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含超笼的硅铝酸盐沸石EMM-28由连续旋转电子衍射测定

Aluminosilicate Zeolite EMM-28 Containing Supercavities Determined by Continuous Rotation Electron Diffraction.

作者信息

Cichocka Magdalena O, Burton Allen W, Afeworki Mobae, Mabon Ross, Schmitt Kirk D, Strohmaier Karl G, Vroman Hilda B, Marella Michael A, Weston Simon C, Zou Xiaodong, Willhammar Tom

机构信息

Department of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden.

Corporate Strategic Research, ExxonMobil Research & Engineering Co., 1545 Route 22 East, Annandale, New Jersey 08801, United States.

出版信息

Inorg Chem. 2022 Jul 25;61(29):11103-11109. doi: 10.1021/acs.inorgchem.2c00856. Epub 2022 Jul 11.

DOI:10.1021/acs.inorgchem.2c00856
PMID:35816337
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9490810/
Abstract

A new aluminosilicate zeolite, denoted EMM-28, has been successfully synthesized on a large scale using 1,1-(3,3-(1,3-phenylene)bis(propane-3,1-diyl))bis(1-methylpyrrolidinium) hydroxide as an organic structure directing agent (OSDA), which was scaled up to an ∼20 g scale with a yield of 77%. It crystallizes as thin plates (40-100 nm in thickness), and the corresponding powder X-ray diffraction (PXRD) pattern shows significant peak broadening which makes it insufficient for structure determination. Continuous rotation electron diffraction (cRED) data collected from 13 crystals were successfully used to solve and refine the structure of EMM-28. This illustrates that cRED data are capable of performing structure determination despite limited PXRD data quality. EMM-28 has a unique framework structure containing supercavities, >21 Å in size, connected by one-dimensional 10-ring channels. High-resolution transmission electron microscopy (HRTEM) confirmed the structure model. The structure of EMM-28 is related to several known zeolite structures with large cavities.

摘要

一种新的铝硅酸盐沸石，记为EMM - 28，已成功地以1,1-(3,3-(1,3 - 亚苯基)双(丙烷 - 3,1 - 二基))双(1 - 甲基吡咯烷鎓)氢氧化物作为有机结构导向剂(OSDA)进行了大规模合成，放大至约20 g规模时产率为77%。它结晶为薄板(厚度为40 - 100 nm)，相应的粉末X射线衍射(PXRD)图谱显示出明显的峰展宽，这使得其不足以用于结构测定。从13个晶体收集的连续旋转电子衍射(cRED)数据成功用于解析和精修EMM - 28的结构。这表明尽管PXRD数据质量有限，cRED数据仍能够进行结构测定。EMM - 28具有独特的骨架结构，包含尺寸大于21 Å 的超笼，通过一维10元环通道相连。高分辨率透射电子显微镜(HRTEM)证实了该结构模型。EMM - 28的结构与几种已知的具有大孔穴的沸石结构有关。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/6a24eba15770/ic2c00856_0006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/0e666181ea31/ic2c00856_0001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/bb58b4ced37a/ic2c00856_0002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/3bf813fda9cd/ic2c00856_0003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/9742c4168b3b/ic2c00856_0004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/1fa7be1b6144/ic2c00856_0005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/6a24eba15770/ic2c00856_0006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/0e666181ea31/ic2c00856_0001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/bb58b4ced37a/ic2c00856_0002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/3bf813fda9cd/ic2c00856_0003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/9742c4168b3b/ic2c00856_0004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/1fa7be1b6144/ic2c00856_0005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/354d/9490810/6a24eba15770/ic2c00856_0006.jpg

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