY - JOUR
T1 - In situ generation by cyclisation of an organic structure directing agent for the synthesis of high silica zeolite ERS‐7
AU - Lozinska, Magdalena Malgorzata
AU - Chitac, Ruxandra Georgiana
AU - Bruce, Elliott
AU - Manoj, Malavika
AU - Du, Yuanyuan
AU - Dawson, Daniel
AU - Ashbrook, Sharon
AU - Cox, Paul
AU - Wright, Paul Anthony
PY - 2025/4/3
Y1 - 2025/4/3
N2 - Zeolites with high framework Si/Al ratios are of interest for industrial applications due to their hydrothermal stability. They are usually synthesized in the presence of pre-prepared organic structure directing agents (OSDAs). The high silica ERS-7 zeolite (topology type ESV) can be crystallized using N,N-dimethylpyrrolidinium (dmpyrr) that is formed in situ via cyclization of N,N,N’,N’-tetramethyl-1,4-diaminobutane (tmdab) when a cationic polymer is also present. The in situ generation of dmpyrr is demonstrated by solid-state 13C NMR spectroscopy and supported by both chemical analyses and comparative syntheses using pre-prepared dmpyrr. The cationic polymer inhibits the crystallization of mordenite, which is otherwise observed to be the favored product. The ERS-7 prepared via in situ dmpyrr synthesis (Si/Al = 14) is characterized by PXRD and solid-state NMR spectroscopy. The CO2 adsorption seen for the H- and Na-forms indicates interactions with accessible Na+ cations. The synthetic studies indicate the potential for in situ generation of OSDAs to reduce the need for extended OSDA syntheses.
AB - Zeolites with high framework Si/Al ratios are of interest for industrial applications due to their hydrothermal stability. They are usually synthesized in the presence of pre-prepared organic structure directing agents (OSDAs). The high silica ERS-7 zeolite (topology type ESV) can be crystallized using N,N-dimethylpyrrolidinium (dmpyrr) that is formed in situ via cyclization of N,N,N’,N’-tetramethyl-1,4-diaminobutane (tmdab) when a cationic polymer is also present. The in situ generation of dmpyrr is demonstrated by solid-state 13C NMR spectroscopy and supported by both chemical analyses and comparative syntheses using pre-prepared dmpyrr. The cationic polymer inhibits the crystallization of mordenite, which is otherwise observed to be the favored product. The ERS-7 prepared via in situ dmpyrr synthesis (Si/Al = 14) is characterized by PXRD and solid-state NMR spectroscopy. The CO2 adsorption seen for the H- and Na-forms indicates interactions with accessible Na+ cations. The synthetic studies indicate the potential for in situ generation of OSDAs to reduce the need for extended OSDA syntheses.
U2 - 10.1002/chem.202500327
DO - 10.1002/chem.202500327
M3 - Article
SN - 0947-6539
JO - Chemistry
JF - Chemistry
M1 - e202500327
ER -