沸石基工业多组元催化剂的结构设计及组元间相互作用研究★

doi:10.6023/A25050163

化学学报 ›› 2025, Vol. 83 ›› Issue (9): 1072-1088.DOI: 10.6023/A25050163 上一篇下一篇

综述

沸石基工业多组元催化剂的结构设计及组元间相互作用研究^★

徐亦璞^a^,^b, 徐舒涛^b^,^*(), 魏迎旭^b, 阎子峰^a^,^*(), 刘中民^b

^a 中国石油大学(华东) 重质油全国重点实验室青岛 266580
^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大连 116023

投稿日期:2025-05-12 发布日期:2025-07-04

作者简介:

徐亦璞, 中国石油大学(华东)重质油全国重点实验室博士生, 中国科学院大连化学物理研究所联合培养博士生. 本科毕业于中国石油大学(华东)化学化工学院. 主要研究方向为多级孔沸石的合成及催化应用和沸石催化剂的扩散及动力学.

徐舒涛, 中国科学院大连化学物理研究所研究员, 优青. 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. 现为大连化学物理研究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, 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.

魏迎旭, 中国科学院大连化学物理研究所研究员. 1993年于上海交通大学获得学士学位, 2001年于中国科学院大连化学物理研究获得博士学位, 毕业后在中国科学院大连化学物理研究所工作, 期间于2003~2004年赴比利时Namur大学进行博士后研究. 现为低碳催化技术国家工程研究中心研究员, 催化反应机理和新反应探索研究组组长. 从事分子筛催化、甲醇制烯烃、烷烃转化及二氧化碳耦合烷烃转化制高值化学品的基础和应用研究. 入选科技部创新人才推进计划中青年科技创新领军人才、大连化学物理研究所首席研究员及张大煜优秀学者等.

阎子峰, 中国石油大学(华东)重质油全国重点实验室教授. 于兰州大学化学系获得学士、硕士学位, 于中国科学院兰州化学物理研究所获得博士学位. 目前为中国石油大学(华东)二级教授, 同时兼任中国化学会催化委员会委员、中国化学会分子筛委员会委员、中国化工学会理事及山东省化学化工学会常务理事兼催化专业委员会主任委员. 二十多年来, 主持承担30余项国家/山东省重点研发项目、国家自然科学基金重点项目等国家、省部级重大研究课题和攻关项目, 承担5项与Shell、KACST等的国际合作项目, 先后实现多项技术的工业化. 主要研究方向为催化材料与催化剂的结构设计、定向合成及催化应用, 新型电极材料及新能源领域应用研究.

刘中民, 中国工程院院士, 中国科学院大连化学物理研究所所长、低碳催化技术国家工程研究中心主任、国家能源低碳催化与工程研发中心主任. 1983年于郑州大学获得学士学位, 1986年于中国科学院大连化学物理研究所获得硕士学位业, 1990年在中国科学院大连化学物理研究所获得博士学位, 1996年3月至1996年10月, 在法国科研中心CNRS418 (Montpellier)开展博士后工作. 刘中民院士长期从事应用催化研究, 作为技术总负责人合作完成了多项创新成果并实现产业化. 完成了世界首次甲醇制烯烃(DMTO)技术工业性试验及首次工业化, 完成了世界首套10万吨/年煤基乙醇(DMTE)工业示范项目, 引领了我国新兴煤制大宗化学品和清洁燃料产业的发展.

^★ “中国青年化学家”专辑.

基金资助:
国家自然科学基金(22241801); 国家自然科学基金(22288101); 国家自然科学基金(22022202); 国家自然科学基金(22032005); 大连市杰出青年科学家基金(2021RJ01); 辽宁国际联合实验室(2024JH2/102100005); 中国石油大学(华东)研究生创新基金及中央高校基本科研业务费专项资金(24CX04004A)

Studies on Structural Engineering and Intercomponent Interactions of Zeolite-Based Industrial Multicomponent Catalysts^★

Yipu Xu^a^,^b, Shutao Xu^b^,^*(), Yingxu Wei^b, Zifeng Yan^a^,^*(), Zhongmin Liu^b

^a State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580
^b National Engineering Research Center of Lower-Carbon Catalysis Technology, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023

Received:2025-05-12 Published:2025-07-04
Contact: * E-mail: xushutao@dicp.ac.cn;zfyancat@upc.edu.cn
About author:
^★ For the VSI “Rising Stars in Chemistry”.
Supported by:
National Natural Science Foundation of China(22241801); National Natural Science Foundation of China(22288101); National Natural Science Foundation of China(22022202); National Natural Science Foundation of China(22032005); Dalian Outstanding Young Scientist Foundation(2021RJ01); Liaoning International Joint Laboratory Project(2024JH2/102100005); Innovation Fund Project for Graduate Student of China University of Petroleum (East China) and the Fundamental Research Funds for the Central Universities(24CX04004A)

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摘要/Abstract

催化领域的最终目标是在工业技术层面提高催化效率. 工业催化剂通常是由沸石组元与基质和粘结剂等“非沸石组元”共同构成的多组元多活性敏感结构复合体, 其性能不仅取决于单一组元的性质, 更受组元间相互作用的显著影响. 然而, 实验室的大量研究多聚焦于沸石组元的调控, 而忽视了非沸石组元的影响及其与沸石组元的相互作用, 导致工业催化剂的设计与实际性能之间存在显著差异. 对于沸石-非沸石组元间的结构设计及各组元间结构-性质-功能关系的理解在很大程度上被忽视. 本综述着重强调了工业沸石-非沸石一体化催化剂组元间相互作用的复杂性. 以典型的催化裂解催化剂为例, 分析了催化裂化多组元催化剂的等级特征及其等级结构协同接力催化功能. 重点探讨了沸石-非沸石组元间的三类相互作用机制: (1)铝物种迁移及其对酸性质的调控; (2)阳离子交换及金属在组元间落位的距离效应对酸性位点的动态调节; (3)组元间孔道匹配联通性对扩散效率的影响. 最后, 展望了多组元催化剂设计的未来方向, 强调通过先进表征技术与计算模拟揭示组元相互作用的微观机制, 为开发高效、低能耗且环境友好的催化裂化催化剂提供理论指导.

关键词: 沸石催化材料, 工业催化剂, 催化裂化, 组元相互作用, 扩散

The ultimate goal of catalysis research is to enhance catalytic efficiency under industrial conditions. Industrial catalysts are typically complex multicomponent systems, comprising zeolitic components integrated with non-zeolitic components such as silica, alumina, amorphous aluminosilicate, clay, etc. Their catalytic performance is not only determined by the intrinsic properties of each component, but also is strongly influenced by the nature and extent of intercomponent interactions. However, most academic studies have focused primarily on tailoring zeolitic components, while the critical roles of non-zeolitic components and their interactions with zeolitic components were overlooked. This oversight has contributed to a persistent gap between laboratory research and practical industrial catalyst design. This review focuses on the structural integration and functional synergy between zeolitic and non-zeolitic components in industrial catalysts, with particular emphasis on fluid catalytic cracking systems as a representative case. We discuss the hierarchical and cooperative behavior of multicomponent catalytic architectures and highlight three key types of zeolitic and non-zeolitic components interactions: (1) aluminum species migration and redistribution and its influence on Brønsted and Lewis acidity; (2) cation exchange and proximity-induced modulation of acid sites between components; and (3) pore network matching and interconnectivity, which critically influence molecular diffusion and transport efficiency. By establishing correlations of structure-property-reactivity between the interface of zeolitic and non-zeolitic components, this review provides a conceptual framework to better understand and control these complex systems. We further propose future directions for the rational design of integrated industrial catalysts, emphasizing the use of advanced characterization techniques and computational simulations to unravel microscopic interaction mechanisms. These insights are expected to guide the development of more efficient, energy-saving, and environmentally benign catalytic materials for industrial applications.

Key words: zeolite catalytic material, industrial catalyst, fluid catalytic cracking, intercomponent interaction, diffusion

引用此文

徐亦璞, 徐舒涛, 魏迎旭, 阎子峰, 刘中民. 沸石基工业多组元催化剂的结构设计及组元间相互作用研究^★[J]. 化学学报, 2025, 83(9): 1072-1088.

Yipu Xu, Shutao Xu, Yingxu Wei, Zifeng Yan, Zhongmin Liu. Studies on Structural Engineering and Intercomponent Interactions of Zeolite-Based Industrial Multicomponent Catalysts^★[J]. Acta Chimica Sinica, 2025, 83(9): 1072-1088.

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图/表 12

图1. 炼油化工行业发展现状: (a) OPEC世界石油展望; (b)炼油能力数据表(数据统计来源于国家统计局)及(c)典型的炼油＋化工工艺路线(来源于UOP).

Figure 1. Current status of the refining and petrochemical industry: (a) global energy outlook by OPEC, (b) refining capacity data (sourced from the National Bureau of Statistics of China), and (c) typical integrated refining and petrochemical process flow (sourced from UOP)

图2. 催化裂化催化剂的典型结构组成[8]

图3. 面向低碳烯烃生产的理想催化裂化一体化催化剂的结构与组成

Figure 3. Structure and composition of integrated catalysts for low-carbon olefin-oriented catalytic cracking

图4. 工业催化剂中沸石与非沸石组元之间典型的相互作用类型[34]

图5. 组元间相互作用导致的新酸性位点的生成[42-43]: (a, b)沸石及其挤出物上CO吸附前后的差异光谱[43][(a) OH区, (b) CO区]及(c)沸石挤出物的27Al-{29Si} J-HMQC NMR谱图[42]

Figure 5. Formation of new acid sites induced by intercomponent interactions[42-43]: (a, b) difference spectra before and after CO saturation on zeolite and its extrudates[43] [(a) OH region (b) CO region] (Copyright 2020, with permission from Elsevier) and (c) 27Al-{29Si} J-HMQC NMR spectra on extrudates[42] (Copyright 2021, American Chemical Society)

图6. 二氧化硅作为粘结剂对催化剂酸性特征的影响[55-57]: (a) ZSM-5沸石及SiO2(左图)或Al2O3(右图)非沸石组元复合催化剂的三维共聚焦荧光显微镜图像[55]、(b)复合催化剂的27Al NMR谱图[56]及(c) NH3吸附的FT-IR光谱在不同多组元催化剂上(NaY-SiO2, NaY, SiO2[57])

Figure 6. Effect of silica as a binder on the acidity of catalysts[55-57]: (a) 3D confocal fluorescence microscopy images of the ZSM-5-binder-bound pellets combined with either SiO2 (left) or Al2O3 (right) as non-zeolitic components[55] (Copyright 2019, Bert M. Weckhuysen, Martijn Burgers, Anton-Jan Bons, et al. Published by Wiley-VCH Verlag GmbH & Co. KGaA), (b) 27Al solid state MAS NMR of multicomponent catalysts[56] (Copyright 2018 Elsevier B. V. All right reserved), and (c) FT-IR of NH3 adsorbed on different multicomponent catalyst (NaY-SiO2, NaY, and SiO2)[57] (Copyright 2015, American Chemical Society)

图7. 金属阳离子在沸石与非沸石组元之间的迁移: (a)不同催化剂(多级孔ZSM-5与凹凸棒、HCl处理的凹凸棒土、高岭土和MgO掺杂高岭土的混合物)上的MTH反应寿命[64]、(b)对比相应物理混合催化剂的平均产物选择性的差异[64]及(c)沸石基成型催化剂早期失活阶段的可视化共聚焦荧光显微镜(CFM)图像[66]

Figure 7. Migration of metal cations between zeolitic and non-zeolitic components: (a) MTH lifetime over milled hierarchical ZSM-5 admixtures with attapulgite, HCl-treated attapulgite, kaolin, and MgO-doped kaolin,[64] (b) differences in average product selectivity compared with respect to the corresponding physical mixtures,[64] (Copyright 2014, American Chemical Society) and (c) visualizing early stages of deactivation in zeolite-based shaped catalyst bodies by confocal fluorescence microscopy (CFM) images[66] (Copyright 2023 The Nikolaos Nikolopoulos, Luke A. Parker, Maurits W. Vuijk, Bert M. Weckhuysen. Published by Elsevier Inc)

图8. 金属颗粒在整体催化剂上分布位点的影响: (a)正庚烷转化率与反应温度的关系及(b)总C7异构体和裂解产物的产率[72]以及(c)组元间纳米尺度的邻近对加氢裂化活性和选择性的影响[73]

Figure 8. Effect of metal particle deposition sites on the performance of composite catalysts: (a) n-heptane conversion against the reaction temperature, and (b) yields of total C7 isomers and cracking products[72] (Copyright 2019 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim) and (c) impact of nanoscale intimacy on hydrocracking activity and selectivity[73] (Copyright 2015, Springer Nature Limited)

图9. 非沸石组元的引入对整体催化剂的孔梯度影响: (a)非沸石组元的引入使得整体催化剂的孔梯度重排[4]、(b)构建从大孔到微孔多尺度孔径大小匹配的多孔材料, 提高质量传输[22]及(c)组元间孔径匹配方面存在强扩散限制[80]

Figure 9. Effect of incorporating non-zeolitic components on the pore hierarchy of the overall catalyst: (a) pore hierarchy reorganization induced by non-zeolitic components[4] (Copyright 2019, American Chemical Society), (b) construction of multiscale pores with well-matched pore sizes from macropores to micropores enhances mass transport[22] (Copyright 2022, Sun, Ming-Hui; Gao Shu-shu 2022. Published by Oxford University Press on behalf of China Science Publishing) and (c) significant diffusion limitations arise from poor pore-size matching between components

图10. (a)沸石组元与非沸石组元孔道取向引起的连通程度改变[81,84]示意图(左图为沸石组元(蓝)与非沸石组元(粉)的微介孔道取向一致, 右图为沸石组元(蓝)与非沸石组元(粉)的微介孔道取向不一致)、(b)频率相应(FR)技术对沸石-非沸石界面阻力的识别[81]及(c)由沸石晶体孔隙堵塞引起的表面传质阻力[84]

Figure 10. (a) Schematic illustration of pore interconnectivity alteration induced by orientation mismatch between zeolitic and non-zeolitic components[81,84] [Left panel shows aligned orientation between the micropores of the zeolitic component (blue) and the mesopores of the non-zeolitic component (pink). Right panel shows a misaligned pore orientation between the zeolitic and non-zeolitic components], (b) frequency response (FR) technique for identifying zeolitic and non-zeolitic components interfacial resistance[81] (Copyright © 2014 Published by Elsevier B.V. All rights reserved), and (c) surface mass transfer resistance caused by blocked pore openings on zeolite crystals[84] (Copyright 2011 Aptara Inc. All rights reserved)

图11. 沸石-非沸石组元模型催化剂孔道匹配联通性对扩散及反应动力学的影响[34]: (a) HP 129Xe NMR对组元间扩散行为的识别、(b)时间分辨原位红外光谱对多组元扩散系数的测试及(c)催化效率因子的评估

Figure 11. Crucial roles of pore interconnectivity between zeolitic and non-zeolitic components in enhancing diffusion and catalytic efficiency[34]: (a) Identification of multicomponent hierarchical pore network connectivity by HP 129Xe NMR, (b) relating pore interconnectivity to diffusion in multicomponent model catalysts by time-resolved rapid-scan in situ FTIR technology, and (c) catalytic efficiency assessment of multicomponent model catalysts (Copyright 2025, American Chemical Society)

图12. (a)沸石组元与非沸石组元空间相对位置分布导致的扩散路径改变示意图[75-76,95](左图为非沸石组元的填充较为松散的情况; 右图为非沸石组元的填充相对较为紧密的情况)、(b)客体分子在纳米沸石中的扩散路径以及表面覆盖硅球的影响[75]及(c, d)沸石组元表面质量传输[76,95]

Figure 12. (a) Schematic of the effect of the spatial distribution between zeolitic and non-zeolitic components on diffusion pathways[75-76,95] (The left panel illustrates a loosely packed configuration of non-zeolitic components, whereas the right panel shows more uniformly coated), (b) guest molecules in nano-zeolite and the impact of surface covering with small silica particles[75]. (Copyright 2019, Zhou, Jian; Fan, Wei 2019. Published by Oxford University Press on behalf of China Science Publishing) and (c, d) surface barrier schemes for mass transport in zeolitic component[76,95] (Copyright 2021, Shen Hu, Junru Liu, Guanghua Ye, et al. Angewandte Chemie International Edition published by Wiley VCH GmbH. Copyright 2011, American Chemical Society)

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沸石基工业多组元催化剂的结构设计及组元间相互作用研究^★

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沸石基工业多组元催化剂的结构设计及组元间相互作用研究★

Studies on Structural Engineering and Intercomponent Interactions of Zeolite-Based Industrial Multicomponent Catalysts★

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沸石基工业多组元催化剂的结构设计及组元间相互作用研究^★

Studies on Structural Engineering and Intercomponent Interactions of Zeolite-Based Industrial Multicomponent Catalysts^★