LSPR效应助力S型W18O49/ZnO异质结高效光催化CO2参与的苯胺N-甲酰化反应

doi:10.1016/S1872-2067(24)60149-X

催化学报 ›› 2024, Vol. 67: 124-134.DOI: 10.1016/S1872-2067(24)60149-X

LSPR效应助力S型W₁₈O₄₉/ZnO异质结高效光催化CO₂参与的苯胺N-甲酰化反应

陈家法^a^,^b, 白鹏^a^,^b, 袁士博^a^,^b, 何熠^a^,^b, 牛子凡^a^,^b, 赵宜成^a^,^b^,^d(), 李永丹^c

^a天津大学化工学院, 天津市应用催化科学与工程重点实验室, 天津大学化学工程联合国家重点实验室, 天津 300072, 中国
^b天津化学化工协同创新中心, 天津 300072, 中国
^c阿尔托大学化工学院, 化学与冶金工程系, 埃斯波, 芬兰
^d河北省工业副产气制燃料氢技术创新中心, 河北唐山 064099, 中国

收稿日期:2024-07-29 接受日期:2024-09-19 出版日期:2024-11-30 发布日期:2024-11-30
通讯作者: 赵宜成
基金资助:
国家重点研发项目(2022YFB4101800);国家自然科学基金(22075205)

LSPR-assisted W₁₈O₄₉/ZnO S-scheme heterojunction for efficient photocatalytic CO₂ N-formylation of aniline

Jiafa Chen^a^,^b, Peng Bai^a^,^b, Shibo Yuan^a^,^b, Yi He^a^,^b, Zifan Niu^a^,^b, Yicheng Zhao^a^,^b^,^d(), Yongdan Li^c

^aState Key Laboratory of Chemical Engineering (Tianjin University), Tianjin Key Laboratory of Applied Catalysis Science and Technology, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
^bCollaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072, China
^cDepartment of Chemical and Metallurgical Engineering, School of Chemical Engineering, Aalto University, Kemistintie 1, Espoo, P.O. Box 16100 Aalto FI-00076, Finland
^dHebei Technical Innovation Center for Fuel Hydrogen Production from Industrial By-product Gas, Tangshan 064099, Hebei, China

Received:2024-07-29 Accepted:2024-09-19 Online:2024-11-30 Published:2024-11-30
Contact: Yicheng Zhao
Supported by:
National Key Research and Development Program of China(2022YFB4101800);National Natural Science Foundation of China(22075205)

摘要/Abstract

摘要：

大量化石燃料快速消耗排放过量CO₂, 导致了包括温室效应和全球性气候变化在内的一系列严重后果, 对环境构成了巨大威胁. 利用CO₂作为原料生产高附加值化学品被广泛认为是一种能减少CO₂排放并实现可持续发展的有效方案. 在众多高效的CO₂转化途径中, CO₂参与的胺类N-甲酰化反应因为酰胺类产品在药物合成及工业溶剂等领域的大量应用而被密切关注. 与传统需要苛刻反应条件的热催化手段相比, 光催化CO₂参与的胺类N-甲酰化反应为CO₂转化为具有高附加值的酰胺类产品提供了一种更节能环保的方法. ZnO因具有合适的能带结构和适度的CO₂吸附能力, 在光催化CO₂转化领域备受关注. 然而, 单一ZnO光吸收范围窄及光生载流子复合快等问题限制了其进一步应用.

本文通过两步溶剂热法合成了W₁₈O₄₉/ZnO S型异质结光催化剂. 电感耦合等离子体发射光谱、X射线粉末衍射谱、扫描电镜以及透射电镜等结果证实了W₁₈O₄₉/ZnO异质结光催化剂的成功制备. 此外, 紫外-可见漫反射光谱的结果表明, W₁₈O₄₉独特的局域表面等离子体共振(LSPR)效应提高了催化剂整体的光响应能力. 结合莫特-肖特基曲线, 确定了各材料的能带结构. 同时, 利用光电化学测试以及稳态荧光光谱等表征方法, 研究了各材料的光生载流子分离和传递情况, 结果表明W₁₈O₄₉/ZnO复合材料表现出明显优于单一材料的载流子分离和传递能力. 借助原位光照X射线光电子能谱和密度泛函理论计算, 验证了W₁₈O₄₉/ZnO异质结体系的光生电荷转移路径符合S型机制, 解释了复合材料载流子分离和传递能力提升的原因. 在可见光照射下, W₁₈O₄₉/ZnO催化反应5 h后, 底物苯胺转化率达到99.1%, 产物甲酰苯胺的选择性达100%. 同时, 循环活性测试证明W₁₈O₄₉/ZnO复合材料具有良好的光催化稳定性. 此外, W₁₈O₄₉/ZnO异质结光催化剂还能够高效地催化包括芳香胺、杂环胺以及脂肪胺在内的多种胺类进行CO₂参与的N-甲酰化反应, 表明该材料在光催化CO₂参与的胺类N-甲酰化反应中具有良好的普适性. 利用原位光照傅里叶变换红外光谱以及原位光照电子顺磁共振光谱对CO₂参与的苯胺N-甲酰化反应中间体进行了动态监测, 确定了关键中间体含氮自由基的存在.

综上, 本文通过两步溶剂热法成功制备了一种W₁₈O₄₉/ZnO S型异质结光催化剂. W₁₈O₄₉独特的LSPR效应拓宽了催化剂整体的光吸收范围; S型异质结的构建显著促进了光生载流子的分离与传递, 同时保留了其较强的氧化还原能力, 从而实现了CO₂的快速功能化. 本文为解决ZnO存在的光吸收范围窄及光生载流子复合快等问题, 为开发用于高效转化CO₂生产高附加值化学品的异质结光催化剂提供了新思路.

关键词: 光催化, CO₂价值化, N-甲酰化, S型异质结, 氧化钨, 氧化锌

Abstract:

Designing highly efficient photocatalyst for the valorization of CO₂ is an ideal strategy to reduce greenhouse gas emissions and utilize solar energy. In this study, a S-scheme heterojunction photocatalyst is fabricated by solvothermal impregnation of ZnO on W₁₈O₄₉ for photocatalytic CO₂ N-formylation of aniline. The localized surface plasmon resonance effect of W₁₈O₄₉ improves the absorption capacity for long-wave light significantly, and the hot electrons generated in W₁₈O₄₉ with a high energy can migrate to the conduction band of ZnO and thus enhance the photocatalytic reduction ability. Meanwhile, the S-scheme heterojunction facilitates the separation of photoinduced charge carriers and preserves the redox ability of W₁₈O₄₉/ZnO composite photocatalyst. The conversion of aniline reaches 99.1% after 5 h reaction under visible light irradiation at room temperature with an N-formylaniline selectivity of 100%. A possible photocatalytic reaction mechanism is proposed. This study paves a promising way for the design of highly efficient photocatalyst and the sustainable utilization of CO₂.

Key words: Photocatalysis, CO₂ valorization, N-formylation, Step-scheme heterojunction, Tungsten oxide, ZnO

陈家法, 白鹏, 袁士博, 何熠, 牛子凡, 赵宜成, 李永丹. LSPR效应助力S型W₁₈O₄₉/ZnO异质结高效光催化CO₂参与的苯胺N-甲酰化反应[J]. 催化学报, 2024, 67: 124-134.

Jiafa Chen, Peng Bai, Shibo Yuan, Yi He, Zifan Niu, Yicheng Zhao, Yongdan Li. LSPR-assisted W₁₈O₄₉/ZnO S-scheme heterojunction for efficient photocatalytic CO₂ N-formylation of aniline[J]. Chinese Journal of Catalysis, 2024, 67: 124-134.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60149-X

https://www.cjcatal.com/CN/Y2024/V67/I12/124

图/表 9

Fig. 1. XRD patterns of the photocatalysts.

Fig. 2. SEM images of ZnO (a), W18O49 (b) and 30WZ composite (c). HRTEM image (d), SAED pattern (e) and STEM image and EDX elemental mappings (f) of 30WZ composite.

Fig. 3. (a) Aniline conversion and FA selectivity over different samples after 1 h reaction. (b) Mass spectra of the products with 12CO2 and 13CO2 as the feedstocks over 30WZ composite. (c) Aniline conversion and FA selectivity over 30WZ composite as a function of reaction time. (d) Stability of 30WZ composite during five 5-h reaction cycles.

Table 1 Photocatalytic N-formylation of various amines with CO2 over 30WZ.

Entry	Conversion (%)	Selectivity (%)
1	99.1	100
2	94.5	98.3
3	86.8	93.9
4	99.1	97.3
5	100	99.4
6	63.1	97.6
7	76.9	96.6
8	95.1	100
9	100	97.0
10	100	100
11	100	93.6
12	99.5	100

Fig. 4. UV-vis diffuse reflectance spectra (a), Tauc plots (b), Mott-Schottky plots (500 Hz) (c) and PL spectra (d) of the samples.

Fig. 5. Calculated Fermi levels and work functions for ZnO (101) face (a) and W18O49 (010) face (b). High-resolution XPS spectra of Zn 2p (c) and W 4f (d) of the samples.

Fig. 6. Mechanism of charge-transfer processes in S-scheme W18O49/ZnO heterojunction.

Fig. 7. (a) Aniline conversion and FA selectivity over 30WZ composite after 1 h reaction under various conditions. (b) In situ FTIR spectra during the reaction over 30WZ composite. (c) In situ EPR spectra after 10 min reaction over 30WZ composite in the dark and under light irradiation.

Fig. 8. Possible mechanism of photocatalytic N-formylation of aniline with CO2 over W18O49/ZnO composite.

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LSPR效应助力S型W₁₈O₄₉/ZnO异质结高效光催化CO₂参与的苯胺N-甲酰化反应

LSPR-assisted W₁₈O₄₉/ZnO S-scheme heterojunction for efficient photocatalytic CO₂ N-formylation of aniline

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