沸石铝分布精准调控: 策略、表征与展望

doi:10.6023/A25100345

化学学报 ›› 2026, Vol. 84 ›› Issue (1): 173-188.DOI: 10.6023/A25100345 上一篇

综述

沸石铝分布精准调控: 策略、表征与展望

高红霞^a, 陈慧慧^b, 李林梅^a^,^*(), 赵侦超^a, 徐舒涛^b^,^*()

^a 浙江师范大学化学与材料科学学院先进催化材料教育部重点实验室浙江金华 321004
^b 中国科学院大连化学物理研究所低碳催化与工程研究中心辽宁大连 116023

投稿日期:2025-10-18 发布日期:2025-11-06

作者简介:

高红霞, 浙江师范大学化学与材料科学学院2022级硕士研究生. 主要研究方向为沸石结构单元调控碱处理制备多级孔沸石作用机制.

陈慧慧, 中国科学院大连化学物理研究所博士研究生. 主要研究方向为原位固体核磁研究分子筛酸性质子的离域性质.

李林梅, 浙江师范大学化学与材科学学院, 讲师. 2013年博士毕业于武汉大学分析化学专业. 主要研究方向为基于微流控芯片的电化学分析、材料合成及催化应用.

赵侦超, 浙江师范大学化学与材科学学院, 双龙学者特聘教授. 2007年本科毕业于郑州大学化学系, 2013年博士毕业于中国科学院大连化学物理研究所. 主要研究方向为沸石、氧化铝等催化材料的固体核磁共振表征以及多相催化反应机理研究.

徐舒涛, 中国科学院大连化学物理研究所研究员. 2004年本科毕业于复旦大学化学系, 2010年博士毕业于中国科学院大连化学物理研究所. 现为大连化物所低碳催化技术国家工程研究中心科研骨干. 2016年获第16届国际催化大会青年科学家奖(Young Scientist Prize), 2020年获国家自然科学基金委优秀青年基金资助, 2023年获中国化学会分子筛青年奖. 主要研究方向为原位固体核磁谱学技术在分子筛催化中的应用.

基金资助:
国家自然科学基金(22472153); 国家自然科学基金(22241801); 国家自然科学基金(22032005); 国家自然科学基金(22022202); 浙江省教育厅一般科研项目(Y202456744); 大连市杰出青年科学家基金(2021RJ01); 辽宁国际联合实验室项目(2024JH2/102100005)

Precise Control of Aluminum Distribution in Zeolites: Strategies, Characterization, and Perspectives

Hongxia Gao^a, Huihui Chen^b, Linmei Li^a^,^*(), Zhenchao Zhao^a, Shutao Xu^b^,^*()

^a Key Laboratory of Advanced Catalytic Materials of the Ministry of Education, Zhejiang Normal University, Jinhua, Zhejiang 321004, China
^b National Engineering Research Center of Lower-Carbon Catalysis Technology, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, Liaoning 116023, China

Received:2025-10-18 Published:2025-11-06
Contact: * E-mail: lilinmei@zjnu.edu.cn;xushutao@dicp.ac.cn
Supported by:
National Natural Science Foundation of China(22472153); National Natural Science Foundation of China(22241801); National Natural Science Foundation of China(22032005); National Natural Science Foundation of China(22022202); Zhejiang Provincial Education Department(Y202456744); Dalian Outstanding Young Scientist Foundation(2021RJ01); Liaoning International Joint Laboratory Project(2024JH2/102100005)

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摘要/Abstract

精准调控化学反应转化是多相催化的终极目标. 沸石催化剂凭借其独特的择形选择性在化工生产中应用广泛, 但要实现高效反应转化仍依赖对活性位结构的精确调控, 以抑制副反应的发生. 沸石的活性中心由分布在晶体学不等价T位的铝(Al)原子构成, 因此, 调控Al在局域(T位)及区域(空间)层面的分布已成为该领域研究热点. 此综述以局域Al分布调控为主线, 系统综述了调控策略(自下而上与自上而下)及相关先进表征技术. 在自下而上策略中, 以典型的沸石结构为例, 重点阐明了有机/无机结构导向剂调控Al分布的机制, 结合理论计算揭示了范德华力、静电库仑作用及氢键对Al分布定位的影响规律; 在自上而下策略中, 基于不同T位点杂原子(或Al原子)的稳定性差异, 实现了Al的选择性脱除与植入, 并评述了该策略的优势与局限. Al分布结构的精准表征是评估Al分布调控效果的关键. 此综述还总结了关于Al分布表征的最新研究进展, 强调多技术联用可提供更可靠的结构信息. 最后, 基于各合成策略及表征手段的优势与挑战, 展望了人工智能与大数据驱动的高通量微通道沸石合成实现Al分布精准调控, 通过多表征技术融合实现Al分布的精确结构解析, 最终实现定向反应型高效沸石催化剂的理性设计.

关键词: 铝分布, 沸石, 结构导向剂, 主客体相互作用, 催化

The ultimate goal of heterogeneous catalysis is to precisely regulate chemical reaction transformations. Zeolite catalysts, with their unique shape-selective properties, have been widely used in chemical production, however, achieving highly efficient catalytic reactions requires accurate control over the structure of active sites to minimize side reactions. Since aluminum (Al) atoms located at crystallographically nonequivalent T-sites form the active centers of zeolites, controlling the distribution of Al at both local (T-site level) and spatial (regional) scales has become a research focus in zeolite science. This review systematically summarizes strategies for regulating Al distribution in zeolites—both bottom-up and top-down approaches—as well as advanced characterization techniques. In the bottom-up strategy, using representative zeolite frameworks as examples, we elucidate the mechanism by which organic and inorganic structure-directing agents influence Al distribution. Combined with theoretical calculations, we reveal how van der Waals forces, electrostatic interactions, and hydrogen bonding govern the spatial positioning of Al. In the top-down strategy, selective removal or incorporation of Al atoms is achieved based on variations in the stability of heteroatoms (or Al atoms) at different T-sites, and the advantages and limitations of this method are critically discussed. Accurate characterization of Al distribution is essential for evaluating the effectiveness of regulation strategies; thus, recent advances in Al site characterization are reviewed, emphasizing that multi-technique approaches can yield more reliable structural information. Finally, the review summarizes the merits and drawbacks of each strategy and envisions the future integration of artificial intelligence and big-data-driven high-throughput microchannel zeolite synthesis to realize precise control of Al distribution. The fusion of multiple characterization techniques is further expected to enable accurate structural elucidation, ultimately guiding the rational design of reaction-specific, high-performance zeolite catalysts.

Key words: Al distribution, zeolite, structure directing agent, host-guest interactions, catalysis

引用此文

高红霞, 陈慧慧, 李林梅, 赵侦超, 徐舒涛. 沸石铝分布精准调控: 策略、表征与展望[J]. 化学学报, 2026, 84(1): 173-188.

Hongxia Gao, Huihui Chen, Linmei Li, Zhenchao Zhao, Shutao Xu. Precise Control of Aluminum Distribution in Zeolites: Strategies, Characterization, and Perspectives[J]. Acta Chimica Sinica, 2026, 84(1): 173-188.

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图/表 11

图1. 沸石不同孔道Al分布及反应选择性示意图(a), 不同Al分布(孤立Al, “Al对”)稳定金属离子类型及活性中间物种(b); 沸石晶粒内及表面Al的空间不均匀分布示意图(c)

Figure 1. Schematic of zeolites with different channel Al distributions and reaction selectivity (a); types of metal ions stabilized by different Al distributions (isolated and paired Al) and active intermediate species (b); and spatial heterogeneity of Al distribution within and on the surface of zeolite crystals (c)

图2. FER沸石结构及典型有机结构导向剂分布示意图(a)[46], 用于合成FER沸石的不同结构导向剂及相应8元环孔穴酸位占比(b), 有机、无机结构导向剂与沸石骨架之间的不同作用示意图(c). *数据来自于文献[47-48]

Figure 2. Schematic diagram of FER zeolite structure and distribution of typical OSDAs (a) (Adapted with permission from reference [46], Copyright 2013, American Chemical Society), different OSDAs used to synthesize FER zeolite and the corresponding proportion of acid sites on 8-membered ring cave annotated in parentheses (b), and schematic diagram of interactions between organic/inorganic SDAs and the framework of zeolite (c). * Data adapted from references [47-48]

图3. 合成ZSM-5沸石控制Al分布的常见结构导向剂及刚性季铵盐与柔性可成氢键有机胺导向不同Al分布示意图[63]

Figure 3. Schematic draws of common SDAs used to synthesize ZSM-5 zeolite for controlling Al distribution, and the different Al distributions directed by rigid quaternary ammonium salts versus flexible, hydrogen-bond-capable organic amine. (Adapted with permission from reference [63], Copyright 2024, American Chemical Society)

图4. TMAda+与Na+, K+协同调控SSZ-13沸石孤立Al、“Al对”分布示意图[70]

Figure 4. Schematic illustration of the cooperative regulation of isolated Al and Al pairs distribution in SSZ-13 zeolite by TMAda+ with Na+and K+. (Reprinted with permission from reference [70], Copyright 2020, American Chemical Society)

图5. 不同有机结构导向剂(a)及其在AEI笼中最为稳定排布及对应不同T位Al分布的相对能量(b)[82]

Figure 5. Different organic structure-directing agents (a) and their most stable configurations in the AEI cage, along with the relative energies corresponding to different T-site Al distributions (b)[82]

图6. FAU沸石转晶合成CHA沸石, FAU前驱体中的Al分布影响产物CHA沸石中Al分布的作用机制示意图(a)[96]及在FAU转晶合成CHA沸石所采用的分裂合成法示意图(b)[101]

Figure 6. Schematic diagram illustrating (a) the mechanism of Al distribution in CHA zeolite product governed by FAU precursor during the FAU-to-CHA interzeolite conversion (IZC),[96] and (b) the split synthesis strategy used in the FAU-to-CHA IZC process[101]

图7. 利用SiCl4脱除MOR沸石12元环骨架Al并补充8元环侧边袋中Al分布的作用机制示意图[118]

Figure 7. Schematic diagram of the mechanism by which SiCl4 removes framework Al from the 12-membered rings of MOR zeolite and replenishes Al distribution in the 8-membered-ring side pockets[118] (Copyright 2022, Wiley-VCH GmbH)

图8. Al从具有8元环孔口的小孔沸石骨架中脱除、迁移出晶体示意图[126]

Figure 8. Proposed scheme of dealumination and extraction of EFAl species in small-pore zeolites with 8 membered-ring aperture[126] (Reproduced from Tatsushi Yoshioka et al., Science Advances, doi:10.1126/sciadv.abo3093 [2022], AAAS.)

图9. 27Al MQMAS NMR区分ZSM-5沸石中不同T位Al的27Al NMR信号(a), 相应实验所得27Al NMR化学位移与不同T位Al分布理论计算得到27Al NMR化学位移分布的对比图(b)[127]

Figure 9. 27Al MQMAS NMR distinguishing the 27Al NMR signals of different T-site Al in ZSM-5 zeolite (a), and comparison of the experimentally observed 27Al NMR chemical shifts with the distribution of 27Al NMR chemical shifts calculated from the theoretical distribution of Al among different T sites (b)[127] (Copyright 2007, Wiley-VCH GmbH)

图10. 以HMI和CHA为模板剂合成的MCM-49(HMI)和MCM-49(CHA)的27Al MAS NMR (a, b)及1H-27Al D-RINEPT NMR谱图(c, d)[135]

Figure 10. 27Al MAS NMR spectra (a, b) and 1H-27Al D-RINEPT spectra (c, d) of MCM-49 (HMI) and MCM-49 (CHA) synthesized using HMI and CHA as structure-directing agents. (Adapted with permission from reference [135], Copyright 2021, American Chemical Society)

图11. 软X射线在改变能量(共振、非共振)条件下, ZSM-5沸石的不同晶面散射强度变化(a), 由散射信号结构精修获得Al原子在不同T位的占有率(b), 中子散射获得ND3在ZSM-5沸石Brønsted酸位上的吸附构型图(c), 及利用15N MAS NMR (d) 15N-27Al S-RESPDOR (e~f)得到不同酸位点吸附的NH3及其与27Al核之间的距离[147]

Figure 11. Soft X-ray scattering intensity changes of different ZSM-5 zeolite crystal facets under varying energy conditions (resonant, non-resonant) (a); Al atom site occupancies at different T-sites obtained by refinement of scattering signals (b); neutron scattering-derived adsorption configuration of ND3 on ZSM-5 zeolite Brønsted acid sites (c); and NH3 adsorbed on different acid sites and their distances to 27Al nuclei obtained using 15N MAS NMR (d) and 15N-27Al S-RESPDOR (e~f). (Reproduced from Guangchao Li et al., Science, doi:10.1126/science.adq6644 [2025], AAAS.)

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沸石铝分布精准调控: 策略、表征与展望

Precise Control of Aluminum Distribution in Zeolites: Strategies, Characterization, and Perspectives

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