高硅小晶粒Y型分子筛的合成研究进展★

doi:10.6023/A26070258

化学学报 ›› 2026, Vol. 84 ›› Issue (8): 1355-1364.DOI: 10.6023/A26070258 上一篇下一篇

综述

高硅小晶粒Y型分子筛的合成研究进展^★

陈雪娇^a, 刘小琦^a, 魏麟骄^a^,^b, 白鹏^a^,^*(), 阎子峰^a^,^*()

^a 中国石油大学(华东)化学化工学院重质油全国重点实验室化学化工学院重质油全国重点实验室青岛 266580
^b 山东石油化工学院山东省绿色电氢科学与技术重点实验室山东省绿色电氢科学与技术重点实验室东营 257061

投稿日期:2026-07-22 发布日期:2026-08-26

作者简介:

陈雪娇, 中国石油大学(华东)化学化工学院2022级博士研究生. 主要研究方向为无机非金属多孔材料的制备及其在丙烷脱氢中的应用.

刘小琦, 中国石油大学(华东)重质油国家重点实验室博士研究生. 主要研究方向为长寿命水系锌离子电池的设计与电化学机理研究.

魏麟骄, 中国石油大学(华东)博士研究生, 山东石油化工学院讲师. 2012年获广西大学应用化学专业学士学位, 2016年获中国石油大学(华东)化学工程专业硕士学位. 主要研究方向为分子筛催化材料与水系锌离子电池.

白鹏, 中国石油大学(华东)化学工程学院教授, 博士生导师. 2009~2012年在新加坡科技研究局(A*STAR)下属的化学与工程科学研究院(ICES)任I级科学家. 长期从事高性能氧化铝粉体的制备、改性及催化性能研究, 尤其在氧化铝孔结构、晶相、结构缺陷、微观形貌、表面酸性调变等方面做了系统深入的探索. 近年来主持和参与国家自然科学基金重大项目、国家重点研发计划、国家自然科学基金青年基金、山东省自然科学基金面上基金、新加坡教育部和科技局科技研发项目等多个项目.

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.

^★“纪念兰州大学化学学科创建80周年”专辑

基金资助:
国家自然科学基金(22372197); 国家自然科学基金(22478431); 国家重点研发计划项目(2022YFA1503400)

Advances in Synthesizing High-Silica Small-Crystal Zeolite Y^★

Xuejiao Chen^a, Xiaoqi Liu^a, Linjiao Wei^a^,^b, Peng Bai^a^,^*(), Zifeng Yan^a^,^*()

^a State Key Laboratory of Heavy Oil Processing, College of Chemistry & Chemical Engineering, China University of Petroleum (East China), Qingdao 266580, China
^b Shandong Key Laboratory of Green Electricity & Hydrogen Science and Technology, Shandong Institute of Petroleum and Chemical Technology, Dongying 257061, China

Received:2026-07-22 Published:2026-08-26
Contact: *E-mail: baipeng@upc.edu.cn; zfyancat@upc.edu.cn
About author:
^★For the VSI “Celebration of 80th Anniversary of Chemistry in Lanzhou University”
Supported by:
National Natural Science Foundation of China(22372197); National Natural Science Foundation of China(22478431); National Key Research and Development Program of China(2022YFA1503400)

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摘要/Abstract

小晶粒(<1 μm), 尤其是纳米级(<100 nm) Y型分子筛, 因其独特的拓扑结构和优异的催化性能, 在石油炼制等领域具有巨大的商业潜力. 然而, 如何在纳米尺度下协同优化晶粒尺寸与骨架硅铝比(SAR, SiO₂/Al₂O₃物质的量比), 以兼顾高效传质与高水热稳定性, 仍是该领域面临的核心科学难题. 本综述重点介绍高硅小晶粒和纳米Y型分子筛的合成策略、脱铝机理及脱铝对材料性能的影响. 直接合成和后处理改性法的比较分析表明, 直接合成受到成核动力学和经济可行性的限制, 后处理脱铝仍是实现高硅铝比的主要工业方法. 此外, 本综述还深入分析了高温蒸汽诱导的骨架重组、SiCl₄同晶取代以及利用NH₄SiF₆液相脱铝-补硅的微观反应机制. 纳米Y型分子筛的后处理面临着特殊挑战: 高温蒸汽处理很容易引起晶粒聚合与结构坍塌. 气相超稳定法补硅效率较高, 但由于SiCl₄具有强腐蚀性, 对设备提出了严苛的要求. 类似地, 由于脱铝和补硅过程之间的动力学不平衡, 氟硅酸铵法会面临孔道堵塞和表面硅富集等问题. 此外, 本综述系统地阐明了脱铝过程对分子筛物化性质的双重影响. 具体来说, 适度的脱铝能诱导晶胞参数的各向异性收缩并提高酸强度, 而过度的脱铝往往会产生结构缺陷和骨架外铝(EFAl)物质. 因此, 未来的研究应集中在精确控制高硅纳米Y型分子筛的结晶过程和脱铝动力学上, 促进晶体尺寸与水热稳定性的协同优化, 推进高硅纳米Y型分子筛的工业化应用.

关键词: 纳米Y型分子筛, 高硅铝比, 脱铝机理, 水热稳定性

Small-crystal (<1 μm), particularly nano-sized (<100 nm) zeolite Y hold immense commercial potential in petroleum refining and related fields, owing to their unique topological structures and superior catalytic performance. However, synergistically optimizing crystallite size and framework silicon-to-aluminum ratio (SAR, SiO₂/Al₂O₃ molar ratio) at nanoscale to balance efficient mass transfer with high hydrothermal stability remains a core scientific challenge. This article focuses on the synthesis strategies for high-silica small-crystal and nano-sized zeolite Y, the mechanisms of post-synthesis dealumination, and the impacts on material properties. A comparative analysis of direct synthesis and post-treatment modification reveals that direct synthesis is constrained by nucleation kinetics and economic feasibility, whereas post-treatment dealumination remains the predominant industrial approach for achieving high SAR. Furthermore, this review provides an in-depth analysis of the microscopic reaction mechanisms underlying high-temperature steam-induced skeletal restructuring, isomorphous substitution via SiCl₄ vapor, and the liquid-phase dealumination-silicon replacement process utilizing NH₄SiF₆. However, post-treatment of nanocrystals presents specific challenges: high-temperature steam treatment can readily induce particle sintering and structural collapse. Although the vapor-phase super-stabilization method offers high silicon-incorporation efficiency, it imposes stringent requirements on equipment due to the corrosive nature of SiCl₄. Similarly, the ammonium fluorosilicate method often suffers from pore blockage and surface silicon enrichment due to the kinetic imbalance between dealumination and silica replacement. Additionally, this article systematically elucidates the dual effects of the dealumination process on the physicochemical properties of zeolites. Specifically, moderate dealumination can induce anisotropic contraction of unit cell parameters and enhance acid strength, whereas excessive dealumination tends to generate structural defects and extra-framework aluminum (EFAl) species. Therefore, future research should focus on precisely controlling dealumination kinetics and regulating the crystallization process of nano-sized zeolite Y. This will facilitate the syn-ergistic optimization of crystallite size and hydrothermal stability, ultimately advancing the industrial application of high-silica nano-sized zeolite Y.

Key words: nanosized zeolite Y, high silica-alumina ratio, dealumination mechanism, hydrothermal stability

引用此文

陈雪娇, 刘小琦, 魏麟骄, 白鹏, 阎子峰. 高硅小晶粒Y型分子筛的合成研究进展^★[J]. 化学学报, 2026, 84(8): 1355-1364.

Xuejiao Chen, Xiaoqi Liu, Linjiao Wei, Peng Bai, Zifeng Yan. Advances in Synthesizing High-Silica Small-Crystal Zeolite Y^★[J]. Acta Chimica Sinica, 2026, 84(8): 1355-1364.

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图/表 7

Figure 1. The cooperative OSDA blueprint using Ch and Na-15-crown-5 (CE complex) for high-silica FAU zeolite synthesis. The Al atoms in red are randomly inserted, with 3~4 Al per SOD cage. Reprinted with permission from ref. [29]. Copy right © 2021 Wiley-VCH GmbH

Figure 2. Schematic illustration of the formation mechanism for highly siliceous Faujasite-type zeolite by low charge density organic structure- directing agents (TMA+ & TBA+). Reprinted with permission from ref. [38]. Copy right © 2025 American Chemical Society

图3. 典型的高硅小晶粒Y型分子筛SY15.6的(a) SEM图像, (b) NH3-TPD, (c) 27Al和(d) 29Si MAS NMR谱图. (e) 1,3,5-三异丙基苯(TIPB)裂化性能图. 反应条件: T=160 ℃, WHSVTIPB=4.1 h−1. (f)正十二烷转化率及产物分布图. 反应条件: T=250 ℃, WHSVn-dodecane=50.0 h−1, TOS=2 min. 已获得参考文献[39]转载许可, 版权所有© 2020 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Figure 3. (a) SEM image, (b) NH3-TPD, (c) 27Al and (d) 29Si MAS NMR spectra of typical high-silica small-crystal zeolite Y (SY15.6); (e) 1,3,5-triisopropylbenzene (TIPB) cracking versus time on stream. Reaction conditions: T=160 ℃, WHSVTIPB=4.1 h−1; (f) N-dodecane conversion and products distribution. Reaction conditions: T=250 ℃, WHSVn-dodecane=50.0 h−1, TOS=2 min. Reprinted with permission from ref. [39]. Copy right © 2020 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Figure 4. Mechanism of the initiation of dealumination (Al—O bond breaking) by the attack in anti of a bridging Brønsted acid site by a water molecule in a zeolite. Reprinted with permission from ref. [82]. Copy right © 2024 American Chemical Society

图5. 气相超稳化脱铝过程示意图(黄色: Si原子, 粉色: Al原子, 红色: O原子, 绿色: Cl原子, 蓝色: Na原子)

Figure 5. Mechanism of two-step dealumination reaction in gas phase ultra-stabilization (Yellow: Si atom, pink: Al atom, red: O atom, green: Cl atom, blue: Na atom)

Figure 6. Defect generation in Y zeolite during dealumination and silicon incorporation via (NH4)2SiF6 treatment. Reprinted with permission from ref. [10]. Copy right © 2017 American Chemical Society

图7. (a) Y-MWAC的2D SQ-SQ1H同核偶极相关MAS核磁共振光谱. (b) Y-MWAC的2D DQ-SQ 27Al同核对应NMR光谱. (a)中用虚线框表示Y-MWAC中BAS与EFAl质子之间的交叉峰, 强度被放大了2倍. (a)中顶部和左侧显示天际线投影, 而(b)中顶部光谱显示一维27Al MAS核磁共振光谱作对比. 已获得参考文献[90]转载许可, 版权所有© 2025 The Author(s). ChemCatChem published by Wiley-VCH GmbH, 采用知识共享署名CC BY 4.0 授权. (c) Y和(d) USY的红外光谱图. (A) 723 K活化, (B)真空吸附吡啶并在423 K再次真空, (C)真空吸附2,6-二叔丁基吡啶并在423 K再次真空. 已获得参考文献[92]转载许可, 版权所有© 2021 Wiley-VCH GmbH

Figure 7. (a) 2D SQ-SQ 1H homonuclear dipolar correlation MAS NMR spectra of Y-MWAC. (b) 2D DQ-SQ 27Al homonuclear dipolar correlation NMR spectrum of Y-MWAC. Cross peaks between BAS and EFAl protons of Y-MWAC, denoted by dashed boxes in (a), have been scaled in intensity by a factor of 2. Top and left in (a) show skyline projections, whereas the top spectrum in (b) shows the 1D 27Al MAS NMR spectrum, for comparison. Reprinted with permission from ref. [90]. Copy right © 2025 The Author(s). ChemCatChem published by Wiley-VCH GmbH, Licensed under the Creative Commons Attribution CC BY 4.0. IR spectra of Y (c) and USY (d) after (A) activation at 723 K, (B) adsorption of Py and evacuation at 423 K under secondary vacuum, and (C) adsorption of DTBPy and evacuation at 423 K under secondary vacuum. Reprinted with permission from ref. [92]. Copy right © 2021 Wiley-VCH GmbH

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高硅小晶粒Y型分子筛的合成研究进展^★

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