Au/Co3O4-ZnO催化剂上CO2-丙三醇羰基化合成丙三醇碳酸酯

doi:10.3866/PKU.WHXB202308005

物理化学学报 >> 2024, Vol. 40 >> Issue (9): 2308005.doi: 10.3866/PKU.WHXB202308005

Au/Co₃O₄-ZnO催化剂上CO₂-丙三醇羰基化合成丙三醇碳酸酯

李亚晋¹, 刘会敏²^,*(), 马兰³, 刘佳雄¹, 贺德华¹^,*()

¹ 清华大学化学系, 北京 100084
² 辽宁工业大学化学与环境工程学院, 辽宁锦州 121001
³ 防化学院, 北京 102205

收稿日期:2023-08-03 修回日期:2023-10-06 录用日期:2023-10-10 发布日期:2023-10-16
通讯作者: Email: hedeh@mail.tsinghua.edu.cn (贺德华)liuhuimin08@tsinghua.org.cn; Tel.: +86-13522893188 (刘会敏)
基金资助:
国家自然科学基金(21573120); 辽宁省教育厅基金(JQL202015401)

Photothermal Synthesis of Glycerol Carbonate via Glycerol Carbonylation with CO₂ over Au/Co₃O₄-ZnO Catalyst

Yajin Li¹, Huimin Liu²^,*(), Lan Ma³, Jiaxiong Liu¹, Dehua He¹^,*()

¹ Department of Chemistry, Tsinghua University, Beijing 100084, China
² School of Chemical and Environmental Engineering, Liaoning University of Technology, Jinzhou 121001, Liaoning Province, China
³ Institute of NBC Defense, Beijing 102205, China

Received:2023-08-03 Revised:2023-10-06 Accepted:2023-10-10 Published:2023-10-16
Contact: Email: hedeh@mail.tsinghua.edu.cn (Dehua He)liuhuimin08@tsinghua.org.cn; Tel.: +86-13522893188 (Huimin Liu)
Supported by:
the National Natural Science Foundation of China(21573120); Education Department of Liaoning Province(JQL202015401)

摘要/Abstract

摘要：

CO₂与丙三醇羰基化合成丙三醇碳酸酯是一项前景广阔的CO₂利用途径。尽管该反应可以通过热驱动的催化途径实现，但受热力学平衡的限制。在本研究中，我们开发了xAu/20Co₃O₄-ZnO系列催化剂，并引入太阳光辐射能量来实现光热协同催化反应，以突破热力学限制。由p型半导体Co₃O₄和n型半导体ZnO复合而成的Co₃O₄-ZnO氧化物具有异质结构，而负载于Co₃O₄-ZnO表面的Au纳米粒子具有局域表面等离子体共振(LSPR)效应。我们研究了xAu/20Co₃O₄-ZnO的可见光吸收性能、光生电子-空穴对分离效率以及Au添加对xAu/20Co₃O₄-ZnO催化剂光热协同催化性能的影响。此外，我们还研究了Au掺杂对xAu/20Co₃O₄-ZnO的体相和表面性质(晶相结构、形貌、比表面积、元素结合能、表面酸碱性、还原行为)的影响。研究结果显示，Au/20Co₃O₄-ZnO的异质结构有助于吸收可见光并提高电子-空穴对的分离效率。负载于Co₃O₄-ZnO表面的Au纳米颗粒约为50 nm，Au的加入改变了Zn和Co的电子密度，增强了Co物种的还原性，并增加了Co₃O₄-ZnO表面的氧空位。此外，Au纳米粒子的LSPR进一步提高了Au/20Co₃O₄-ZnO的可见光吸收能力，并改善了光生电子-空穴对的分离，从而提高了光热协同催化性能。在优化的条件下(150 ℃、5 MPa、6 h、25 W可见光照射)，2%Au/20Co₃O₄-ZnO表现出良好的光热协同催化性能，丙三醇碳酸酯的产率为6.5%。这项工作有望为合理设计更好的CO₂-丙三醇羰基化制丙三醇碳酸酯光热催化剂提供参考。

关键词: CO₂利用, 丙三醇羰基化, 丙三醇碳酸酯, 等离子体金属, 光热催化

Abstract:

Glycerol carbonylation with CO₂ to synthesize glycerol carbonate is a promising approach for CO₂ utilization. This reaction can be achieved through a thermally-driven catalytic pathway, but it is constrained by thermodynamic equilibrium. In the present study, we introduced solar energy into the reaction system to enable a photo-thermal synergistic catalytic reaction, breaking through the thermodynamic limitations. We developed a series of xAu/20Co₃O₄-ZnO catalysts, where Co₃O₄-ZnO, a composite of p-type semi-conductor Co₃O₄ and n-type semi-conductor ZnO, exhibited a heterojunction structure, and Au nanoparticles loaded onto the surface of Co₃O₄-ZnO revealed the localized surface plasmon resonance (LSPR). We investigated the ability of xAu/Co₃O₄-ZnO to absorb visible light absorption, the efficiency of separating photo-generated hole-electron pairs, and the impact of Au on the photothermal synergistic catalytic performances of Au/Co₃O₄-ZnO catalysts. We also examined the effects of Au doping on the bulk and surface properties, including crystalline structures, morphologies, specific surface areas and pore structures, the binding energies of the elements, surface acid-base sites, and reduction behaviors of xAu/Co₃O₄-ZnO. Our findings revealed that the heterojunction structure of Au/20Co₃O₄-ZnO facilitated visible light absorption and hole-electron pair separation. The size of Au nano-particles (NPs) loaded on Co₃O₄-ZnO surface was approximately 50 nm. The loading of Au altered the electron density of Co and Zn, improved the reducibility of Co species, and enhanced the presence of oxygen vacancies on Co₃O₄-ZnO surface. The LSPR of Au NPs further enhanced the visible light absorption capacity of Au/20Co₃O₄-ZnO, and improved the separating of photogenerated hole-electron pairs, thus enhancing the photothermal catalytic performances. With the optimizing conditions (150 ℃, 5 MPa, 6 h, and 225 W visible light irradiation), the 2%Au/20Co₃O₄-ZnO catalyst demonstrated excellent performances, yielding a glycerol carbonate yield of 6.5%. This study is expected to serve as a reference for the rational design of improved photothermal catalysts for glycerol carbonylation with CO₂ to produce glycerol carbonate in the future.

Key words: CO₂ utilization, Glycerol carbonylation, Glycerol carbonate, Plasmonic metal, Photo-thermal catalysis

李亚晋, 刘会敏, 马兰, 刘佳雄, 贺德华. Au/Co₃O₄-ZnO催化剂上CO₂-丙三醇羰基化合成丙三醇碳酸酯[J]. 物理化学学报, 2024, 40(9), 2308005. doi: 10.3866/PKU.WHXB202308005

Yajin Li, Huimin Liu, Lan Ma, Jiaxiong Liu, Dehua He. Photothermal Synthesis of Glycerol Carbonate via Glycerol Carbonylation with CO₂ over Au/Co₃O₄-ZnO Catalyst[J]. Acta Phys. -Chim. Sin. 2024, 40(9), 2308005. doi: 10.3866/PKU.WHXB202308005

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB202308005

https://www.whxb.pku.edu.cn/CN/Y2024/V40/I9/2308005

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Catalyst	Lattice oxygen (O_L) ^a	Adsorbed oxygen (O_S) ^b	Hydroxyl group (O_H) ^c
20Co₃O₄-ZnO	10.8%	30.3%	58.9%
0.1%Au/20Co₃O₄-ZnO	11.7%	36.4%	51.9%
0.5%Au/20Co₃O₄-ZnO	13.4%	41.3%	45.3%
2%Au/20Co₃O₄-ZnO	16.3%	52.3%	31.4%

Catalyst	Base sites (μmolCO₂∙g⁻¹)			Total base sites (μmol CO₂∙g⁻¹)
Catalyst	Weak (< 250 ºC)	Medium (250–450 ºC)	Strong (> 450 ºC)	Total base sites (μmol CO₂∙g⁻¹)
20Co₃O₄-ZnO	33.08 (74% ^a)	10.49 (23%)	1.27 (3%)	44.84
0.5%Au/20Co₃O₄-ZnO	22.68 (55%)	3.94 (10%)	14.25 (35%)	40.87
1%Au/20Co₃O₄-ZnO	18.12 (54%)	2.28 (7%)	12.86 (39%)	33.26
2%Au/20Co₃O₄-ZnO	17.86 (53%)	2.06 (6%)	13.40 (40%)	33.32

Support/catalyst	Specific surface area/(m²∙g⁻¹)
20Co₃O₄-ZnO	20.2
0.1%Au/20Co₃O₄-ZnO	19.9
1.0%Au/20Co₃O₄-ZnO	20.9

Recycle number	Glycerol carbonate yield (%)
1	6.5
2	6.3
3	6.2

Catalyst	Reaction conditions	Performance	Reference
Au/Co₃O₄-ZnO	100 mL stainless steel autoclave, 10 mmol glycerol, 0.50 g catalyst, 20 mL dimethyl fumarate, 150 ℃, 5 MPa CO₂, 6 h and 225 W visible light irradiation.	6.5% glycerol carbonate yield.	This work
Zn-doped CeO₂	50 mL high-pressure reactor, 0.92 g glycerol (10 mmol), 0.17 g catalyst, 3.12 g 2-cyanopyridine, 10 mL dimethylformamide, 150 ℃, 40 bar (1 bar = 0.1 MPa) CO₂ pressure, and 5 h.	19.1% glycerol conversion and 18.9% glycerol carbonate yield.	44
La/ZIF-8	100 mL stainless steel autoclave, 0.1 g catalyst, 7 bar CO₂, 150 ℃, in the presence of MgCO₃ as the dehydrating agent.	46.5% glycerol conversion and 35.3% glycerol carbonate yield.	45
CeO₂	100 mL stainless steel autoclave, 10 mmol glycerol, 0.34 g CeO₂, 30 mmol 2-cyanopyridine, 10 mL dimethyl formamide, 150 ℃, 4 MPa and reaction time 5 h.	20.8% glycerol carbonate yield.	16
Cu/La₂O₃	100 mL stainless steel autoclave, glycerol 50 mmol, acetonitrile 10 mL, catalyst 0.08 g, 150 ℃, CO₂ 7 MPa, 3 h.	8.9% glycerol conversion and 29.3% selectivity towards glycerol carbonate.	46
Zn/Al/La/X (X = F, Cl, Br)	50 mL stainless-steel autoclave, 4.60 g glycerol, 0.14 g catalyst and 5.0 mL acetonitrile, CO₂ 4.0 MPa, 170 ℃ for 12 h.	35.5% glycerol conversion and 16.0% glycerol carbonate yield.	47
La₂O₂CO₃-ZnO	100 mL stainless steel autoclave, 0.92 g glycerol, 0.50 g catalyst, 20 mL of N, N-dimethylformamide, 150 ℃, 5.5 MPa CO₂, and reaction time of 6 h, visible light irradiation.	6.9% glycerol conversion and 6.1% glycerol carbonate yield.	24
Au/ZnWO₄-ZnO	100 mL stainless steel autoclave, 10 mmol glycerol, 1.0 g catalyst, 20 mL N, N-dimethylformamide, 5.0 MPa CO₂, 150 ℃, 6 h, with 250 W visible light irradiation.	8.4% glycerol carbonate yield.	48

Au/Co₃O₄-ZnO催化剂上CO₂-丙三醇羰基化合成丙三醇碳酸酯

Photothermal Synthesis of Glycerol Carbonate via Glycerol Carbonylation with CO₂ over Au/Co₃O₄-ZnO Catalyst

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Catalyst	Reaction condition	Glycerol carbonate yield (%)
2%Au/20Co₃O₄-ZnO	Thermal	4.5
2%Au/20Co₃O₄-ZnO	Photo-thermal	6.5
20Co₃O₄-ZnO	Thermal	3.1
20Co₃O₄-ZnO	Photo-thermal	5.3
2%Au/Co₃O₄	Thermal	2.6
2%Au/Co₃O₄	Photo-thermal	3.2
2%Au/ZnO	Thermal	1.3
2%Au/ZnO	Photo-thermal	1.8

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