Crystal facet-dependent CO<sub>2</sub> cycloaddition to epoxides over ZnO catalysts

doi:10.1007/s11705-024-2412-6

Front. Chem. Sci. Eng.

2024, Vol. 18

Issue (5) : 53 https://doi.org/10.1007/s11705-024-2412-6

Crystal facet-dependent CO₂ cycloaddition to epoxides over ZnO catalysts

Yongjian Wei^1,², Ying Li^1,²(

), Yunfei Xu^1,², Yinghui Sun^1,², Tong Xu^1,², Haiou Liang^1,², Jie Bai^1,²

¹. Inner Mongolia Key Laboratory of Industrial Catalysis, Hohhot 010051, China
². College of Chemical Engineering, Inner Mongolia University of Technology, Hohhot 010051, China

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Abstract

With regard to green chemistry and sustainable development, the fixation of CO₂ into epoxides to form cyclic carbonates is an attractive and promising pathway for CO₂ utilization. Metal oxides, renowned as promising eco-friendly catalysts for industrial production, are often undervalued in terms of their impact on the CO₂ addition reaction. In this work, we successfully developed ZnO nanoplates with (002) surfaces and ZnO nanorods with (100) surfaces via morphology-oriented regulation to explore the effect of crystal faces on CO₂ cycloaddition. The quantitative data obtained from electron paramagnetic resonance spectroscopy indicated that the concentration of oxygen vacancies on the ZnO nanoplate surfaces was more than twice that on the ZnO nanorod surfaces. Density functional theory calculations suggested that the (002) surfaces have lower adsorption energies for CO₂ and epichlorohydrin than the (100) surfaces. As a result, the yield of cyclochloropropene carbonate on the ZnO nanoplates (64.7%) was much greater than that on the ZnO nanorods (42.3%). Further evaluation of the reused catalysts revealed that the decrease in the oxygen vacancy concentration was the primary factor contributing to the decrease in catalytic performance. Based on these findings, a possible catalytic mechanism for CO₂ cycloaddition with epichlorohydrin was proposed. This work provides a new idea for the controllable preparation of high-performance ZnO catalysts for the synthesis of cyclic carbonates from CO₂ and epoxides.

Keywords carbon dioxide cycloaddition zinc oxide crystal face oxygen vacancy

Corresponding Author(s): Ying Li

About author:

Li Liu and Yanqing Liu contributed equally to this work.

Just Accepted Date: 19 January 2024 Issue Date: 15 April 2024

Cite this article:

Yongjian Wei,Ying Li,Yunfei Xu, et al. Crystal facet-dependent CO₂ cycloaddition to epoxides over ZnO catalysts[J]. Front. Chem. Sci. Eng., 2024, 18(5): 53.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-024-2412-6
https://academic.hep.com.cn/fcse/EN/Y2024/V18/I5/53

Fig.1 XRD patterns of P-ZnO and R-ZnO catalysts.

Fig.2 SEM images of (a) P-ZnO and (b) R-ZnO; HRTEM images and crystal plots of (c, e) P-ZnO and (d, f) R-ZnO.

Tab.1 BET and BJH results for the P-ZnO and R-ZnO materials

Fig.3 (a) N₂-physisorption isotherms of P-ZnO and R-ZnO and (b) pore size distributions of P-ZnO and R-ZnO.

Fig.4 (a) Raman spectra of P-ZnO and R-ZnO, (b) O 1s XPS spectra of P-ZnO and R-ZnO, (c) EPR spectra of P-ZnO and R-ZnO, and (d) total spin number associated with oxygen vacancies and zinc vacancies of P-ZnO and R-ZnO.

Fig.5 (a) The effects of reaction temperature on the CO₂ cycloaddition reaction over ZnO catalysts (reaction conditions: 6 mL of ECH, 0.05 mL of DMF, 0.1 g of ZnO catalysts, 125 °C, 2 MPa CO₂, and 4 h). (b) Arrhenius plot of the reaction over P-ZnO and R-ZnO.

Fig.6 Recyclability of (a) P-ZnO and (b) R-ZnO catalysts in CO₂ cycloaddition (reaction conditions: 6 mL of ECH, 0.05 mL of DMF, 0.1 g of ZnO catalyst, 130 °C, 2 MPa CO₂, and 4 h).

Fig.7 (a) TG curve of the reused P-ZnO and R-ZnO catalysts at 400 °C, (b) total spin number associated with oxygen vacancies and zinc vacancies of the reused P-ZnO and R-ZnO, and (c, d) total spin number associated with vacancies of the reused P-ZnO and R-ZnO.

Fig.8 (a) Effect of reaction pressure at 130 °C, 4 h reaction time, 76.5 mmol ECH, 0.1 g P-ZnO, and 50 μL DMF. (b) Effect of reaction time at 130 °C, 1.5 MPa, 76.5 mmol ECH, 0.1 g P-ZnO, and 50 μL DMF. (c) Effect of DMF dosage at 130 °C, 1.5 MPa, 4 h reaction time, 76.5 mmol ECH, and 0.1 g P-ZnO.

Tab.2 Cycloaddition of CO₂ to various epoxides over the P-ZnO catalyst (reaction conditions: 0.1 g P-ZnO, 70 μL DMF, 76.5 mmol epoxides, 130 °C, 1.5 MPa, and 4 h)

Fig.9 (a) Adsorption energy of CO₂ on oxygen vacancies at the ZnO (002) and ZnO (100) surfaces. (b) Adsorption energy of ECH on oxygen vacancies at the ZnO (002) and ZnO (100) surfaces. (c) Plausible reaction mechanism of the synthesis of CPC from CO₂ and ECH over P-ZnO. (d) Plausible reaction mechanism of the synthesis of CPC from CO₂ and ECH over P-ZnO and DMF.

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