异金属取代的多金属氧酸盐@光响应型金属-有机框架用于高选择性光催化CO2还原

doi:10.1016/S1872-2067(23)64453-5

催化学报 ›› 2023, Vol. 50: 343-351.DOI: 10.1016/S1872-2067(23)64453-5

异金属取代的多金属氧酸盐@光响应型金属-有机框架用于高选择性光催化CO₂还原

李慧杰, 池漫洲, 辛兴, 王瑞杰, 刘天府, 吕红金^*(), 杨国昱

北京理工大学化学与化工学院, 光电/电光转换材料北京重点实验室, 原子分子簇科学教育部重点实验室, 北京 102488

收稿日期:2023-04-06 接受日期:2023-05-12 出版日期:2023-07-18 发布日期:2023-07-25
通讯作者: *电子信箱: hlv@bit.edu.cn (吕红金).
基金资助:
国家自然科学基金(21871025);国家自然科学基金(21831001);国家海外高层次人才引进计划青年项目;北理工高层次人才科研启动计划项目

Highly selective photoreduction of CO₂ catalyzed by the encapsulated heterometallic-substituted polyoxometalate into a photo-responsive metal-organic framework

Huijie Li, Manzhou Chi, Xing Xin, Ruijie Wang, Tianfu Liu, Hongjin Lv^*(), Guo-Yu Yang

MOE Key Laboratory of Cluster Science, Beijing Key Laboratory of Photoelectroic/Electrophotonic Conversion Materials, School of Chemistry and Chemical Engineering, Beijing Institute of Technology, Beijing 102488, China

Received:2023-04-06 Accepted:2023-05-12 Online:2023-07-18 Published:2023-07-25
Contact: *E-mail: hlv@bit.edu.cn (H. Lv).
Supported by:
National Natural Science Foundation of China(21871025);National Natural Science Foundation of China(21831001);Recruitment Program of Global Experts (Young Talents);BIT Excellent Young Scholars Research Fund

摘要/Abstract

摘要：

传统化石燃料的过度消耗以及CO₂的持续排放, 使开发可再生的碳中性燃料迫在眉睫. 利用太阳能将CO₂光还原为能量密集的有机分子(CO, HCOOH, HCHO和CH₃OH等)被认为是一种绿色可持续但极具挑战性的方案. 实现该方案所面临的关键难点是开发高效、廉价的光催化CO₂还原催化剂. 作为一种具有前景的多电子转移催化剂, 过渡金属取代的多金属氧酸盐(POM)因其结构丰富且物化性质可调, 越来越多地被应用于光催化CO₂还原研究. 其结构中的缺位多酸配体可用作电子存储海绵以实现光催化CO₂还原反应中的多电子转移过程. 然而, 目前均相催化体系面临的主要挑战在于可溶性POMs催化剂的可回收性不高和催化活性低等. 为解决上述挑战, 可行的策略是将可溶性POMs催化剂装载到多孔金属有机框架(MOFs)中, 制备POM@MOF复合材料, 从而将可溶性POMs催化剂优越的催化活性与多孔材料的可回收性结合起来. 作为一类光敏型MOF材料, NU-1000具有良好的光响应能力和合适的孔道结构, 可容纳不同尺寸的POMs客体分子. 目前, 基于POM@NU-1000的复合材料在光驱动分解水制氢领域已有一些报道; 然而, 该类复合材料在太阳能驱动的光催化CO₂还原中的应用研究仍然较少.

本文构筑了一种异金属取代的POM@NU-1000复合材料(P₂W₁₅Ni₃{Re(CO)₃}₃@NU-1000)通过浸渍法将Ni-Re异金属取代POMs (Na(NH₄)₅[P₂W₁₅O₅₆Ni₃(H₂O)₃(μ₃-OH)₃{Re(CO)₃}₃]·18H₂O)锚定到NU-1000 MOF孔道中. 系列实验实验证实了P₂W₁₅Ni₃{Re(CO)₃}₃客体团簇成功装载进NU-1000主体的孔道中. 在最佳条件下, P₂W₁₅Ni₃{Re(CO)₃}₃@NU-1000复合材料能有效地进行光催化CO₂还原, 反应10 h的CO产量高达28982 μmol g^-1, 选择性达93.5%. 此外, 该催化体系具有良好的光催化稳定性和至少4次连续循环的可重复性. 催化反应机理研究表明, 高效的光催化CO₂还原性能归因于P₂W₁₅Ni₃{Re(CO)₃}₃团簇独特的结构完整性、NU-1000优良的光响应能力以及二者之间强的主-客体相互作用. 综上, 本工作展示了引入CO₂还原功能单元到POMs客体分子的策略可调节POM@MOF功能复合材料的催化活性, 为设计和合成高效率CO₂还原光催化剂提供了实验参考.

关键词: CO₂还原, 多金属氧酸盐, 金属有机框架材料, 异金属取代, 光催化

Abstract:

The highly selective photoreduction of CO₂ into valuable chemical fuels such as CO has been considered as an effective strategy to address modern energy and environmental issues. In this work, we have adopted the well-established impregnation approach to construct a P₂W₁₅Ni₃{Re(CO)₃}₃@NU-1000 composite by incorporating heterometallic-substituted P₂W₁₅Ni₃{Re(CO)₃}₃ polyoxometalate (POM) into the pores of metal-organic framework (NU-1000) host. Upon light irradiation, the resulting P₂W₁₅Ni₃{Re(CO)₃}₃@NU-1000 composite can effectively photocatalyze CO₂ reduction, obtaining a CO production of 28982 μmol g^-1 with 93.5% selectivity during 10-h photocatalysis. The catalytic system exhibits great long-term recyclability and stability for at least four successive recycles. The proposed photocatalytic mechanism was confirmed by a series of photochemical and spectroscopic analyses.

Key words: CO₂ reduction, Polyoxometalate, Metal-organic framework, Heterometallic substitution, Photocatalysis

李慧杰, 池漫洲, 辛兴, 王瑞杰, 刘天府, 吕红金, 杨国昱. 异金属取代的多金属氧酸盐@光响应型金属-有机框架用于高选择性光催化CO₂还原[J]. 催化学报, 2023, 50: 343-351.

Huijie Li, Manzhou Chi, Xing Xin, Ruijie Wang, Tianfu Liu, Hongjin Lv, Guo-Yu Yang. Highly selective photoreduction of CO₂ catalyzed by the encapsulated heterometallic-substituted polyoxometalate into a photo-responsive metal-organic framework[J]. Chinese Journal of Catalysis, 2023, 50: 343-351.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64453-5

https://www.cjcatal.com/CN/Y2023/V50/I7/343

图/表 7

Scheme 1. Schematic illustration of the synthetic procedure of the P2W15Ni3{Re(CO)3}3@NU-1000 composite.

Fig. 1. SEM images of NU-1000 (a) and 1.13-P2W15Ni3 {Re(CO)3}3@NU-1000 composite (b). TEM images of NU-1000 (c) and 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 composite (d). (e) selective SEM image and the corresponding elemental mapping images of 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 composite.

Fig. 2. (a) The pore size distribution curves of P2W15Ni3{Re(CO)3}3, NU-1000, and P2W15Ni3{Re(CO)3}3@NU-1000; UV-vis diffuse reflectance spectra (b), FT-IR spectra (c), and PXRD patterns (d) of P2W15Ni3{Re(CO)3}3, NU-1000, and 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 composite.

Fig. 3. (a) The yield of gas products in the photocatalytic CO2 reduction with different molar ratios of P2W15Ni3{Re(CO)3}3@NU-1000 in 10 h. (b) Control experiments of CO2 reduction by varying experimental conditions (Note: the moles of comparative catalysts including P2W15Ni3{Re(CO)3}3, NU-1000, Re(CO)5Cl, NiCl2, and others were kept the same as that in 1 mg 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 photocatalyst). (c) Recycling tests of the 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 photocatalyst. (d) Long-term photocatalytic CO2 reduction using 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 composite.

Fig. 4. PL spectra (a) and normalized time-resolved PL decay kinetics (b) of NU-1000 and 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 solid samples upon excitation at 365 nm.

Fig. 5. (a) High-resolution XPS spectra of Zr 3d in NU-1000 and 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 before and after photocatalysis; high-resolution XPS spectra of Ni 2p (b), W 4f (c), and Re 4f (d) in 1.13-P2W15Ni3{Re(CO)3}3@NU-1000 before and after photocatalysis.

Fig. 6. Schematic diagram of the proposed photocatalytic CO2 reduction mechanism using P2W15Ni3{Re(CO)3}3@NU-1000 photocatalyst.

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异金属取代的多金属氧酸盐@光响应型金属-有机框架用于高选择性光催化CO₂还原

Highly selective photoreduction of CO₂ catalyzed by the encapsulated heterometallic-substituted polyoxometalate into a photo-responsive metal-organic framework

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