苯并三噻吩基共价有机框架连接结构调控实现高效光合成H2O2

doi:10.1016/S1872-2067(25)64925-4

催化学报 ›› 2026, Vol. 83: 271-281.DOI: 10.1016/S1872-2067(25)64925-4

苯并三噻吩基共价有机框架连接结构调控实现高效光合成H₂O₂

谢可慧^a^,¹, 刘从学^b^,¹, 耿琰^a^,^*(), 阚京兰^a, 王广博^a^,^*(), 董育斌^a

^a山东师范大学化学化工与材料科学学院, 山东省高校化学成像功能探针协同创新中心, 分子与纳米探针教育部重点实验室, 山东济南 250014
^b北京大学深圳研究生院, 新材料学院, 广东深圳 518055

收稿日期:2025-08-08 接受日期:2025-10-19 出版日期:2026-04-18 发布日期:2026-03-04
通讯作者: * 电子信箱: guangbo.wang@sdnu.edu.cn (王广博), gengyan@sdnu.edu.cn (耿琰).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22371172);国家自然科学基金(22171169);山东省泰山学者攀登计划;山东省自然科学基金(ZR2024MB119);山东省自然科学基金(ZR2024MB161);山东省高等学校青创团队计划(2023KJ194)

Efficient H₂O₂ photosynthesis through linker engineering of benzotrithiophene-based covalent organic frameworks

Ke-Hui Xie^a^,¹, Cong-Xue Liu^b^,¹, Yan Geng^a^,^*(), Jing-Lan Kan^a, Guang-Bo Wang^a^,^*(), Yu-Bin Dong^a

^aCollege of Chemistry, Chemical Engineering and Materials Science, Collaborative Innovation Center of Functionalized Probes for Chemical Imaging in Universities of Shandong, Key Laboratory of Molecular and Nano Probes, Ministry of Education, Shandong Normal University, Jinan 250014, Shandong, China
^bSchool of Advanced Materials, Peking University, Shenzhen Graduate School, Shenzhen 518055, Guangdong, China

Received:2025-08-08 Accepted:2025-10-19 Online:2026-04-18 Published:2026-03-04
Contact: * E-mail: guangbo.wang@sdnu.edu.cn (G.-B. Wang), gengyan@sdnu.edu.cn (Y. Geng).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22371172);National Natural Science Foundation of China(22171169);Taishan Scholars Climbing Program of Shandong Province;Natural Science Foundation of Shandong Province(ZR2024MB119);Natural Science Foundation of Shandong Province(ZR2024MB161);Youth Innovation Science and Technology Program of Higher Education Institution of Shandong Province(2023KJ194)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种重要的基础化学品, 在消毒杀菌、工业漂白、生物医药和有机合成等领域具有广泛应用, 被列为全球100种最重要化学品之一. 目前工业上主要采用蒽醌法生产H₂O₂, 但该方法存在能耗高、工艺复杂和环境污染等问题. 因此, 在绿色温和条件下开发高效合成H₂O₂的新方法已成为催化领域的重要研究方向. 共价有机框架(COFs)是一类新兴晶态多孔材料, 因其结构可调、激子迁移率高以及能带可控等优势, 在光催化领域显现出巨大潜力. 在水相光催化体系中, 光生载流子的分离效率与材料的亲疏水性是影响光催化性能的两个关键因素, 如何实现二者的协同调控是当前面临的主要挑战. 本文提出通过在COFs构筑单元中引入不同亲疏水性官能团, 以同时实现材料电荷分离效率与亲疏水特性的精准调控, 从而实现高效光催化合成H₂O₂.
本研究通过引入羟基(-OH)、未修饰氢原子(-H)及氟原子(-F)三种不同性质的官能团, 设计合成了一系列具有相同网络拓扑结构的苯并三噻吩基COFs材料(分别为BTT-BD-OH-COF, BTT-BD-COF, BTT-BD-F-COF). 粉末X射线衍射和Materials Studio结构模拟表明, 所得COFs均为P6/M空间群的AA堆积结构. 傅里叶变换红外光谱、固体¹³C核磁共振以及X射线光电子能谱结果共同证实了亚胺键的成功构建; 水接触角测试结果表明, -OH官能团的引入可以显著提升材料的亲水性(接触角≈16.5°), 而-F官能团则显著增强材料疏水性(接触角≈134.1°). 光电化学测试结果表明, BTT-BD-OH-COF具有更窄的光学带隙, 更宽的可见光吸收范围和更高的光生载流子分离效率. 光催化合成H₂O₂的性能测试中, BTT-BD-OH-COF表现出卓越的催化活性, 其在纯水中的H₂O₂生成速率高达6105 μmol g^-1 h^-1, 显著优于其它两种材料, 且表现出良好的循环稳定性与结构稳定性. 为深入探究其反应机制, 通过同位素标记实验和密度泛函理论(DFT)计算, 系统分析了H₂O₂的生成路径, 结果表明, H₂O₂的合成主要通过氧气还原反应(ORR)和水氧化反应(WOR)两条路径协同进行. 在ORR路径中, 三种COFs均遵循两步1e^-过程, 光生电子与O₂还原为^•O₂^-, 进而转化为H₂O₂; 在WOR路径中, BTT-BD-OH-COF和BTT-BD-COF遵循2e^-路径直接将H₂O氧化为H₂O₂, 而BTT-BD-F-COF则倾向于通过4e^-路径生成O₂, 再经过ORR过程转化为H₂O₂. DFT计算表明, BTT-BD-OH-COF在ORR路径的关键步骤(*OOH中间体生成)和WOR路径的关键步骤(*OH中间体生成)中具有最低的吉布斯自由能, 这从热力学角度解释了其优异光催化活性的内在机制.
综上, 本文通过配体功能化策略同时实现了COFs材料亲疏水特性和光生载流子的协同调控,在纯水中实现了H₂O₂的高效光合成, 并阐明了反应机制, 为后续设计开发高效光合成H₂O₂催化体系提供了新的思路和理论依据.

关键词: 共价有机框架材料, 光催化, 过氧化氢, 连接结构调控, 苯并三噻吩

Abstract:

The photogenerated carrier separation efficiency and material wettability are of critical importance for aqueous-phase photocatalytic reactions, achieving both simultaneously poses a significant challenge owing to the inherent interdependencies and trade-offs involved. In this work, a series of isoreticular benzotrithiophene-based covalent organic frameworks (COFs) were successfully synthesized by incorporating diverse hydrophobic and hydrophilic functional groups (-OH, -F, -H) onto their skeletons, thereby modulating their characteristic charge separation and transport as well as their wettability, and systematically studied their photocatalytic H₂O₂ production performance in O₂-saturated water under visible-light irradiation. Remarkably, the synthesized hydrophilic BTT-BD-OH-COF demonstrates the highest H₂O₂ production rate of 6105 μmol g^-1 h^-1 in the absence of any sacrificial agent in pure water, attributed to its extended light absorption range, improved hydrophilicity, and enhanced photo-induced charge separation and transport efficiency. Combined experimental results and the density functional theory calculations elucidate the reaction mechanism, revealing the overall H₂O₂ photosynthesis via both oxygen reduction reaction and water oxidation reaction dual pathways. This study demonstrates that functional-group-mediated linker engineering is a powerful approach for significantly enhancing the efficiency of COF-based photocatalysts.

Key words: Covalent organic frameworks, Photocatalysis, Hydrogen peroxide, Linker engineering, Benzotrithiophene

谢可慧, 刘从学, 耿琰, 阚京兰, 王广博, 董育斌. 苯并三噻吩基共价有机框架连接结构调控实现高效光合成H₂O₂[J]. 催化学报, 2026, 83: 271-281.

Ke-Hui Xie, Cong-Xue Liu, Yan Geng, Jing-Lan Kan, Guang-Bo Wang, Yu-Bin Dong. Efficient H₂O₂ photosynthesis through linker engineering of benzotrithiophene-based covalent organic frameworks[J]. Chinese Journal of Catalysis, 2026, 83: 271-281.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64925-4

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图/表 5

Fig. 1. Schematic synthesis of the COFs (a). The experimental as well as simulated PXRD patterns of BTT-BD-OH-COF (b), BTT-BD-COF (c), and BTT-BD-F-COF (d) with the AA eclipsed stacking mode.

Fig. 2. The solid state 13C CP/MAS NMR spectrum of BTT-BD-OH-COF (a). High resolution N 1s (b), S 2p (c), O 1s (d) XPS spectra of BTT-BD-OH-COF. The N2 adsorption-desorption isotherm of BTT-BD-OH-COF was measured at 77 K, a standard temperature for such analyses, to characterize its porosity. (e) The inset figure illustrates the pore size distribution of BTT-BD-OH-COF, derived from NLDFT. (f) Water contact angle measurements of BTT-BD-X-COFs.

Fig. 3. (a) The UV-vis DRS of the COFs. (b) The Tauc plots of the COFs for band gap calculation. (c) The M-S plot of BTT-BD-OH-COF. (d) The energy band alignment of the COFs, as determined experimentally. (e) Comparative analysis of the photocurrent responses in the COFs. (f) The EIS Nyquist plots of the COFs. (g) The PL spectra of the COFs. (h) The TRPL spectra of the COFs. (i) The distributions of the photo-excited electrons and holes of BTT-BD-OH-COF (blue and green represent electrons and holes, respectively).

Fig. 4. (a) Time-dependent H2O2 production curves of all the COFs under visible-light irradiation over 2 h. (b) The AQYs of BTT-BD-OH-COF at different wavelengths (450, 475, 520, 550, 600, 650 nm). (c) The Kf and Kd rate constants of H2O2 for all the COFs. (d) Recyclability of BTT-BD-OH-COF for photocatalytic hydrogen peroxide production. (e) The comparison of hydrogen peroxide generation rates of COFs under different atmosphere conditions. (f) The control experiments showing the H2O2 production performance of COFs under O2 atmosphere conditions. ρ-BQ: 1,4-benzoquinone.

Fig. 5. (a) The EPR spectra of BTT-BD-OH-COF in dark and light with DMPO as the spin-trap agent. (b) The time-dependent photocatalytic O2 evolution profiles of BTT-BD-F-COF over 4 h. (c,d) The isotopic experiments with BTT-BD-F-COF as the photocatalyst in H218O. (e) RRDE voltammograms of BTT-BD-OH-COF with a potential of -0.23 V vs. Ag/AgCl on Pt ring electrode to detect O2. (f) RRDE voltammograms of BTT-BD-OH-COF with a potential of +0.60 V vs. Ag/AgCl on Pt ring electrode to detect H2O2. (g) The corresponding ESP map of BTT-BD-OH-COF model. (h) The ΔG diagram for ORR pathway into H2O2 over the COFs. (i) The ΔG diagram for the WOR pathway into H2O2 over BTT-BD-OH-COF and BTT-BD-COF.

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苯并三噻吩基共价有机框架连接结构调控实现高效光合成H₂O₂

Efficient H₂O₂ photosynthesis through linker engineering of benzotrithiophene-based covalent organic frameworks

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