双向主客体作用促进水溶液中选择性光催化CO2还原与醇氧化

doi:10.1016/S1872-2067(23)64509-7

催化学报 ›› 2023, Vol. 52: 176-186.DOI: 10.1016/S1872-2067(23)64509-7

双向主客体作用促进水溶液中选择性光催化CO₂还原与醇氧化

张雯^a^,¹, 宋彩彩^a^,¹, 王嘉蔚^b, 蔡舒婷^a, 高梦语^a, 冯有祥^a, 鲁统部^a^,^*()

^a天津理工大学化学与化工学院, 有机太阳能电池与光化学转化天津重点实验室, 材料科学与工程学院, 新能源材料与低碳技术研究院, 材料微结构教育部国际合作联合实验室, 天津300384
^b中山大学化学学院, 环境与能源化学系KLGHEI, 广东广州510275

收稿日期:2023-05-17 接受日期:2023-08-13 出版日期:2023-09-18 发布日期:2023-09-25
通讯作者: *电子信箱: lutongbu@tjut.edu.cn (鲁统部).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(21702146);国家自然科学基金(21790052);国家自然科学基金(21931007);国家重点研发计划项目(2017YFA0700104);国家111项目(D17003);天津市自然科学基金资助项目(19JCQNJC05500)

Bidirectional host-guest interactions promote selective photocatalytic CO₂ reduction coupled with alcohol oxidation in aqueous solution

Wen Zhang^a^,¹, Cai-Cai Song^a^,¹, Jia-Wei Wang^b, Shu-Ting Cai^a, Meng-Yu Gao^a, You-Xiang Feng^a, Tong-Bu Lu^a^,^*()

^aMOE International Joint Laboratory of Materials Microstructure, Institute for New Energy Materials and Low Carbon Technologies, School of Materials Science and Engineering, Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384, China
^bKLGHEI of Environment and Energy Chemistry, School of Chemistry, Sun Yat-sen University, Guangzhou 510275, Guangdong, China

Received:2023-05-17 Accepted:2023-08-13 Online:2023-09-18 Published:2023-09-25
Contact: *E-mail: lutongbu@tjut.edu.cn (T.-B. Lu).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21702146);National Natural Science Foundation of China(21790052);National Natural Science Foundation of China(21931007);National Key R&D Program of China(2017YFA0700104);111 Project of China(D17003);Natural Science Foundation of Tianjin(19JCQNJC05500)

摘要/Abstract

摘要：

CO₂还原与H₂O氧化耦合被认为是将太阳能转化为化学能的理想方法. 然而, H₂O氧化反应的显著动力学障碍限制了该类反应的转化效率. 此外, 额外的电子牺牲剂的消耗不仅在经济上不可行, 而且浪费了光生空穴的氧化能力. 因此, 将CO₂还原与有机物的有效氧化相结合将是有效利用太阳能和解决能源危机的有效途径之一. 对于包含光敏剂、催化剂和反应底物的离散光催化体系来说, 电子转移效率主要由离散组分之间的扩散过程控制. 为了提高光反应组分之间的电子转移效率, 研究人员尝试通过共价键在催化剂和光敏剂之间建立“桥梁”, 从而获得更快的电子转移速率. 然而, 该类体系存在合成过程复杂、共价键断裂及使用贵金属等问题. 与共价键相比, 非共价体系更便于合成, 且具有更好的稳定性.

本文利用双向主客体相互作用构筑高效光催化体系, 其中水溶性β-环糊精修饰的CdS纳米晶与CoTPP(助催化剂)和有机醇(反应底物)均通过非共价主客体作用连接, 促使光生电子和光生空穴的同步快速消耗. 核磁共振氢谱结果表明, 环糊精作为主体分子可以识别客体分子四苯基卟啉钴与呋喃醇. 利用Job曲线测得环糊精与四苯基卟啉钴以及呋喃醇的键合比分别为2:1和1:1. 紫外-可见吸收光谱结果表明, 环糊精与四苯基卟啉钴以及呋喃醇之间存在不同强度的主客体键合. 光催化CO₂还原反应与呋喃醇氧化性能测试结果表明, 与无配体的CdS纳米晶(CdS-BF₄)以及其它配体(油酸、2-巯基乙醇和硫代甘油)修饰的CdS纳米晶相比, 环糊精修饰的CdS-CD纳米晶在水相中表现出更高的CO₂还原为HCOOH的活性与选择性, 同时, 表现出最佳的呋喃醇氧化活性与选择性. 相反, 表面无配体的CdS-BF4纳米晶活性较低, 且有严重的析氢副反应发生. 为了更好地理解双向主客体相互作用对光反应性能的贡献, 利用一系列稳态和瞬态荧光光谱实验研究了三个组分之间的电子转移过程. 结果表明, CdS-CD与CoTPP之间以及CdS-CD与呋喃醇之间的双向主客体相互作用可以有效促进这些组分之间的电子转移过程. 原位漫反射傅立叶变换红外光谱和密度泛函理论研究表明, 随着光辐射时间的增加, HCOO*信号逐渐增强. 电子顺磁共振波谱结果表明, 在光催化呋喃醇氧化的过程中产生了呋喃醇苄基自由基. 在以上光还原和光氧化的全反应过程中, 双向主客体作用同时将助催化剂和反应物聚集在吸光物质CdS NCs表面, 这对于促进快速电子/空穴转移和随后的氧化还原反应发挥着关键作用.

综上所述, 选择合适的有机物不仅可以促进光还原反应的发生, 还可以生产更高附加值的化学品. 本文采用双向主客体策略构建新型的人工光合作用系统, 为构建具有实际应用潜能的人工光合作用系统提供了新的思路.

关键词: 人工光合成, 主客体相互作用, CO₂还原, 醇氧化, 快速电子转移

Abstract:

Existing artificial photosynthesis systems often underperform due to challenges in water oxidation and extensive photogenerated carrier transfer. Herein, we demonstrate that β-cyclodextrin-decorated CdS nanocrystals (CdS-CD) can simultaneously anchor cobalt tetraphenyl porphyrin (CoTPP) catalysts and alcohol reductants onto CdS surfaces through bidirectional host-guest interactions between β-CD and CoTPP/alcohol. This configuration ensures swift electron transfer from CdS to β-CD bonded CoTPP, facilitating CO₂ reduction to HCOOH. Results showcase a remarkable yield of 1610 μmol g^-1 h^-1 and a 96.5% selectivity. Meanwhile, photogenerated holes in CdS are efficiently neutralized by β-CD bonded furfuryl alcohol, achieving a furfural yield of 1567 μmol g^-1 h^-1 and > 99% selectivity. In contrast, the discrete CoTPP-CdS system achieved a HCOOH yield of only 306 μmol g^-1 h^-1 and a poor HCOOH selectivity of 46.4%. It was also observed that the CoTPP@CdS-CD system maintained high CO₂-to-HCOOH conversion rates when using other alcohols as reductants.

Key words: Artificial photosynthesis, Host-guest interaction, CO₂ reduction, Alcohol oxidation, Fast electron transfer

张雯, 宋彩彩, 王嘉蔚, 蔡舒婷, 高梦语, 冯有祥, 鲁统部. 双向主客体作用促进水溶液中选择性光催化CO₂还原与醇氧化[J]. 催化学报, 2023, 52: 176-186.

Wen Zhang, Cai-Cai Song, Jia-Wei Wang, Shu-Ting Cai, Meng-Yu Gao, You-Xiang Feng, Tong-Bu Lu. Bidirectional host-guest interactions promote selective photocatalytic CO₂ reduction coupled with alcohol oxidation in aqueous solution[J]. Chinese Journal of Catalysis, 2023, 52: 176-186.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64509-7

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图/表 6

Scheme 1. (a) Four different connection modes between reductant, photosensitizer, and catalyst in a photocatalytic system. (b) Self-assembly of CdS-CD NCs with CoTPP through host-guest interactions and their photoredox reactions of CO2 to HCOOH and furfuryl alcohol to furfural.

Fig. 1. (a) CV curves for CoTPP bonded on Au electrode covered with ?S-β-CD in 0.5 mol L?1 KHCO3 solution (inset: CoTPP in DMF). (b) CV curves for furfuryl alcohol. (c) Tauc plot (αhv)2 vs. photon energy (inset) and Mott-Schottky plot of CdS-CD. (d) Band structures of CdS-CD and redox potentials of CoTPP and furfuryl alcohol.

Fig. 2. (a) Job's plot of CoTPP/β-CD (red dot) and furfuryl alcohol/β-CD (black dot), ?A = A(with β-CD) ? A(without β-CD), where A refers to the absorbance of CoTPP or furfuryl alcohol, and ?A represents the change of the absorbance for CoTPP/furfuryl after adding various proportions of β-CD. (b) UV-vis absorption spectra changes for CoTPP upon the addition of β-CD in water (inset: the calculated binding constant (KS) value). (c) DLS measurements of CdS-CD and CoTPP@CdS-CD assembly. (d) TEM image of CoTPP@CdS-CD assembly (inset: size distribution of individual CdS-CDs).

Table 1 Comparative experiments for the photocatalytic reduction of CO2 coupled with furfuryl alcohol oxidation.

Entry	Ps	H₂(μmol g^-1 h^-1)	HCOOH (μmol g^-1 h^-1)	Select. HCOOH (%)	Furfural (μmol g^-1 h^-1)	Select. furfural (%)	e^-/h⁺
1	CdS-CD	47.0	1609.9	96.5	1567.0	> 99	1.05
2	CdS-BF₄	352.5	305.5	46.4	705.0	> 99	0.93
3	CdS-OA	0	70.1	> 99	68.2	> 99	1.03
4	CdS-ME	523.9	621.6	54.3	605.7 (221.1)	73.2	1.09
5	CdS-BF₄+CD	11.8	481.8	97.6	519.2	> 99	0.95
6 ^a	CdS-CD	37.6	477.2	96.1	474.9	> 99	1.08
7 ^b	CdS-CD	74.5	634.1	89.5	793.2	> 99	0.89

Fig. 3. (a) Production of HCOOH over CdS-OA, CdS-CD, CdS-BF4, the physical mixture of CdS-BF4 and β-CD, CdS-CD+AD, and CdS-ME. (b) Comparison of photocatalytic systems coupling the CO2 reduction with the oxidation of alcohols. (c) Fluorescence decay traces of CdS-CD with furfuryl alcohol and CoTPP. (d) In-situ Co 2p XPS spectra for the CoTPP@CdS-CD assembly under irradiation by a 300 W Xe lamp equipped with a 420 nm light filter.

Fig. 4. (a) EPR spectra of the photoreactions under dark and illumination conditions. (b) Proposed mechanism of CoTPP@CdS-CD assembly for CO2 reduction and furfuryl alcohol oxidation. (c) In-situ DRIFT spectra of CO2 photocatalytic reduction under the atmosphere of CO2. (d) DFT calculated energy diagram for CO2 reduction catalyzed by CoTPP. Optimized structures of the intermediates are shown with brown (carbon), pink (hydrogen), red (oxygen), gray (nitrogen), and blue (cobalt).

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双向主客体作用促进水溶液中选择性光催化CO₂还原与醇氧化

Bidirectional host-guest interactions promote selective photocatalytic CO₂ reduction coupled with alcohol oxidation in aqueous solution

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