In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application★

doi:10.6023/A23040177

Acta Chimica Sinica ›› 2023, Vol. 81 ›› Issue (8): 937-948.DOI: 10.6023/A23040177 Previous Articles Next Articles

Special Issue: 庆祝《化学学报》创刊90周年合辑

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原位刻蚀调控多级孔分子筛策略及其应用进展^★

洪梅^*(), 高金强, 李彤, 杨世和^*()

广东省纳米微米材料研究重点实验室省部共建肿瘤化学基因组学国家重点实验室北京大学深圳研究生院化学生物学与生物技术学院深圳 518055

投稿日期:2023-04-28 发布日期:2023-09-14

作者简介:

洪梅, 北京大学深圳研究生院副教授、广东省纳米微米材料研究重点实验室副主任. 2002年在南京大学获得硕士学位, 2007年在美国科罗拉多大学博尔德分校获得博士学位, 2007~2008年在美国加州大学戴维斯分校开展博士后研究, 2008~2013年在瑞士龙沙集团担任研发技术经理, 2014年起任北京大学博士生导师. 研究方向: (1)多孔纳米微米材料的设计与合成; (2)功能复合材料的关键技术; (3)分离、催化产品的开发和应用.

高金强, 北京大学深圳研究生院助理研究员. 2020年在日本新澙大学获得博士学位, 2020~2022年在北京大学深圳研究生院开展博士后研究, 2022年起任职于北京大学深圳研究生院和广东省纳米微米材料研究重点实验室. 研究方向: (1)膜分离, 及纳微结构调控与结晶理论; (2)电解水催化剂的设计和研究.

李彤, 北京大学深圳研究生院研究助理. 2022年起任职于北京大学深圳研究生院和广东省纳米微米材料研究重点实验室. 研究方向: 多孔纳米微米材料的合成与应用.

杨世和, 教育部长江讲座教授, 国家杰出青年(海外), 深圳市孔雀团队带头人, 现任北京大学深圳研究生院教授、香港科技大学兼职教授、广东省纳米微米材料研究重点实验室主任. 长期从事团簇和低维纳米材料的化学物理基础和应用研究. 近年来, 研究着重于发展和集成新型可持续材料以实现高效光电及化学转换. 已在国际权威期刊上发表论文690余篇, 被 SCI引用60000余次, H-index 128 (Google Scholar), 连续多年被评为科睿唯安(Clarivate Analytics)年度“全球Top1%高被引学者”, 担任多个国际期刊的编委或顾问, 曾两次获得国家自然科学二等奖, 授权国际国内发明专利数十项.

^★庆祝《化学学报》创刊90周年.

基金资助:
项目受国家自然科学基金(21972006); 深圳市科技计划(JCYJ20200109140421071); 深圳市科技计划(JSGG20211029095546003)

In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application^★

Mei Hong(), Jinqiang Gao, Tong Li, Shihe Yang()

Guangdong Provincial Key Laboratory of Nano-Micro Materials Research, State Key Laboratory of Chemical Oncogenomics, School of Chemical Biology & Biotechnology, Peking University Shenzhen Graduate School (PKUSZ), Shenzhen 518055, China

Received:2023-04-28 Published:2023-09-14
Contact: *E-mail: hongmei@pku.edu.cn; chsyang@pku.edu.cn
About author:
^★Dedicated to the 90th anniversary of Acta Chimica Sinica.
Supported by:
National Natural Science Foundation of China(21972006); Shenzhen Science and Technology Program(JCYJ20200109140421071); Shenzhen Science and Technology Program(JSGG20211029095546003)

Zeolite molecular sieve is by far the most widely used porous material with the greatest contribution to society. Hierarchical zeolites, which possess dual advantages of large diffusion coefficient and high activity, are increasingly important as catalysts and adsorbents in many chemical processes. A class of organic mesoporogens named organic mesopore generating agents (OMeGAs), such as amino acids, phenols, and azoles were found to produce intracrystalline mesopores by one pot method, wherein the nucleophilic etching effect of the in-situ generated anions, including oxyanions, nitranions, or carbanions, plays the key role. By adding mild OMeGAs in-situ into the reaction solution of zeolite synthesis, the nucleophilic etching assisted growth could overcome the energy-intensive mesoscale template calcination associated with the “bottom-up” strategy and the zeolite structure destruction of the “top-down” post-synthetic strategy. The interplay between in-situ etching and growth on the early precursor or nuclei has enabled effective control over crystallinity, size, morphology, mesopores, and performance of zeolites. In this account, the existing preparation strategies of hierarchical zeolite are first briefly introduced. Then, the in-situ etching-assisted growth strategies are discussed in detail, including the selection of mild etchant OMeGAs, mechanism and advantages of the etching-assisted zeolite crystallization process. Finally, the application of in-situ etching-manipulated hierarchical zeolite is summarized.

Key words: hierarchical zeolite, small organic molecules, mesopore generating agent, nucleophilic etching, synthesis

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Mei Hong, Jinqiang Gao, Tong Li, Shihe Yang. In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application^★[J]. Acta Chimica Sinica, 2023, 81(8): 937-948.

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Fig. & Tab. 9

Figure 1. Summary of “bottom-up” and “top-down” approaches to hierarchical zeolites[5]

Figure 2. In-situ etching assisted growth of hierarchical zeolites with strong acid or base. Left shows excess HF assisted macroporous SAPO-34[52], scale bars in b1 and c1 represent 5 μm, in b2 and c2 represent 1 μm; right shows excess NaOH and TPA+ assisted hierarchical ZSM-5[53], scale bars from a to d represent 500 nm, 100 nm, 200 nm, and 20 nm respectively

Figure 3. Summary of in-situ etching modulated hierarchical zeolites with mild organic small molecules. (a~d) SEM images: (a) threonine mediated mesoporous A-type zeolite[55], (b) L-carnitine mediated mesoporous Y-type zeolite[56], (c) phenol mediated mesoporous ZSM-5 zeolite[57], (d) 3-hydroxy-4-triethylaminobutyric acid mediated mesoporous SAPO-34 zeolite[58]; (e~h) cross-sectional TEM images with corresponding high resolution TEM images and selected area electron diffraction: (e) mesoporous A[55], (f) mesoporous Y[56], (g) mesoporous ZSM-5[57], some mesoporous areas and positions are represented by dashed line boxes and arrows, (h) mesoporous SAPO-34[58], some mesoporous areas are represented by dashed line boxes

Figure 4. pKa values of small organic molecules play an important role in the mesopore formation of A-type zeolite: (a) small molecules with pKa value less than the pH value of the synthetic mixture can dissociate to anions in the zeolite synthesis environment, thus generating mesoporous; (b) OMeGA reagents include precursors of oxyanions, carbanions and nitranions, while organic alcohols or amines that cannot be deprotonated in-situ do not generate mesoporous zeolite; (c) energy profiles and reaction paths of desilication (deSi, blue) and dealumination (deAl, red) by alanine attack[54]

Figure 5. Regulation of ZSM-5 synthesis with in-situ etchant of homologous para-substituted phenols by changing functional groups at para- position[61]

Figure 6. Time-dependent spectroscopies confirming the etching process during phenol mediated ZSM-5 crystallization. (a) FTIR spectra; (b) 27Al MAS NMR spectra, inset shows time dependent change in full width at half maximum; (c) 29Si MAS NMR spectra, inset shows time dependent change in ratio of Q4/(Q2＋Q3)[57]

Figure 7. Effect of (a) pKa values and (b) nucleophilicity N indexes of the added para-substituted phenols on the resulting ZSM-5 crystal sizes, and (c~j) the corresponding SEM images[57]

Figure 8. The proposed mechanism highlighting the effect of phenolic compounds during ZSM-5 synthesis[61]

Figure 9. Summarized research progress of "bottom-up" and "top-down" methods for the preparation of hierarchical zeolite. Nucleophilic etching growth of zeolites using OMeGA molecules could potentially bridge the "bottom-up" and "top-down" methods with etching on diminishing nuclei to obtain better quality hierarchical molecular sieve

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原位刻蚀调控多级孔分子筛策略及其应用进展^★

In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application^★

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原位刻蚀调控多级孔分子筛策略及其应用进展★

In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application★

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原位刻蚀调控多级孔分子筛策略及其应用进展^★

In-situ Etching Strategy for Manipulation of Hierarchical Zeolite and Its Application^★