“一体化”共价有机框架光催化二氧化碳还原研究

doi:10.1016/S1872-2067(22)64143-3

催化学报 ›› 2022, Vol. 43 ›› Issue (9): 2425-2433.DOI: 10.1016/S1872-2067(22)64143-3

“一体化”共价有机框架光催化二氧化碳还原研究

宋邓萌^a^,^†, 许文华^a^,^†, 李珺^a^,^*(), 赵佳乐^a, 史晴^a, 李斐^b^,^#(), 孙旭镯^c, 王宁^a^,^b^,^$()

^a西北大学化学与材料科学学院, 合成与天然功能分子教育部重点实验室, 陕西西安710069
^b大连理工大学精细化工国家重点实验室, 辽宁大连116024
^c河南工业大学化学化工学院, 河南郑州450001

收稿日期:2022-04-19 接受日期:2022-06-17 出版日期:2022-09-18 发布日期:2022-07-20
通讯作者: 李珺,李斐,王宁
作者简介:第一联系人：
†共同第一作者.
基金资助:
国家自然科学基金(21773184);国家自然科学基金(22172018);国家自然科学基金(21671158);大连理工大学精细化工国家重点实验室开放课题(KF2110);河南省自然科学基金(212300410339)

"All-in-one" covalent organic framework for photocatalytic CO₂ reduction

Dengmeng Song^a^,^†, Wenhua Xu^a^,^†, Jun Li^a^,^*(), Jiale Zhao^a, Qing Shi^a, Fei Li^b^,^#(), Xuzhuo Sun^c, Ning Wang^a^,^b^,^$()

^aKey Laboratory of Synthetic and Natural Functional Molecule of the Ministry of Education, College of Chemistry & Materials Science, Northwest University, Xi’an 710069, Shaanxi, China
^bState Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, Liaoning, China
^cCollege of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, Henan, China

Received:2022-04-19 Accepted:2022-06-17 Online:2022-09-18 Published:2022-07-20
Contact: Jun Li, Fei Li, Ning Wang
About author:First author contact:
†Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21773184);National Natural Science Foundation of China(22172018);National Natural Science Foundation of China(21671158);State Key Laboratory of Fine Chemicals, Dalian University of Technology(KF2110);Natural Science Foundation of Henan Province(212300410339)

摘要/Abstract

摘要：

自工业革命以来, 温室气体CO₂大量排放使得环境问题日益突出, 严重制约了人类的生存和发展. 人工光合作用可利用取之不尽的阳光作为驱动力, 将CO₂还原为可实际应用的化学燃料(CO、HCOOH等). 人工光合作用体系通常包括两部分: 光敏剂和催化剂. 光敏剂吸收入射光的能量, 电子由基态(价带)跃迁至激发态(导带); 处于激发态的光敏剂将电子转移到催化剂上; 最终由催化剂实现CO₂还原. 对光敏剂和催化剂进行合理的调变可以构建更加高效、稳定的人工光合作用体系.

共价有机框架(COFs)材料是由轻元素(C, H, O, N, B等)组成的有机小分子构筑单元通过动态共价键组装, 所形成的具有预先设计的拓扑结构的一维、二维或三维的晶态有机多孔骨架材料. 自从2005年首次报道COFs材料的成功合成以来, COFs逐渐地发展成为了一种具有高潜力和广泛的功能化应用前景的多孔骨架聚合物. 特别是二维共价有机框架(2D-COFs). 2D-COFs独特的平面扩展共轭π-π结构, 使其具有较好的光吸收性能, 轴向的π堆叠结构, 有利于光生电荷的分离和转移, 2D-COFs材料在光催化领域极具应用潜质.

本文以四(4-氨基苯基)卟啉和Re(bpy)(CO)₃Cl为结构单元, 通过希夫碱反应合成了一种集光敏剂和催化剂于一体的2D-COF. 所制H₂PRebpy-COF不仅继承两种单体与COF的性能特点, 并且使三者充分融合、相互促进: (1)卟啉对可见光具有较好的吸收能力, 形成COF后扩展了其π-π共轭结构, 从而增大了光吸收范围; (2)作为最常见的CO₂还原催化剂, 大量内置的Re(bpy)(CO)₃Cl赋予了H₂PRebpy-COF催化CO₂还原的能力; (3)通过较为稳定的共价键和配位键将Re(bpy)(CO)₃Cl修饰在COF结构中, 抑制了其在催化过程中发生的二聚失活. 在可见光照射下, H₂PRebpy-COF光催化CO₂还原的产物为CO和HCOOH, 其中CO的产率达到1200 μmol g^-1 h^-1, 选择性为78%. 同等条件下, 不含Re(bpy)(CO)₃Cl催化中心的参比物H₂Pbpy-COF则几乎没有催化活性. ¹³C同位素标记实验结果表明CO₂还原反应产物中的C来源于反应物CO₂, 而非催化体系中其他物质的分解. 经过三次催化循环后, H₂PRebpy-COF的扫描电镜、红外光谱图与反应前基本一致, 说明结构具有一定的稳定性. 最后, 结合实验和DFT计算对光催化CO₂还原过程提出了一种可能的催化机理: 在可见光的驱动下, 卟啉吸收光的能量, 受激发的电子从卟啉(HOMO中心)转移到Re(bpy)(CO)₃Cl(LUMO中心); Re(bpy)(CO)₃Cl作为催化活性中心实现CO₂还原. 综上, 从微观到宏观, 充分利用各结构的特点, 合成具有特定结构的COFs, 从而具有更优异的性能.

关键词: 共价有机框架, 光催化二氧化碳还原, 卟啉, Re配合物, 可见光

Abstract:

Constructed by selecting appropriate building blocks, covalent organic frameworks (COFs) can be endowed with a variety of specific functions. Herein, we successfully synthesized an imine-linked H₂PReBpy-COF with the CO₂ reduction catalyst [Re^I(bpy)(CO)₃Cl] and the porphyrin photosensitizer as the monomeric building units. The light-harvesting properties of the porphyrin itself, augmented by the extended π-conjugated planar structure of 2D COF, enable H₂PReBpy-COF the excellent light-harvesting capability, efficient charge separation, and fast interfacial charge transfer. In addition, a large amount of uniformly distributed [Re^I(bpy)(CO)₃Cl] units offer H₂PReBpy-COF an excellent activity toward photocatalytic CO₂ reduction with moderate selectivity and reusability. This study demonstrated a proof of concept in which the advantages of COFs and functional monomers are rationally integrated for photocatalytic solar fuel conversion.

Key words: Covalent organic framework, CO₂ photoreduction, Porphyrin, Re complex, Visible-light

宋邓萌, 许文华, 李珺, 赵佳乐, 史晴, 李斐, 孙旭镯, 王宁. “一体化”共价有机框架光催化二氧化碳还原研究[J]. 催化学报, 2022, 43(9): 2425-2433.

Dengmeng Song, Wenhua Xu, Jun Li, Jiale Zhao, Qing Shi, Fei Li, Xuzhuo Sun, Ning Wang. "All-in-one" covalent organic framework for photocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2022, 43(9): 2425-2433.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(22)64143-3

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图/表 7

Fig. 1. (a) Schematic showing the synthesis of H2PReBpy-COF. (b) PXRD patterns of experimental H2PReBpy-COF (blue) and simulated for AA stacking (yellow). (c) The ideal AA eclipsed structures for H2PReBpy-COF from the views of top.

Fig. 2. (a) XPS survey of H2PReBpy-COF and H2PBpy-COF. (b) Re 4f XPS spectrum of H2PReBpy-COF. (c) and (d) BET surface areas (inset illustration: pore size distribution diagram) of H2PReBpy-COF and H2PBpy-COF.

Fig. 3. SEM (a) and HR-TEM (b) images, and the elemental mapping (c) of H2PReBpy-COF.

Fig. 4. UV-vis DRS (a) and the corresponding Tauc plots (b) of H2PReBpy-COF and H2PBpy-COF. (c) LUMO and HOMO positions of H2PReBpy-COF and H2PBpy-COF. (d) Transient photocurrent signals for H2PReBpy-COF and H2PBpy-COF. (e) EIS Nyquist plots of H2PReBpy-COF and H2PBpy-COF. (f) Time-resolved PL decay profiles of H2PReBpy-COF and H2PBpy-COF.

Fig. 5. (a) CO and HCOOH produced during the CO2 photoreduction on H2PReBpy-COF. (b) Catalysis performance under various reaction conditions. (c) The mass spectrum for the gas product and (d) the 13C NMR spectra for the liquid product in the photocatalytic reduction of 13CO2.

Fig. 6. (a) PET route of H2PReBpy-COF under light excitation. (b) The proposed photocatalytic mechanism of H2PReBpy-COF.

Fig. 7. Schematic of the calculated energy profile for the elementary steps during CO2 reduction process by simplified models.

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“一体化”共价有机框架光催化二氧化碳还原研究

"All-in-one" covalent organic framework for photocatalytic CO₂ reduction

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“一体化”共价有机框架光催化二氧化碳还原研究

"All-in-one" covalent organic framework for photocatalytic CO2 reduction

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"All-in-one" covalent organic framework for photocatalytic CO₂ reduction