可定量调控的双助催化剂协同电子-空穴传输体系的构筑及其增强的光催化性能

doi:10.1016/S1872-2067(25)64729-2

催化学报 ›› 2025, Vol. 74: 319-328.DOI: 10.1016/S1872-2067(25)64729-2

可定量调控的双助催化剂协同电子-空穴传输体系的构筑及其增强的光催化性能

高文婧, 刘玉婵, 陈琛瑶, 练梓棋, 叶融凯, 戚朝荣^*(), 胡建强^*()

华南理工大学化学与化工学院, 广东省燃料电池技术重点实验室, 广东省功能分子工程重点实验室, 中国广州 510641

收稿日期:2025-01-17 接受日期:2025-04-07 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: jqhusc@scut.edu.cn (胡建强),crqi@scut.edu.cn (戚朝荣).
基金资助:
国家自然科学基金(22272058);国家自然科学基金(22271098)

Constructing dual-cocatalyst-directed quantifiable electron and hole transfer for enhanced photocatalytic performance

Wenjing Gao, Yuchan Liu, Chenyao Chen, Ziqi Lian, Rongkai Ye, Chaorong Qi^*(), Jianqiang Hu^*()

Key Lab of Fuel Cell Technology of Guangdong Province, Key Laboratory of Functional Molecular Engineering of Guangdong Province, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510641, Guangdong, China

Received:2025-01-17 Accepted:2025-04-07 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: jqhusc@scut.edu.cn (J. Hu), crqi@scut.edu.cn (C. Qi).
Supported by:
National Natural Science Foundation of China(22272058);National Natural Science Foundation of China(22271098)

摘要/Abstract

摘要：

可见光催化技术为高附加值化学品的绿色合成提供了可持续途径, 但传统光催化剂受限于载流子易复合等问题, 难以满足实际应用需求. 亚胺作为重要的化学和生物医药中间体具有广泛的应用前景, 但通过可见光催化合成亚胺的反应效率仍然较低, 限制了其大规模的生产和应用. 半导体纳米材料虽具有可见光响应特性, 但单一材料的催化剂体系难以实现电子-空穴的分离. 目前, 通过使用助催化剂优化半导体纳米材料的研究大多聚焦于促进电子转移, 而忽视了空穴的协同调控. 因此, 开发能同时定向迁移电子和空穴的双助催化剂修饰体系, 以提高半导体基复合纳米材料的光催化性能, 提升光催化合成亚胺的效率具有重要意义.

本文通过使用不同量的还原助催化剂Ti₃C₂T_x和氧化助催化剂2-巯基苯并咪唑(MBI)修饰CdS纳米粒子, 成功构建了一系列CdS/Ti₃C₂T_x/MBI复合纳米材料. CdS/Ti₃C₂T_x/MBI复合纳米材料的Ti₃C₂T_x和MBI能分别从CdS纳米粒子中提取电子和捕获空穴, 最终实现定向的电荷转移, 从而提高电子-空穴的分离效率. CdS纳米粒子, CdS/MBI和CdS/Ti₃C₂T_x/MBI复合纳米材料的透射电子显微镜测试表明, CdS纳米粒子的直径约为7 nm, 修饰MBI分子后, CdS纳米粒子表面有一层无定形的MBI膜, 但该复合纳米材料的整体形貌未发生明显变化. 红外光谱表征结果表明, MBI分子成功键合到CdS纳米粒子表面. CdS/Ti₃C₂T_x/MBI复合纳米材料的电子-空穴分离情况取决于Ti₃C₂T_x和MBI的含量, 且电子和空穴转移的数量最终定量地决定CdS/Ti₃C₂T_x/MBI复合纳米材料的光催化效率. 最优含量的CdS/Ti₃C₂T_x/MBI复合纳米材料的瞬态光电流密度约是CdS纳米粒子的6倍. 光催化模型反应结果表明, 具有最优载流子分离效率的CdS/Ti₃C₂T_x/MBI复合纳米材料对于光催化胺的自偶联反应表现出最佳的催化速率(约8000 μmol·g^-1·h^-1)且其产率可达~96%, 其催化速率约是CdS纳米粒子(约2500 μmol·g^-1·h^-1)的3倍. 对于不同类型胺的自偶联反应, CdS/Ti₃C₂T_x/MBI复合纳米材料都能有良好的催化效果, 这表明其具有底物普适性. 除此之外, CdS/Ti₃C₂T_x/MBI光催化纳米材料还具有良好的稳定性和可重复使用性, 在连续重复使用五次后, 其胺自偶联产物的产率依然可以维持在93%左右, 且CdS/Ti₃C₂T_x/MBI光催化纳米材料的晶体结构几乎不变. 通过淬灭实验和电子顺磁共振测试表明, 该胺自偶联产物的产率很大程度上取决于CdS/Ti₃C₂T_x/MBI复合纳米材料的电子-空穴分离能力, 较强电子-空穴分离能力的CdS/Ti₃C₂T_x/MBI复合纳米材料具有较高的光催化效率.

综上所述, 本文成功构建了具有可量化的定向电荷转移通道的CdS/Ti₃C₂T_x/MBI复合纳米材料. 通过还原助催化剂Ti₃C₂T_x和氧化助催化剂MBI的协同作用, 实现了CdS/Ti₃C₂T_x/MBI复合纳米材料电子和空穴的高效定量分离, 并将该复合纳米材料用于催化胺的自偶联反应, 取得了令人满意的反应速率和产率, 为半导体纳米材料在光催化有机合成中的高效应用提供了新思路.

关键词: 氧化还原双助催化剂, 电子-空穴分离, 光催化剂, 有机转化, MXene

Abstract:

Photocatalysts are essential for the preparation of wanted fine chemical and biomedical intermediates via visible photocatalysis, but existing photocatalysts with low catalytic efficiency limit their wide applications. Herein, CdS/Ti₃C₂T_x/MBI nanocomposites have been successfully fabricated through anchoring reduction cocatalyst Ti₃C₂T_x with electron-drawing ability and oxidation cocatalyst 2-mercaptobenzimidazole (MBI) with hole-capturing capacity on CdS nanoparticles. The Ti₃C₂T_x and MBI of CdS/Ti₃C₂T_x/MBI nanocomposites can extract electrons and holes from CdS nanoparticles to come true electron-hole separation, respectively. Moreover, the electron-drawing and hole-capturing abilities of the CdS/Ti₃C₂T_x/MBI nanocomposites depend on Ti₃C₂T_x and MBI contents, and the quantifiable electron and hole transfers finally determine photocatalytic efficiency of the CdS/Ti₃C₂T_x/MBI nanocomposites. The transient photocurrent density of the CdS/Ti₃C₂T_x/MBI nanocomposites is 6-fold higher than that of the CdS nanoparticles. The CdS/Ti₃C₂T_x/MBI nanocomposites with strong electron-hole separation capability exhibit outstanding visible photocatalytic organic transformation properties. The CdS/Ti₃C₂T_x/MBI nanocomposites produce (E)-N-benzyl-1-phenylmethylimine in ~96% yield (~8000 μmol·g^-1·h^-1), which is 3-fold higher than the CdS nanoparticles (~2500 μmol·g^-1·h^-1, 30%). This work provides a new strategy for constructing efficient and stable photocatalysts that can be used for efficient visible light-driven organic transformations.

Key words: Redox dual cocatalyst, Electron-hole separation, Photocatalyst, Organic transformation, MXene

高文婧, 刘玉婵, 陈琛瑶, 练梓棋, 叶融凯, 戚朝荣, 胡建强. 可定量调控的双助催化剂协同电子-空穴传输体系的构筑及其增强的光催化性能[J]. 催化学报, 2025, 74: 319-328.

Wenjing Gao, Yuchan Liu, Chenyao Chen, Ziqi Lian, Rongkai Ye, Chaorong Qi, Jianqiang Hu. Constructing dual-cocatalyst-directed quantifiable electron and hole transfer for enhanced photocatalytic performance[J]. Chinese Journal of Catalysis, 2025, 74: 319-328.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64729-2

https://www.cjcatal.com/CN/Y2025/V74/I7/319

图/表 8

Fig. 1. Schematic plot of the synthesis of CdS/Ti3C2Tx/MBI nanocomposites fabricated thus.

Fig. 2. XRD patterns (A) and UV-vis absorption spectra (in water) (B) of CdS NPs and CdS/MBI, CdS/Ti3C2Tx and CdS/Ti3C2Tx-3/MBI-6 nanocomposites. (C) FT-IR spectra of MBI, CdS NPs and CdS/MBI, CdS/Ti3C2Tx and CdS/Ti3C2Tx-3/MBI-6 nanocomposites. SEM images of Ti3C2Tx (D), CdS/Ti3C2Tx (E) and CdS/Ti3C2Tx-3/MBI-6 (F) nanocomposites. TEM images of CdS/Ti3C2Tx-3/MBI-6 (G) and CdS/MBI (I) nanocomposites. (H) Element mapping images of CdS/Ti3C2Tx-3/MBI-6 nanocomposites.

Fig. 3. High-resolution XPS spectra of N 1s (A) and C 1s (B) of the CdS/Ti3C2Tx-3/MBI-6 nanocomposites and Cd 3d (C) and S 2p (D) of the CdS NPs and CdS/Ti3C2Tx and CdS/Ti3C2Tx-3/MBI-6 nanocomposites. (E) UV-vis diffuse reflectance spectra (solid) of the CdS NPs and CdS/MBI, CdS/Ti3C2Tx and CdS/Ti3C2Tx-3/MBI-6 nanocomposites. Tauc plots (F) and Mott-Schottky plots (G) of the CdS NPs. (H) Schematic plot of charge transfer of the CdS/Ti3C2Tx/MBI nanocomposites prepared by the present method.

Fig. 4. PL emission spectra (excitation wavelength: 370 nm) (A), electrochemical impedance spectroscopy Nyquist plots (B), TRPL spectra (λ = 375 nm) (C) and transient photocurrent response (D) of the CdS NPs and CdS/MBI, CdS/Ti3C2Tx and CdS/Ti3C2Tx-3/MBI-6 nanocomposites.

Fig. 5. (A) Yields and TOF of oxidative coupling of amines under different photocatalysts. (B) Reusability of the CdS/Ti3C2Tx-3/MBI-6 nanocomposites used for coupling of amines. (C) XRD patterns of the CdS/Ti3C2Tx-3/MBI-6 nanocomposites and corresponding photocatalysts after five cycles.

Table 1 Photocatalytic oxidative coupling of amines under different conditions.a

Entry	Photocatalyst	Yield^b (%)	TOF^c (μmol·g^-1·h^-1)
1	CdS	30	2500
2	CdS/MBI	47	3917
3	CdS/Ti₃C₂T_x	48	4000
4	CdS/Ti₃C₂T_x-1/MBI-4	55	4583
5	CdS/Ti₃C₂T_x-2/MBI-4	64	5333
6	CdS/Ti₃C₂T_x-3/MBI-4	80	6667
7	CdS/Ti₃C₂T_x-4/MBI-4	69	5750
8	CdS/Ti₃C₂T_x-3/MBI-2	56	4667
9	CdS/Ti₃C₂T_x-3/MBI-6	96	8000
10	CdS/Ti₃C₂T_x-3/MBI-8	76	6333

Table 2 Substrate scope of photocatalytic oxidative coupling of amines catalyzed by CdS/Ti3C2Tx/MBI nanocomposites a.

Fig. 6. (A) The catalytic activity of the CdS/Ti3C2Tx/MBI nanocomposites under various reaction conditions. (B) EPR spectra of CdS/Ti3C2Tx/MBI nanocomposites and DMPO. (C) Possible photocatalytic mechanism of CdS/Ti3C2Tx/MBI-mediated oxidative coupling of amines.

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可定量调控的双助催化剂协同电子-空穴传输体系的构筑及其增强的光催化性能

Constructing dual-cocatalyst-directed quantifiable electron and hole transfer for enhanced photocatalytic performance

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