高等学校化学学报 ›› 2021, Vol. 42 ›› Issue (1): 60.doi: 10.7503/cjcu20200687
所属专题: 分子筛功能材料 2021年,42卷,第1期
刘启予,范炜
收稿日期:
2020-09-15
出版日期:
2021-01-10
发布日期:
2021-01-12
基金资助:
Received:
2020-09-15
Online:
2021-01-10
Published:
2021-01-12
Contact:
FAN Wei
E-mail:wfan@engin.umass.edu
Supported by:
摘要:
具有内部介孔结构的多级孔分子筛兼具微孔分子筛和介孔材料的功能, 拥有良好的传质和催化特性. 在过去的几十年内, 介孔分子筛在催化、 吸附和分离领域发展迅速. 近年来, 新型合成方法的开发在很大程度上实现了介孔分子筛孔道结构、 组分及形貌灵活可控的调节. 本综述讨论了近期出现的多种新合成路径, 重点介绍了近期发展起来的二次合成制备低硅/铝介孔分子筛、 超分子自组装合成介孔分子筛及有机小分子原位合成介孔分子筛技术. 对这些合成技术的机理进行了讨论, 以期为介孔分子筛未来的发展提供思路. 文章的最后还讨论了不同的合成策略所面临的一些关键性挑战.
中图分类号:
TrendMD:
刘启予, 范炜. 介孔分子筛制备技术新进展—二次合成、超分子自组装和介孔生成剂法. 高等学校化学学报, 2021, 42(1): 60.
LIU Qiyu, FAN Wei. Recent Advances in the Synthesis of Mesoporous Zeolites by Post-synthetic Method, Supramolecular Self-assembly and Mesopore Generation Agent. Chem. J. Chinese Universities, 2021, 42(1): 60.
Fig.1 SEM(A, B) and TEM(C, D) images of pristine and hierarchical ZSM?5 zeolites[56](A, B) Pristine zeolite with a Si/Al ratio of 13.9; (C, D) mesoporous ZSM?5 with a Si/Al ratio of 10.4 synthesized by steam treatment at 500 ℃ for 3 h and alkaline treatment in NaOH solution(0.2 mol/L) at 80 ℃ for 30 min.Copyright 2017, Wiley.
Fig.2 Schematic representation of preparation of the mesoporous ZSM?5 nanoboxes via rapid ageing (of the precursor sol gel mixture) and post?synthetic TPAOH treatment(A); HRTEM images of as?made MFI with extra framework Al(B1, B2) and synthesized ZSM?5 nanoboxes made(C1, C2) by the treatment in 0.1 mol/L of TPAOH for 6 h; STEM images of as?made MFI(D) and synthesized ZSM?5 nanoboxes(E) made by the treatment in 0.1 mol/L of TPAOH for 6 h; HRTEM images(F, G) of synthesized ZSM?5 nanoboxes made by the treatment in 0.1 mol/L of TPAOH for 6 h[57]Inset in (G): the corresponding fast Fourier transform(FFT) of HRTEM.Copyright 2020, Wiley.
Fig.3 Synthesis and characterization of mesoporous zeolites by post?synthetic method in the presence of surfactants(A) Schematic representation for conventional USY zeolite synthesis and mesoporous USY synthesized using the post?synthetic method in the presence of surfactants. Conventional synthesis*(above), mesostructuring(center), and dissolution and reassembly(bottom) of USY zeolite, and the apparent activation energies of the steps involved[66]. (B) NLDFT pore size distribution curves calculated from Ar isotherms at 87 K for mesoporous USY obtained with trimethylalkylammonium?based surfactants with increasing alkyl chin length (C10?C22)[65]. (C) In situ time?resolved synchrotron XRD study of formation of mesoporous USY in the presence of surfactants[68].(A) Copyright 2018, Wiley; (B) Copyright, 2016 American Chemical Society; (C) Copyright 2014, Wiley. * obtained from Kacirek H., Lechert J. H., Phys. Chem., 1976, 80, 1291.
Fig.4 SEM and TEM images of the MFI nanosheets synthesized using C22?6?6 [C22H45?N(CH3)2?C6H12?N(CH3)2?C6H13Br2] as the surfactant(A)[81] and schematic diagrams of the atomic and mesoscopic material structures that evolve during the hydrothermal crystallization of the zeolite MFI nanosheets(B—D)[83](B)?Initially amorphous silica frameworks(gray) with weak hexagonal mesophase ordering; (C)?intermediate nanolayered silicates; (D)?zeolite MFI nanosheets. Si and O framework atoms are represented by blue and white spheres, respectively. The surfactant headgroups and alkyl chains are represented by black circles and gray lines, respectively.(A) Copyright 2009, Springer Nature; (B—D) Copyright 2015, Wiley.
Fig.5 Typical amino acids used as mesoporogens to form mesopore in LTA zeolite(A)[101] and the trend of decreasing mesopore size in LTA zeoltie as a function of the hydrophathy index of amino acids(B)[18](A) Copyright 2017, Elsevier; (B) Copyright 2019, Wiley.
Fig.6 Structure characterizations of mesoporous LTA(A—J) and effect of small molecule pKa values on generated mesopore surface areas represented by SBET of NaA crystals(K)[102](A—J) SEM images(A—D) and cross?sectional TEM images(E—J) after ultramicrotomy of mesoporous LTA crystals synthesized in the presence of L?alanine(A, E, I), phenol(B, F), 1,2,3?triazole(C, G, J), or nitromethane(D, H). Insets in (I) and (J) are the corresponding high?resolution TEM and selected?area electron diffraction images showing lattice fringes and diffraction patterns, respectively. (K) Data points are distributed only in quadrant II, indicating mesopore generation by OMeGA, and in quadrant IV, illustrating no significant mesopores by small molecules not deprotonated in situ.Copyright 2019, American Chemical Society.
Fig.7 Schemetic representation for the evolution process of single?crystalline and defect?free hierarchical zanozeolites in the presence of L?Lysine[104]Copyright 2019, American Chemical Society.
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