CaAl-LDH层板金属元素同晶取代构建高密度单原子催化剂用于N-杂芳烃选择性加氢

doi:10.1016/S1872-2067(24)60217-2

催化学报 ›› 2025, Vol. 70: 353-362.DOI: 10.1016/S1872-2067(24)60217-2

CaAl-LDH层板金属元素同晶取代构建高密度单原子催化剂用于N-杂芳烃选择性加氢

贺捷婷^a, 梁瑜^b, 赵斌彬^c, 刘雷^a^,^*(), 何迁^c^,^*(), 王定胜^d, 董晋湘^a^,^*()

^a太原理工大学化学与化工学院, 山西省化学产品工程重点实验室, 山西太原 030024, 中国
^b山西农业大学植物保护学院, 山西晋中 030801, 中国
^c新加坡国立大学材料科学与工程系, 新加坡
^d清华大学化学系, 北京 100084, 中国

收稿日期:2024-10-22 接受日期:2024-12-16 出版日期:2025-03-18 发布日期:2025-03-20
通讯作者: * 电子信箱: liulei@tyut.edu.cn (刘雷),mseheq@nus.edu.sg (何迁),dongjinxiangwork@hotmail.com (董晋湘).
基金资助:
国家自然科学基金(22478276);国家自然科学基金(21978194);山西省重点研发计划(202102090301005);山西省科技创新团队专项资金(201705D131028-9);新加坡研究基金会(NRF-NRFF11-2019-0002)

Isomorphous substitution in CaAl-hydrotalcite to construct high density single-atom catalysts for selective N-Heteroarene hydrogenation

Jieting He^a, Yu Liang^b, Binbin Zhao^c, Lei Liu^a^,^*(), Qian He^c^,^*(), Dingsheng Wang^d, Jinxiang Dong^a^,^*()

^aShanxi Key Laboratory of Chemical Product Engineering, College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China
^bCollege of Plant Protection, Shanxi Agricultural University, Jinzhong 030801, Shanxi, China
^cDepartment of Materials Science and Engineering, National University of Singapore, Singapore
^dDepartment of Chemistry, Tsinghua University, Beijing 100084, China

Received:2024-10-22 Accepted:2024-12-16 Online:2025-03-18 Published:2025-03-20
Contact: * E-mail: liulei@tyut.edu.cn (L. Liu),mseheq@nus.edu.sg (Q. He),dongjinxiangwork@hotmail.com (J. Dong).
Supported by:
National Natural Science Foundation of China(22478276);National Natural Science Foundation of China(21978194);Key Research and Development Program of Shanxi Province(202102090301005);the special fund for Science and Technology Innovation Teams of Shanxi Province(201705D131028-9);National Research Foundation (NRF) Singapore, under its NRF Fellowship(NRF-NRFF11-2019-0002)

摘要/Abstract

摘要：

单原子催化剂(SACs)具有与均相催化剂类似的原子分散活性位点, 是多相催化与均相催化之间的重要桥梁. 通过调整活性金属位点的配位环境和载体的表面性质,可以显著提高单原子催化剂的反应活性和选择性. 然而, SACs的工业应用面临着巨大挑战. 例如, 需要开发能够适应各种载体和活性金属的通用合成方法,并且在这些载体上实现高负载量且具有热稳定的金属单原子. 因此, 迫切需要探索新的合成策略来解决这些问题, 这对于推动SACs领域的发展具有重要意义.

本文提出了一种创新策略用于合成SACs. 该方通过金属元素同晶置换, 在CaAl-LDH上构建了高密度的SACs, 实现了Rh, Ru, Pd等贵金属的原子级分散. 利用CaAl-LDH层间Ca²⁺的可交换性, 将Rh³⁺引入CaAl-LDH层中, 成功合成了高负载量的Rh单原子, 同时突破了传统金属负载的极限. 这些催化剂在喹啉的选择性氢化反应中展现出卓越的性能及良好的稳定性, 在温和条件下对1,2,3,4-四氢喹啉(Py-THQ)的合成中, 显示出高达99.0%的选择性. 同时也证明了其在N杂环芳烃氢化反应中的广泛适用性, 这对于液态有机氢的储存具有重要意义. 实验结果与DFT计算结果表明, CaAl-LDH中孤立Rh位点更倾向于吸附喹啉的含氮环一侧, 从而实现了对Py-THQ的高选择性. 此外, 通过CO-漫反射红外光谱、X射线光电子能谱和X射线吸附精细结构等技术对催化剂的结构和化学状态进行了详细的表征, 进一步证实了Rh物种在CaAl-LDH中的单原子分散状态. 获得的表征数据不仅验证了Rh单原子催化剂的结构特征, 还为深入理解其催化机制提供了重要依据, 为贵金属单原子催化剂的设计和应用提供了新的思路.

综上, 本文在金属氧化物载体上合成高负载量、热稳定的金属SACs方面取得了显著进展. 我们不仅提出了一种新的方法来合成高密度单原子催化剂, 而且拓宽了其在绿色化学过程中的应用前景. 此外, 本研究还为催化剂的设计和应用提供了理论指导.

关键词: 同晶置换, 高负载, 单原子催化剂, 选择性加氢

Abstract:

Metal oxides as support for constructing precious metal single-atom catalysts hold great promise for a wide range of industrial applications, but achieving a high-loading of thermally stable metal single atoms on such supports has been challenging. Herein, we report an innovative strategy for the fabrication of high-density single-atoms (Rh, Ru, Pd) catalysts on CaAl-layered double hydroxides (CaAl-LDH) via isomorphous substitution. The Rh species have occupied Ca²⁺ vacancies within CaAl-LDH laminate by ion-exchange, facilitating a substantial loading of isolated Rh single-atoms. Such catalysts displayed superior performance in the selective hydrogenation to quinoline, pivotal for liquid organic hydrogen storage, and the universality for the hydrogenation of N-heterocyclic aromatic hydrocarbons was also verified. Combining the experimental results and density functional theory calculations, the pathway of quinoline hydrogenation over Rh₁CaAl-LDH was proposed. This synthetic strategy marks a significant advancement in the field of single-atom catalysts, expanding their horizons in green chemical processes.

Key words: Isomorphous substitution, High-loading, Single‐atom catalyst, Selective hydrogenation

贺捷婷, 梁瑜, 赵斌彬, 刘雷, 何迁, 王定胜, 董晋湘. CaAl-LDH层板金属元素同晶取代构建高密度单原子催化剂用于N-杂芳烃选择性加氢[J]. 催化学报, 2025, 70: 353-362.

Jieting He, Yu Liang, Binbin Zhao, Lei Liu, Qian He, Dingsheng Wang, Jinxiang Dong. Isomorphous substitution in CaAl-hydrotalcite to construct high density single-atom catalysts for selective N-Heteroarene hydrogenation[J]. Chinese Journal of Catalysis, 2025, 70: 353-362.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60217-2

https://www.cjcatal.com/CN/Y2025/V70/I3/353

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Fig. 1. (a) Illustration scheme of synthetic procedure of 1Rh1CaAl-LDH catalyst. (b) The concentration of Ca ions and Rh ions in solution. (c) content of Rh in 1Rh1CaAl-LDH catalyst of exchange using CaAl-LDH.

Fig. 2. Structural characterization of single-atom Rh with xRh1CaAl-LDH. (a) XRD patterns of CaAl-LDH and xRh1CaAl-LDH samples. (b) In-situ DRIFTS spectra of CO adsorbed on xRh1CaAl-LDH catalysts. (c) Nitrogen adsorption-desorption isotherms of the catalysts. HRTEM image of 1Rh1CaAl-LDH (d) and 4Rh1CaAl-LDH (e). (f) STEM-EDS elemental mapping images of 4Rh1CaAl-LDH. The k2-weighted Fourier transform spectra in R space (g) and Rh K-edge XANES spectra (h) of catalysts. (i) Wavelet transform (WT) of the EXAFS spectrum of 4Rh1CaAl-LDH.

Fig. 3. Rh 3d (a) and Ca 2p (b) XPS spectra of 1Rh1CaAl-LDH catalyst. The k2-weighted Fourier transform spectra in R space of 0.8Pd1CaAl-LDH (c) and 1.6Ru1CaAl-LDH (d). Wavelet transform (WT) of the EXAFS spectrum of 0.8Pd1CaAl-LDH (e) and 1.6Ru1CaAl-LDH (f).

Fig. 4. (a) Possible products of the quinoline hydrogenation. (b) metal-normalized activity (per unit mass of Rh) of the xRhCaAl-LDH in hydrogenation of quinoline (Temperature: 80 °C; H2 Pressure: 2 MPa). (c) Effect of reaction time on hydrogenation activity with 1Rh1CaAl-LDH. (d) Hydrogenation properties of different noble metals catalysts (Reaction times are respectively: 5, 2, 1 h). (e) The comparison of noble metal catalyst performance.

Fig. 5. (a) Quinoline adsorption energies (ΔEads) of C=N over Rh1CaAl-LDH and Rh10/CaAl-LDH. (b) Proposed route for quinoline hydrogenation on Rh1CaAl-LDH.

Table 1 The catalytic hydrogenation of functional group substituted quinoline and other N-heteroarenes over 1Rh1CaAl-LDH catalyst.

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CaAl-LDH层板金属元素同晶取代构建高密度单原子催化剂用于N-杂芳烃选择性加氢

Isomorphous substitution in CaAl-hydrotalcite to construct high density single-atom catalysts for selective N-Heteroarene hydrogenation

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