调控COF共价连接的多吡啶镍催化剂微环境促进光催化二氧化碳还原

doi:10.1016/S1872-2067(25)64666-3

催化学报 ›› 2025, Vol. 74: 155-166.DOI: 10.1016/S1872-2067(25)64666-3

调控COF共价连接的多吡啶镍催化剂微环境促进光催化二氧化碳还原

李亚慧, 陈宇, 郭锦瑜, 王锐, 赵淑娜^*(), 李纲^*(), 臧双全^*()

郑州大学化学学院, 河南省晶态分子功能材料重点实验室, 河南郑州 450001

收稿日期:2025-01-08 接受日期:2025-03-11 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: zhaosn@zzu.edu.cn (赵淑娜),gangli@zzu.edu.cn (李纲),zangsqzg@zzu.edu.cn (臧双全).
基金资助:
国家自然科学基金(92461304);国家自然科学基金(92356304);国家自然科学基金(22375185);国家自然科学基金(22105175);河南省中原千人计划(中原学者)(234000510007);河南省自然科学基金(252300421181)

Engineering coordination microenvironments of polypyridine Ni catalysts embedded in covalent organic frameworks for efficient CO₂ photoreduction

Ya-Hui Li, Yu Chen, Jin-Yu Guo, Rui Wang, Shu-Na Zhao^*(), Gang Li^*(), Shuang-Quan Zang^*()

Henan Key Laboratory of Crystalline Molecular Functional Materials, College of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, China

Received:2025-01-08 Accepted:2025-03-11 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: zhaosn@zzu.edu.cn (S.-N. Zhao), gangli@zzu.edu.cn (G. Li), zangsqzg@zzu.edu.cn (S.-Q. Zang).
Supported by:
National Natural Science Foundation of China(92461304);National Natural Science Foundation of China(92356304);National Natural Science Foundation of China(22375185);National Natural Science Foundation of China(22105175);Zhongyuan Thousand Talents (Zhongyuan Scholars) Program of Henan Province(234000510007);Natural Science Foundation of Henan Province(252300421181)

摘要/Abstract

摘要：

在全球气候变化与能源危机双重挑战下, 利用太阳能驱动CO₂转化为高附加值化学品是实现“双碳”目标与能源可持续的重要途径. 多吡啶配合物因其可调的电子结构与优异的电荷转移能力, 已成为光催化CO₂还原领域的研究热点. 然而, 分子催化剂普遍存在回收困难、易失活等问题, 严重制约其实际应用. 近年来, 将分子催化剂负载于多孔载体(如金属有机框架、共价有机框架(COFs)等)构建非均相催化体系, 成为突破该瓶颈的有效策略. COFs凭借高结晶性、可设计孔道的结构以及优异的稳定性, 为精准调控催化活性位点的配位微环境提供了理想平台.

本文通过后合成修饰策略, 将结构明确的多吡啶镍分子催化剂(联吡啶(BPY)、三联吡啶(TPY)和2,6-二(1-吡唑基)吡啶(BPP))共价锚定于羟基功能化COFs骨架上, 系统研究配体类型与配位阴离子(Cl⁻, CH₃COO⁻和NO₃⁻)对光催化性能的影响机制. 结果表明, 与COF-O-BPYNi(NO₃⁻)和COF-O-BPPNi(NO₃⁻)相比, COF-O-TPYNi(NO₃⁻)在光催化CO₂还原中表现出优异的性能, 其CO产率达到9006.0 μmol·g^-1·h^-1, 选择性高达95.9%. 并且COF-O-TPYNi(NO₃⁻)的性能远超于COF-O-TPYNi(Cl⁻)(4588.4 μmol·g^-1·h^-1, 87.3%)和COF-O-TPYNi(CH₃COO⁻)(3591.8 μmol·g^-1·h^-1, 94.1%). 机理研究表明, COF-OH骨架作为电子传输通道显著提升电荷分离效率. 瞬态吸收光谱(TA)显示, COF-O-TPYNi(NO₃⁻)的光生电子寿命(τ₂ = 122.6 ps)远超物理混合体系(τ₂ = 65.3 ps), 证实共价连接有效抑制电子-空穴复合. 原位X-射线吸收精细结构谱揭示, 光激发下Ni位点发生动态电子转移: CO₂吸附诱导Ni价态升高(+ 0.123 eV), 而光照后Ni价态降低(-0.156 eV), 表明Ni作为活性中心参与CO₂活化. 密度泛函理论计算表明, TPY配体通过π共轭体系降低*COOH形成能垒(0.54 eV), 而NO₃⁻配位进一步优化Ni位点电子结构, 使速率控制步骤能垒低于BPYNi与BPPNi体系. 实验和理论研究表明, 配体和配位阴离子对活性中心的电子结构具有显著影响, 通过增强电荷分离和传输能力, 降低反应中间体*COOH的反应能垒, 从而有效提升光催化CO₂还原的性能.

综上, 本研究通过配位微环境精准调控策略, 成功构建高效、稳定的COF基光催化体系, 为设计新型异相分子催化剂提供了重要参考, 并结合原位表征技术动态解析催化界面反应过程, 推动光催化CO₂还原研究.

关键词: 配位环境, 阴离子调控, 共价有机框架, 多吡啶镍催化剂, 光催化CO₂还原

Abstract:

The coordination engineering of catalytic centers emerges as a pivotal strategy for precise electronic configuration modulation in photocatalytic CO₂ reduction. Herein, the electronic structure of active sites in polypyridine nickel catalysts is well modified through strategic ligand variation (bipyridine, terpyridine (TPY), 2,6-di(1-pyrazolyl)pyridine) and anion coordination (NO₃^-, Cl^-, and CH₃COO^-), achieving enhanced CO₂ performance. Crucially, covalent immobilization of these molecular catalysts within the COF-OH framework not only preserves their precisely defined and structurally adaptable characteristics but also demonstrates synergistic enhancement of CO₂ adsorption capacity and charge transfer kinetics, as verified by CO₂ adsorption isothermal analysis and ultrafast time-resolved transient absorption spectroscopy. Remarkably, COF-O-TPYNi(NO₃^-) catalyst exhibits a CO₂-to-CO reduction activity of 9006.0 μmol·g^-1·h^-1 with 95.9% selectivity, superior to its counterpart catalysts, directly validating the mechanistic significance of precisely tailored coordination microenvironments around Ni active sites. Mechanistic studies through in situ XAFS, in situ ATR-SEIRAS and theoretical calculations reveal that this performance improvement over COF-O-TPYNi(NO₃^-) is attributed to the reduced reaction energy barrier of *COOH generation. This work pioneers a coordination shell engineering paradigm for rational design of molecularly defined catalytic architectures.

Key words: Coordination number, Anion regulation, Covalent organic framework, Polypyridine nickel catalyst, Photocatalytic CO₂ reduction

李亚慧, 陈宇, 郭锦瑜, 王锐, 赵淑娜, 李纲, 臧双全. 调控COF共价连接的多吡啶镍催化剂微环境促进光催化二氧化碳还原[J]. 催化学报, 2025, 74: 155-166.

Ya-Hui Li, Yu Chen, Jin-Yu Guo, Rui Wang, Shu-Na Zhao, Gang Li, Shuang-Quan Zang. Engineering coordination microenvironments of polypyridine Ni catalysts embedded in covalent organic frameworks for efficient CO₂ photoreduction[J]. Chinese Journal of Catalysis, 2025, 74: 155-166.

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图/表 6

Scheme 1. Design of high-efficiency photocatalysts. (a) Polypyridine nickel catalysts and photocatalytic process. (b) Integrating polypyridine nickel catalysts with COF-OH through a covalently linking strategy for enhanced photocatalytic CO2 reduction.

Fig. 1. (a) Synthetic scheme of COF-O-Ni samples. PXRD patterns (b), FT-IR spectra (c), N2 absorption-desorption isotherms at -196 °C (d) of COF-OH and COF-O-Ni samples.

Fig. 2. HR-TEM image (a), the AC-HAADF-STEM image (b), and the EDX elemental mapping (c) of COF-O-TPYNi(NO3-). (d) Normalized XANES spectra at the Ni K-edge of COF-O-Ni samples with Ni foil, NiO, and Cl-TPYNi as the reference. (e) FT-EXAFS spectra at the Ni K-edge of Cl-TPYNi and COF-O-Ni samples with Ni foil, NiO, and NiPc as the reference. (f-i) EXAFS fitting and structure of Cl-TPYNi and COF-O-Ni samples at R space.

Fig. 3. (a) CO and H2 evolution at 2 h catalyzed by COF-O-Ni samples. (b) Summary of Ni-based photocatalytic systems for reduction of CO2 to CO. (c) Control experiments of catalytic conditions. (d) Cycle test of COF-O-TPYNi(NO3-). (e) Transient photoresponsive current density analyst for TPYNi, COF-OH, and COF-O-Ni samples. (f) Nyquist plots of TPYNi, COF-OH, and COF-O-Ni based on EIS measurements.

Fig. 4. (a) In-situ XANES spectra at Ni K-edge of COF-O-TPYNi(NO3-) collected under Ar atmosphere, CO2 atmosphere, and CO2 atmosphere with light illumination. (b) CO2 sorption isotherms at -0.15 °C for COF-OH and COF-O-Ni samples. (c) The isosteric heats of adsorption (Qst) for COF-O-Ni samples. Pseudocolor plots (d,g) and ultrafast time-resolved TA spectra (e,h) of COF-O-TPYNi(NO3-) and the physical mixture of COF-OH and TPYNi. All the samples are tested under 330 nm. (f,i) TA decay curves at 400 and 520 nm of COF-O-TPYNi(NO3-) and the physical mixture of COF-OH and TPYNi.

Fig. 5. (a) ATR-SEIRAS of COF-O-TPYNi(NO3-). (b,c)PDOS of COF-OH and COF-O-TPYNi(NO3-). (d) TDOS of COF-OH and COF-O-TPYNi(NO3-). (e,f) The Gibbs free energy diagram of the CO2RR to CO photocatalytic reaction. (g) Proposed CO2 to CO photocatalytic pathway in the model of COF-O-TPYNi(NO3-).

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调控COF共价连接的多吡啶镍催化剂微环境促进光催化二氧化碳还原

Engineering coordination microenvironments of polypyridine Ni catalysts embedded in covalent organic frameworks for efficient CO₂ photoreduction

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调控COF共价连接的多吡啶镍催化剂微环境促进光催化二氧化碳还原

Engineering coordination microenvironments of polypyridine Ni catalysts embedded in covalent organic frameworks for efficient CO2 photoreduction

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Engineering coordination microenvironments of polypyridine Ni catalysts embedded in covalent organic frameworks for efficient CO₂ photoreduction