缺陷UiO-66(Ce)负载的具有优化微环境和电子态的镍纳米颗粒用于高效烯烃加氢反应

doi:10.1016/S1872-2067(24)60284-6

催化学报 ›› 2025, Vol. 72: 344-358.DOI: 10.1016/S1872-2067(24)60284-6

缺陷UiO-66(Ce)负载的具有优化微环境和电子态的镍纳米颗粒用于高效烯烃加氢反应

李如硕^a, 班涛^a, 赵丹凤^a, 胡发杰^a, 林璟^a, 黄秀兵^a^,^*(), 陶志平^b^,^*(), 王戈^a^,^*()

^a北京科技大学材料科学与工程学院, 北京基因组工程材料高级创新中心, 北京分子与结构构建功能材料重点实验室, 北京 100083
^b中国石化石油化工科学研究院有限公司, 北京 100083

收稿日期:2024-12-15 接受日期:2025-02-06 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: xiubinghuang@ustb.edu.cn (黄秀兵),Taozp.ripp@sinopec.com (陶志平),gewang@ustb.edu.cn (王戈).
基金资助:
国家重点研发计划(2021YFB3500700);国家自然科学基金(51972024);广东省自然科学基金(2022A1515010185)

Defective UiO-66(Ce) supported Ni nanoparticles with optimized microenvironment and electronic state for efficient olefin hydrogenation reaction

Rushuo Li^a, Tao Ban^a, Danfeng Zhao^a, Fajie Hu^a, Jing Lin^a, Xiubing Huang^a^,^*(), Zhiping Tao^b^,^*(), Ge Wang^a^,^*()

^aBeijing Advanced Innovation Center for Materials Genome Engineering, Beijing Key Laboratory of Function Materials for Molecule & Structure Construction, School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China
^bSinopec Research Institute of Petroleum Processing Co., Ltd., Beijing 100083, China

Received:2024-12-15 Accepted:2025-02-06 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: xiubinghuang@ustb.edu.cn (X. Huang), Taozp.ripp@sinopec.com (Z. Tao), gewang@ustb.edu.cn (G. Wang).
Supported by:
National Key Research and Development Program of China(2021YFB3500700);National Natural Science Foundation of China(51972024);Natural Science Foundation of Guangdong Province(2022A1515010185)

摘要/Abstract

摘要：

金属负载型催化剂因其独特的几何和电子结构、电子金属-载体相互作用(EMSI)等特点, 在催化领域中展现了独特的优势. 金属有机框架(MOFs)具有孔隙丰富、表面积大和可达金属位点多等优点, 作为载体负载金属纳米颗粒(MNPs)活性组分(MNPs@MOFs), 可以有效提高MNPs的分散和稳定性, 有望构建高效的金属负载型催化剂. 缺陷工程可以有效调节MOFs载体的性质及EMSI, 从而调控甚至主导MNPs@MOFs的活性和稳定性. 调节剂诱导缺陷法是目前最典型、最简单的MOFs缺陷工程方法之一.

然而, 缺陷工程引起的MOFs特性变化会影响MNPs@MOFs的EMSI、电子态和性能, 而且MNPs和MOFs的状态会协同影响MNPs@MOFs的结构和催化活性, 但其构效关系尚不清楚. 因此, 深入探索MOFs缺陷工程和MNPs对MNPs@MOFs结构和催化性能的影响, 对高效负载型催化剂的精准调控至关重要.

本文以甲酸(FA)为调节剂, 通过调控MOFs缺陷工程和MNPs还原条件, 设计并构建了新型UiO-66(Ce)负载Ni NPs异质催化剂, 实现了出色的催化烯烃加氢性能和循环稳定性. 首先, 通过改变MOFs载体合成过程中FA调节剂的添加量, 调节了UiO-66(Ce)载体的缺陷含量、尺寸和结构稳定性等特性, 从而通过C-O-Ni异质界面优化了UiO-66(Ce)载体与Ni NPs之间的EMSI. 其中, 添加40 eq FA的缺陷U(Ce)-40eq载体具有合适的缺陷含量、小尺寸和结构稳定等特点, 不仅优化了Ni NPs的微环境以及U(Ce)-40eq载体和Ni NPs之间的电子转移, 而且小尺寸载体有利于双环戊二烯(DCPD)和H₂底物分子的高效传质和有效吸附, 进而展现了优异的DCPD加氢活性. 此外, 通过调节还原剂种类和添加量、还原溶剂种类等还原条件, 改变了U(Ce)-40eq载体的形貌、尺寸和框架稳定性等结构特性, 协同还原条件调控了Ni NPs的分散度和电子结构. 因此, 通过研究MOFs缺陷工程和Ni NPs还原条件的影响, 协同调节了MOFs载体和Ni NPs之间的EMSI和Ni NPs的化学状态, 从而促进了高度分散、丰富的缺电子态Ni⁰活性位点的生成. 优化后的U(Ce)-40eq负载5 wt% Ni NPs (Ni₅@U(Ce)-40eq-5)展现了优异的DCPD饱和加氢性能, 在70 °C、2 MPa H₂压、90 min后DCPD转化率为100%、四氢双环戊二烯(THDCPD)选择性为100%, 优于大多数高负载Ni基催化剂, 且催化剂在循环6次以后DCPD加氢性能仍为100%、THDCPD选择性为94.8%. 通过催化剂对底物分子吸附强度和加氢过程的研究进一步表明, 丰富的缺电子态Ni⁰物种是加氢过程中DCPD和H₂底物分子吸附和活化的主要活性位点, 缺陷过程和还原条件协同增强了Ni₅@U(Ce)-40eq-5对H₂和C=C键的吸附和活化, 特别是加快了第二步二氢双环戊二烯(DHDCPD)加氢为THDCPD的速率决定步骤, 因此仅负载5 wt% Ni NPs即实现了优异的DCPD饱和加氢性能.

综上, 本文分析了调节剂诱导的MOFs缺陷工程对MNPs@MOFs电子结构、稳定性等结构特性和催化性能的影响, 进一步揭示了缺陷工程和还原条件对MNPs@MOFs的协同调控和性能增强机制, 为精准制备高效MNPs@MOFs催化剂提供了重要的见解, 并为实际应用中金属负载型催化剂的精确设计提供了重要的实验依据和理论指导.

关键词: 金属有机框架, 配体缺失缺陷, Ni⁰物种, 结构稳定性, 加氢

Abstract:

Defect engineering improves the catalytic performance of metal-organic frameworks (MOFs) loaded metal nanoparticles (MNPs@MOFs), but there is still a challenge in defining the structure-activity relationships. Herein, the content of linker-missing defects in UiO-66(Ce) was systematically regulated via formic acid as the modulators, and defective UiO-66(Ce) loaded Ni nanoparticles (NPs) were constructed for dicyclopentadiene (DCPD) hydrogenation. The fine regulation of defect engineering and reduction conditions affected the structure properties of UiO-66(Ce) and the electronic metal-support interaction between MOFs and Ni NPs, thereby optimizing the microenvironment and electronic state of Ni NPs. The optimized U(Ce)-40eq with suitable defects, small size and structure stability effectively promoted the production of highly dispersed abundant electron-deficient Ni⁰ active sites, enhancing the adsorption and activation of H₂ and C=C bonds, especially accelerating the rate-determining step. Therefore, U(Ce)-40eq loaded 5 wt% Ni NPs achieved DCPD saturated hydrogenation to tetrahydrodicyclopentadiene (70 °C, 2 MPa, 90 min), superior to most high-loading Ni-based catalysts. This work reveals the synergistic mechanism of MOFs defect engineering and electronic structure of Ni NPs, providing effective guidance for the precise preparation of highly efficient and stable MNPs@MOFs heterogeneous catalysts.

Key words: Metal-organic frameworks, Linker-missing defects, Ni⁰ species, Structure stability, Hydrogenation

李如硕, 班涛, 赵丹凤, 胡发杰, 林璟, 黄秀兵, 陶志平, 王戈. 缺陷UiO-66(Ce)负载的具有优化微环境和电子态的镍纳米颗粒用于高效烯烃加氢反应[J]. 催化学报, 2025, 72: 344-358.

Rushuo Li, Tao Ban, Danfeng Zhao, Fajie Hu, Jing Lin, Xiubing Huang, Zhiping Tao, Ge Wang. Defective UiO-66(Ce) supported Ni nanoparticles with optimized microenvironment and electronic state for efficient olefin hydrogenation reaction[J]. Chinese Journal of Catalysis, 2025, 72: 344-358.

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Fig. 1. (a) The schematic illustration for the synthesis process of U(Ce)-xeq (x = 0, 10, 20, 30, 40, 50) loaded Ni NPs. SEM and size distribution statistical images of U(Ce)-0eq (b), U(Ce)-10eq (c), U(Ce)-20eq (d), U(Ce)-30eq (e), U(Ce)-40eq (f), and U(Ce)-50eq (g).

Fig. 2. (a) The BDC linker-missing defect number and size distribution tendency chart of U(Ce)-xeq with the increase of FA modulators addition. (b) Schematic illustration for the introduction of BDC linker-missing defects in the U(Ce)-xeq due to introduce different FA modulators. (c) NH3-TPD curves for U(Ce)-40eq and Ni5@U(Ce)-40eq-5. Low-magnification TEM image and size distribution for Ni NPs (d), high-magnification TEM and corresponding interplanar spacing images (e), HAADF-STEM and EDX elemental mapping images (f) of Ni5@U(Ce)-40eq-5.

Fig. 3. (a) DCPD conversion (Con.DCPD) and THDCPD selectivity (Sel.THDCPD) for Ni5@U(Ce)-xeq-5 (x = 0, 10, 20, 30, 40, 50) (90 min, 2 MPa H2, 70 °C). XPS survey (b), Ni 2p XPS spectra (c), and Ce 3d XPS spectra (d) for Ni5@U(Ce)-40eq-5 and Air-Ni5@U(Ce)-40eq-5. Ni 2p XPS spectra (e), and Ce 3d XPS spectra (f) for Ni5@U(Ce)-40eq-5 in different Ar+ etching depths.

Fig. 4. XPS survey (a), Ni 2p XPS spectra (b), and Ce 3d XPS spectra (c) for Ni5@U(Ce)-xeq-5 (x = 0, 10, 20, 30, 40, 50). (d) The ratio of Ce4+/CeTotal, Ni0/NiTotal and Ce3+/CeTotal for Ni5@U(Ce)-xeq-5. (e) Radar image of DCPD hydrogenation performance, defect content, Ni0/NiTotal and Ce4+/CeTotal for Ni5@U(Ce)-xeq-5. (f) XRD patterns of Ni5@U(Ce)-xeq-5.

Fig. 5. Normalized XANES Ce L-edge (a) and Ni K-edge (b) spectra of Ni5@U(Ce)-0eq-5 and Ni5@U(Ce)-40eq-5. (c) Schematic illustration of electron-deficient Ni0 d-orbital and C=C bond orbital electronic configuration. (d) The possible electronic interaction between electron-deficient Ni0 and C=C bond orbital. (e) Schematic diagram of DCPD adsorbed on Ni NPs of Ni5@U(Ce)-40eq-5.

Fig. 6. DCPD conversion (Con.DCPD) and THDCPD selectivity (Sel.THDCPD) (90 min, 2 MPa H2, 70 °C) (a), XRD patterns (b), and FT-IR spectra (c) for Ni5@U(Ce)-40eq-5-H2O, Ni5@U(Ce)-40eq-5-H2O+Hex, Ni5@U(Ce)-40eq-5-EtOH, and Ni5@U(Ce)-40eq-5. (d) SEM image for Ni5@U(Ce)-40eq-5-EtOH. XRD (e) and TEM images (f) for Ni5@U(Ce)-40eq-5-TB. SEM (g) and HAADF-STEM with elemental mapping images (h) for Ni5@CeO2-5.

Fig. 7. DCPD conversion (Con.DCPD) and THDCPD selectivity (Sel.THDCPD) for Niy@U(Ce)-40eq-5 (a) and Ni5@U(Ce)-40eq-z (b) (90 min, 2 MPa H2, 70 °C). XRD pattern (c), XPS survey spectra (d), Ni 2p spectra (e), Ce 3d spectra (f), and the ratio of Ce4+/CeTotal, Ni0/NiTotal and Ce3+/CeTotal (g) for Ni5@U(Ce)-40eq-z. (h) Radar image of DCPD hydrogenation performance, Ni0/NiTotal and Ce4+/CeTotal for Ni5@U(Ce)-40eq-z.

Fig. 8. DCPD hydrogenation performance cycle test (a), XRD pattern (b), Ni 2p XPS spectra (c), and elemental mapping images (d) of AF-Ni5@U(Ce)-40eq-5.

Fig. 9. H2-TPD profiles (a), FT-IR spectra (b,c) of DCPD substrate molecule adsorption on the surface of different samples, respectively. The DCPD hydrogenation performance of Ni5@U(Ce)-40eq-5 under different reaction conditions: different reaction times (30-90 min, 2 MPa H2, 70 °C) (d), different H2 pressures (90 min, 0.5-2 MPa H2, 70 °C) (e), different reaction temperatures (90 min, 2 MPa H2, 40-70 °C) (f). (g) The potential mechanism of DCPD hydrogenation on the surface of Ni5@U(Ce)-40eq-5.

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缺陷UiO-66(Ce)负载的具有优化微环境和电子态的镍纳米颗粒用于高效烯烃加氢反应

Defective UiO-66(Ce) supported Ni nanoparticles with optimized microenvironment and electronic state for efficient olefin hydrogenation reaction

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