空心球状共价有机框架负载金纳米粒子用于光催化生产过氧化氢

doi:10.1016/S1872-2067(23)64580-2

催化学报 ›› 2024, Vol. 57: 143-153.DOI: 10.1016/S1872-2067(23)64580-2

空心球状共价有机框架负载金纳米粒子用于光催化生产过氧化氢

张勇^a, 邱俊逸^b, 朱必成^c, 孙国太^c, 程蓓^b, 王临曦^c^,^*()

^a湖北理工学院化学与化工学院, 矿区环境污染控制与修复湖北省重点实验室, 湖北黄石 435003
^b武汉理工大学材料复合新技术国家重点实验室, 湖北武汉 430070
^c中国地质大学材料与化学学院太阳燃料实验室, 湖北武汉 430074

收稿日期:2023-10-23 接受日期:2023-11-29 出版日期:2024-02-18 发布日期:2024-02-10
通讯作者: * 电子信箱: linxiwang91@126.com (王临曦).
基金资助:
国家自然科学基金(22378103);国家自然科学基金(52173065);国家自然科学基金(52073223);国家自然科学基金(22278324);国家自然科学基金(22302183);国家自然科学基金(22362004);国家自然科学基金(22208332);矿区环境污染控制与修复湖北省重点实验室开放基金(2022XZ106)

Hollow spherical covalent organic framework supported gold nanoparticles for photocatalytic H₂O₂ production

Yong Zhang^a, Junyi Qiu^b, Bicheng Zhu^c, Guotai Sun^c, Bei Cheng^b, Linxi Wang^c^,^*()

^aSchool of Chemistry and Chemical Engineering, Hubei Key Laboratory of Mine Environmental Pollution Control & Remediation, Hubei Polytechnic University, Huangshi 435003, Hubei, China
^bState Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, Hubei, China
^cLaboratory of Solar Fuel, Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430078, Hubei, China

Received:2023-10-23 Accepted:2023-11-29 Online:2024-02-18 Published:2024-02-10
Contact: * E-mail: linxiwang91@126.com (L. Wang).
Supported by:
National Natural Science Foundation of China(22378103);National Natural Science Foundation of China(52173065);National Natural Science Foundation of China(52073223);National Natural Science Foundation of China(22278324);National Natural Science Foundation of China(22302183);National Natural Science Foundation of China(22362004);National Natural Science Foundation of China(22208332);Open Foundation of Hubei Key Laboratory of Mine Environmental Pollution Control & Remediation(2022XZ106)

摘要/Abstract

摘要：

过氧化氢是一种高效的绿色氧化剂, 广泛应用于纸浆漂白、外科消毒、废水处理和化学合成等领域. 目前, 过氧化氢的工业生产仍依赖于传统的蒽醌氧化法, 该方法存在能耗高、污染大以及工艺复杂等问题. 以太阳能为驱动力, 水和氧气作为原料, 利用半导体材料光催化生产过氧化氢被认为是一种清洁、安全、经济和节能的技术. 该技术的关键是开发高效稳定的半导体光催化材料. 共价有机框架(COF)是一种可用于光催化产过氧化氢的新型晶态多孔有机材料, 具有结构可调控、密度低、比表面积大、热稳定性和化学稳定性高等优点, 但其应用受到光生载流子快速复合的限制. 将助催化剂金纳米粒子负载在COF表面, 可以有效促进光生载流子的迁移与分离, 从而获得较好的光催化产双氧水性能. 然而, 这方面的研究尚未受到较多的关注.

本文采用NaBH₄还原法将金纳米粒子原位负载在一种空心球状COF (TB-COF)的表面, 制得了不同Au含量的Au/TB-COF复合物(记为AT-x, 其中x代表复合物中Au的质量百分含量), 并系统研究了该材料光催化生产过氧化氢的性能. 粉末X射线衍射(XRD)、透射电子显微镜(TEM)和傅里叶转换红外光谱(FT-IR)等表征结果证明了Au/TB-COF复合物的成功制备, 且发现原位负载的金纳米粒子并没有改变TB-COF的晶型、形貌和化学结构. 在光催化反应中, 以乙醇作为牺牲剂时, 复合物AT-1的性能最佳, 表现出最高的过氧化氢生成速率常数(K_f)和最低的过氧化氢分解速率常数(K_d), 在可见光照射下过氧化氢生成速率达到6067 μmol g⁻¹ h⁻¹, 超过大多文献报道的COF基光催化剂性能. 经4次光催化循环反应后, AT-1催化生成过氧化氢的产率略有下降, 且FTIR谱、XRD谱和FESEM显示光催化反应前后AT-1的结构和形态几乎没有变化, 表明其具有较好的光催化稳定性. 此外, 在本实验所制得的AT-x复合物中, AT-1具有最短的荧光平均寿命、最大的光电流响应和最小的阻抗, 表明其具有最高的光生载流子迁移和分离能力. 原位辐照X射线光电子能谱结果表明, 界面电子在光照前后均从TB-COF转移到金纳米粒子, 与密度泛函理论计算结果一致. 电子顺磁共振和原位漫反射傅里叶变换红外光谱等实验证实了光催化过程中超氧自由基的存在, 这表明AT-1光催化生产过氧化氢是连续两步单电子氧气还原的过程. 实验还发现, 当O₂被N₂替代时, 几乎检测不到过氧化氢的产生, 说明过氧化氢来源于O₂的还原反应. 当用硝酸银和对苯醌分别作为捕获剂来消除∙O₂⁻和e⁻时, 光催化过氧化氢的产率显著下降, 可推断∙O₂⁻和e⁻是产生过氧化氢的关键物种.

综上, 本文详细研究了金纳米粒子作为助催化剂对COF光催化生成过氧化氢性能的促进作用, 可为设计高效光催化生成过氧化氢的COF基催化剂提供参考. 目前, 光催化生产过氧化氢技术仍处于起步阶段, 其产率仍处于mmol g⁻¹ h⁻¹的水平, 尚不能达到工业生产要求. 开发高效的半导体催化剂是实现高效光催化生产过氧化氢的关键. 未来还需要进一步提高光催化产过氧化氢的生成效率和选择性, 解决O₂的有效吸附、可见光有效利用、光生载流子的分离与转移效率等问题, 以推进光催化产过氧化氢技术的工业生产和商业应用.

关键词: 共价有机框架, 金纳米粒子, 光催化, 双氧水生产, 氧气还原

Abstract:

Covalent organic frameworks (COFs) are porous crystalline materials with promising applications in photocatalysis, but their performance is greatly hampered by the fast recombination of photogenerated carriers. Herein, a hollow spherical COF was synthesized via the condensation polymerization of 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-benzenetricarbaldehyde, and Au nanoparticles were in-situ deposited onto the COF through NaBH₄ reduction to ameliorate the photocatalytic performance. The composite exhibits impressive photocatalytic H₂O₂-production performance with the highest H₂O₂-evolution rate of 6067 μmol g⁻¹ h⁻¹ under visible light irradiation, which is about 1.9 times that of the pristine COF. The enhanced photocatalytic activity was ascribed to improved light absorption, abundant active Au sites, and efficient transfer and separation of photogenerated carriers in space. This work provides an avenue for designing high-performance H₂O₂-production photocatalysts by decorating porous COFs with active noble-metal sites.

Key words: Covalent organic frameworks, Au nanoparticle, Photocatalysis, H₂O₂ production, O₂ reduction

张勇, 邱俊逸, 朱必成, 孙国太, 程蓓, 王临曦. 空心球状共价有机框架负载金纳米粒子用于光催化生产过氧化氢[J]. 催化学报, 2024, 57: 143-153.

Yong Zhang, Junyi Qiu, Bicheng Zhu, Guotai Sun, Bei Cheng, Linxi Wang. Hollow spherical covalent organic framework supported gold nanoparticles for photocatalytic H₂O₂ production[J]. Chinese Journal of Catalysis, 2024, 57: 143-153.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64580-2

https://www.cjcatal.com/CN/Y2024/V57/I2/143

图/表 11

Fig. 1. Preparation schematics of Au/TB-COF.

Fig. 2. TEM images of AT-1. (a) Low-resolution TEM image. (b) HRTEM image. (c) The crystal lattice of Au nanoparticle in a selected area. (d-g) The elemental mapping images.

Fig. 3. PXRD patterns (a) and TGA curves (b) of TB-COF and Au/TB-COF. (c) FTIR spectra of TAPB, BTCA, TB-COF, and AT-1. (d) N2 adsorption-desorption isotherms of TB-COF and AT-1, where the inset shows pore size distribution.

Fig. 4. (a) UV-vis DRS spectra of TB-COF and Au/TB-COF. (b) Mott-Schottky plots of TB-COF at different frequencies.

Fig. 5. ISI-XPS spectra of Au 4f (a) and N 1s (b) for Au, TB-COF, and AT-1 under different conditions.

Fig. 6. Front-view (a) and side-view (b) of charge density difference of Au/TB-COF. The yellow and blue regions represent electron accumulation and depletion, respectively.

Fig. 7. Photocatalytic H2O2 production (a) and photoinduced H2O2 decomposition (b) over various samples under visible light irradiation. (c) Fitted Kf and Kd for photocatalytic H2O2 production. (d) Cyclic tests of AT-1 for H2O2 production.

Fig. 8. Transient photocurrent curves (a) and EIS spectra (b) of the as-prepared samples.

Fig. 9. (a) H2O2 evolution rate over AT-1 under various conditions. (b) EPR signals of DMPO-?O2? on TB-COF and AT-1 in methanol after irradiation by a 300 W Xe lamp for 5 min.

Fig. 10. In-situ DRIFT spectra of AT-1 under a gas mixture flow containing H2O, EtOH, and O2 in dark (a) and under light irradiation (b).

Fig. 11. Proposed mechanism of photocatalytic H2O2 production on Au/TB-COF.

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空心球状共价有机框架负载金纳米粒子用于光催化生产过氧化氢

Hollow spherical covalent organic framework supported gold nanoparticles for photocatalytic H₂O₂ production

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空心球状共价有机框架负载金纳米粒子用于光催化生产过氧化氢

Hollow spherical covalent organic framework supported gold nanoparticles for photocatalytic H2O2 production

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Hollow spherical covalent organic framework supported gold nanoparticles for photocatalytic H₂O₂ production