构建卟啉基共价有机框架与Nb2C MXene的S型异质结并应用于光催化过氧化氢生产

doi:10.1016/S1872-2067(24)60247-0

催化学报 ›› 2025, Vol. 70: 431-443.DOI: 10.1016/S1872-2067(24)60247-0

构建卟啉基共价有机框架与Nb₂C MXene的S型异质结并应用于光催化过氧化氢生产

许明阳^a^,¹, 李真真^b^,¹, 沈荣晨^a^,¹, 张欣^c^,^*(), 张治红^b^,^*(), 张鹏^d^,^*(), 李鑫^a^,^*()

^a华南农业大学材料与能源学院, 生物质工程研究院, 生物基材料与能源教育部重点实验室, 广东广州 510642
^b郑州轻工业大学材料与化学工程学院, 河南郑州 450001
^c湖北文理学院低维光电材料与器件湖北省重点实验室, 湖北襄阳 441053
^d郑州大学材料科学与工程学院, 设计低碳环保材料国际合作国家中心, 河南郑州 450001

收稿日期:2024-11-24 接受日期:2025-02-22 出版日期:2025-03-18 发布日期:2025-03-20
通讯作者: * 电子信箱: Xinli@scau.edu.cn (李鑫),2006025@zzuli.edu.cn (张治红),xinzhang@hbuas.edu.cn (张欣),zhangp@zzu.edu.cn (张鹏).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22378148);国家自然科学基金(52472110);国家自然科学基金(2230082074);广东省自然科学基金(2024A1515012433)

Constructing S-scheme heterojunction between porphyrinyl covalent organic frameworks and Nb₂C MXene for photocatalytic H₂O₂ production

Mingyang Xu^a^,¹, Zhenzhen Li^b^,¹, Rongchen Shen^a^,¹, Xin Zhang^c^,^*(), Zhihong Zhang^b^,^*(), Peng Zhang^d^,^*(), Xin Li^a^,^*()

^aInstitute of Biomass Engineering, Key Laboratory for Biobased Materials and Energy of Ministry of Education, College of Materials and Energy, South China Agricultural University, Guangzhou 510642, Guangdong, China
^bCollege of Material and Chemical Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, Henan, China
^cHubei Key Lab Low Dimens Optoelect Mat & Devices, Hubei University of Arts and Science, Xiangyang 441053, Hubei, China
^dState Centre for International Cooperation on Designer Low-Carbon & Environmental Materials (CDLCEM), School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, Henan, China

Received:2024-11-24 Accepted:2025-02-22 Online:2025-03-18 Published:2025-03-20
Contact: * E-mail: Xinli@scau.edu.cn (X. Li),2006025@zzuli.edu.cn, (Z. Zhang),xinzhang@hbuas.edu.cn (X. Zhang),zhangp@zzu.edu.cn (P. Zhang).
About author:¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22378148);National Natural Science Foundation of China(52472110);National Natural Science Foundation of China(2230082074);Natural Science Foundation of Guangdong Province(2024A1515012433)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种重要的工业化学氧化剂, 广泛应用于水处理、化学合成、医疗领域、纺织漂白、消毒以及燃料电池等领域. 然而, 目前工业上主要采用的蒽醌氧化法合成H₂O₂, 尽管工艺成熟, 但仍存在能耗高、副产物多、后续纯化复杂等问题. 基于此, 在纯水中通过光催化的两电子氧还原反应(2e^‒ ORR)制备H₂O₂被视为一种绿色、节能且安全的策略. 然而, 该体系的实际应用受到太阳能光动力学缓慢、选择性不足及光能利用效率低等限制. 因此, 我们前期设计了一种新型二维(2D)卟啉基共价有机框架(Tph-Dha-COF)与Nb₂C MXene纳米片组装的S型异质结光催化剂. 该催化剂通过2e^‒ ORR实现了高效光催化合成H₂O₂, 并同时利用原位生成的H₂O₂实现了细菌的高效灭活. 尽管异质结的构建已被证明是提升COF材料光催化性能的有效策略, 但基于Nb₂C的COF光催化剂在H₂O₂光催化合成中的研究仍较为少见.

本文首先通过氨基化处理Nb₂C MXene制备了Nb₂C-NH₂, 随后采用溶剂热法以Tph和Dha为前驱体, 在Nb₂C-NH₂表面原位合成了S型异质结光催化剂(Tph-Dha-COF@Nb₂C). 通过X射线衍射、傅里叶变换红外光谱、高分辨透射电子显微镜及紫外光电子能谱等表征手段, 证实了Tph-Dha-COF@Nb₂C异质结的成功构筑. 同时, 结果表明该异质结在紫外-可见光谱范围内具有良好的光吸收性能, 显著增强了光生电子-空穴对的分离与迁移效率, 并且具备较大的比表面积. 通过紫外-可见分光光度法评估了Nb₂C-NH₂, Tph-Dha-COF及Tph-Dha-COF@Nb₂C的光催化活性. 在可见光照射下, Tph-Dha-COF@Nb₂C的H₂O₂产率达1833 μmol g^‒1 h^‒1, 显著高于Tph-Dha-COF和Nb₂C-NH₂. 此外, 在无牺牲剂条件下, 太阳能转化效率达到0.345%, 明显高于Tph-Dha-COF (0.226%)和Nb₂C-NH₂ (0.051%). 进一步结合原位FT-IR谱与密度泛函理论计算, 揭示了光催化反应路径及关键中间体的种类, 证实了Nb₂C-NH₂的引入促进了O₂在异质结表面的侧位吸附, 从而有利于超氧自由基(•O₂^‒)的生成, 并有效降低了光催化反应的能量势垒. 特别是, 光催化生成的H₂O₂对细菌灭活率超过90%, 进一步验证了其在抗菌领域的潜在应用价值.

综上所述, 本研究通过Nb₂C-NH₂与卟啉基COF材料的协同作用, 成功构建了S型异质结光催化剂, 显著提高了COF的电荷分离与迁移效率, 并拓宽了其光吸收范围, 从而实现了H₂O₂光催化合成的高效性与选择性. 该异质结的构筑为光催化H₂O₂的绿色制备提供了一种新颖而有效的策略, 同时也为其在环境和能源领域的实际应用奠定了基础.

关键词: 光催化, 过氧化氢, 共价有机框架, Nb₂C MXene, S型异质结

Abstract:

We have developed a novel S-scheme heterojunction photocatalyst for the photocatalytic production of hydrogen peroxide (H₂O₂) via a two-electron (2e⁻) oxygen reduction reaction. This S-scheme heterojunction Tph-Dha-COF@Nb₂C was fabricated via the in-situ solvothermal growth of Tph-Dha-COF nanostructures on amino-functionalized Nb₂C MXene nanoflakes (Nb₂C-NH₂). The integration of Nb₂C significantly extended the visible light absorption of Tph-Dha-COF into the near-infrared region for photocatalytic H₂O₂ production. The Tph-Dha-COF@Nb₂C composite demonstrated efficient charge separation, rapid electron transfer, and enhanced oxygen adsorption. Consequently, the Tph-Dha-COF@Nb₂C heterojunction exhibited a high H₂O₂ production rate of 1833 μmol g^‒1 h^‒1 without sacrificial agents. In-situ Fourier transformed infrared spectroscopy and density functional theory calculations revealed the photocatalytic H₂O₂ production mechanism. The generated H₂O₂ demonstrated enhanced antibacterial activity. This work presents the first application of Nb₂C in the photocatalytic synthesis of H₂O₂ and provides a novel strategy for constructing COF-based heterojunctions for photocatalytic H₂O₂ generation and wastewater treatment.

Key words: Photocatalysis, H₂O₂, Covalent organic framework, Nb₂C MXene, S-scheme heterojunction

许明阳, 李真真, 沈荣晨, 张欣, 张治红, 张鹏, 李鑫. 构建卟啉基共价有机框架与Nb₂C MXene的S型异质结并应用于光催化过氧化氢生产[J]. 催化学报, 2025, 70: 431-443.

Mingyang Xu, Zhenzhen Li, Rongchen Shen, Xin Zhang, Zhihong Zhang, Peng Zhang, Xin Li. Constructing S-scheme heterojunction between porphyrinyl covalent organic frameworks and Nb₂C MXene for photocatalytic H₂O₂ production[J]. Chinese Journal of Catalysis, 2025, 70: 431-443.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60247-0

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Fig. 1. (a) Schematic illustration of the preparation of the Tph-Dha-COF@Nb2C heterojunction. XRD patterns (b) and FT-IR spectra (c) of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C. FE-SEM (d), TEM and HR-TEM (e,f), and EDS mapping (g) images of Tph-Dha-COF@Nb2C.

Fig. 2. The high-resolution C 1s (a), N 1s (b), Nb 3d (c) and O 1s (d) of Tph-Dha-COF@Nb2C. N2 adsorption-desorption isotherms (e) and pore size distribution curves (f) of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C.

Fig. 3. (a) UV-vis diffuse reflectance spectroscopy of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C. Tauc plot (b), Mott-Schottky measurement (c) and energy band structures (d) of Nb2C-NH2 and Tph-Dha-COF. Transient photocurrent (e) and EIS spectra (f) of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C.

Fig. 4. UPS spectra in the normalized secondary electron cutoff energy (Ecutoff) regions (a) and calculated Φ stemming based on UPS spectra (b) of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C. In-situ XPS spectra of Nb 3d (c), C 1s (d), N 1s (e), and O 1s (f) of Tph-Dha-COF@Nb2C. (g) Charge transfer mechanism at the interface generated between Tph-Dha-COF and Nb2C-NH2.

Fig. 5. (a) Photocatalytic production of H2O2 for Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C under continuous O2 condition. (b) Photocatalytic reaction of Tph-Dha-COF@Nb2C under different atmosphere. (c) Photocatalytic synthesis performance of H2O2 compared with COFs and COF based catalysts in other literature (Table S2 for details). (d) Photocatalytic H2O2 generation of Tph-Dha-COF@Nb2C for 5 h. The effect of photocatalyst concentration on the H2O2 production (e) and five consecutive cycles (f) of Tph-Dha-COF@Nb2C for H2O2 generation. (g) AQY of Tph-Dha-COF@Nb2C at 365, 420, 450, 500, 600 nm bandpass filters. (h) SCC of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C at λ > 420 nm. (i) Photocatalytic H2O2 production over Tph-Dha-COF@Nb2C in the presence of different sacrificial agents.

Fig. 6. EPR spectra of ?O2? (a) and ?OH (b) for Tph-Dha-COF@Nb2C under different stimulation. (c) Kouteckly-Levich plots obtained by RDE tests in phosphate buffer (pH = 7) solution. (d) In-situ DRIFT spectra of Tph-Dha-COF@Nb2C under UV-vis irradiation at different times. (e) Free energy diagrams of Nb2C-NH2, Tph-Dha-COF and Tph-Dha-COF@Nb2C for the photosynthesis of H2O2 2e? ORR pathway. (f) Proposed 2e? ORR mechanism of H2O2 generation on Tph-Dha-COF@Nb2C.

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构建卟啉基共价有机框架与Nb₂C MXene的S型异质结并应用于光催化过氧化氢生产

Constructing S-scheme heterojunction between porphyrinyl covalent organic frameworks and Nb₂C MXene for photocatalytic H₂O₂ production

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