3D Electron Diffraction Unravels the New Zeolite ECNU-23 from the "Pure" Powder Sample of ECNU-21

Angew Chem Int Ed Engl. 2020 Jan 13;59(3):1166-1170. doi: 10.1002/anie.201912488. Epub 2019 Nov 27.


A novel crystalline high-silica zeolite with 12×8-membered ring (R) channel system is prepared with the aid of the 3D electron diffraction (3D ED) technique. A crystal with the same topology as one of the predicted daughter structures of CIT-13 germanosilicate, named ECNU-23 (East China Normal University 23) was coincidentally detected by the 3D ED investigation during the structure characterization of the "pure" powder sample of existing one-dimension (1D) 10-R ECNU-21. By controlling the alkaline-assisted hydrolysis under moderate conditions, we purified the phase of ECNU-23 by selectively breaking and removing the chemically weak Ge(Si)-O-Ge and metastable Si-O-Si bonds. Its structure was determined based on the 3D ED data, and confirmed by high-resolution TEM images and powder X-ray diffraction (PXRD) data. The aluminosilicate Al-ECNU-23 shows unique catalytic properties in the isomerization/ disproportionation of m-xylene as solid-acid catalyst.

Keywords: 3D electron diffraction; alkali treatment; heterogeneous catalyst; structure determination; zeolites.