Constructing mesoporous CeO2 single-crystal particles in ionic liquids for enhancing the conversion of CO2 and alcohols to carbonates

doi:10.1016/S1872-2067(24)60117-8

Abstract

Abstract:

Catalysts for CO₂ value-added conversion have been extensively explored, but there is still a lack of systematic design for catalysts that achieve efficient CO₂ conversion under mild conditions. Herein, we explored a mesoporous CeO₂ single-crystal formed with the regulation of ionic liquids, which catalyzed the effective carbonylation reaction with CO₂ under mild reaction conditions. By altering the synthetic environment, a series of uniform mesoporous CeO₂ particles with atomically aligned single-crystal frameworks were constructed, which have different surface physicochemical properties and primary aggregation degree. The prepared mesoporous CeO₂ single-crystal achieved efficient activation of CO₂ and alcohols at 0.5 MPa CO₂ and 100 °C, and the CeO₂-IL-M catalyst shows optimal catalytic performance in the synthesis of ethylene carbonate with 46.22 mmol g^-1 h^-1, which was 50.6 times as high as that of the CeO₂ obtained without ionic liquids. Subsequently, the catalytic pathway and mechanism of carbonylation reaction with CO₂ on mesoporous CeO₂ single-crystal were studied via React-IR spectra and C¹⁸O₂ labeling experiments. The research provides a new strategy for controllable nanoscale assembly of mesoporous single-crystal materials and expands the application range of single-crystal materials, aiming to develop novel catalytic materials to meet industrial needs.

Key words: Cerium dioxide, Ionic liquid, Single-crystal material, Surface oxygen vacancy, Carbonylation reaction

Jielin Huang, Jie Wang, Haonan Duan, Songsong Chen, Junping Zhang, Li Dong, Xiangping Zhang. Constructing mesoporous CeO₂ single-crystal particles in ionic liquids for enhancing the conversion of CO₂ and alcohols to carbonates[J]. Chinese Journal of Catalysis, 2024, 66: 152-167.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60117-8

https://www.cjcatal.com/EN/Y2024/V66/I11/152

Figures/Tables 17

Fig. 1. XRD patterns of CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples (a), CeO2 catalysts constructed in different ILs and Comm-CeO2 catalyst (b). (c) FT-IR spectra of all the catalysts. (d) TG curve of CeO2-IL-M sample.

Fig. 2. TEM images of CeO2-M mesocrystals, the growth mode (a), the morphology (b), and the SAED (c) images of CeO2-M.

Fig. 3. TEM images of CeO2-IL-M (a-c), CeO2-IL-W (d-f), and CeO2-IL-M-All (g-i) mesoporous single-crystal. HAADF-STEM image (j) and corresponding elemental mappings images (k,l) of Ce (k) and O (l) of mesoporous CeO2-IL-M single-crystal.

Fig. 4. TEM images of mesoporous CeO2-IL2-M single-crystal (a,b) and mesoporous CeO2-IL3-M single-crystal (c,d).

Scheme 1. The brief preparation process of catalysts, wherein the catalyst obtained from Ce(NO3)3·6H2O in TEAOH/methanol/H2O system was recorded as CeO2-IL-M. Besides, CeO2-M (methanol/H2O system), CeO2-IL-W (TEAOH/H2O/H2O system), and CeO2-IL-M-All (TEAOH/methanol/methanol system) was prepared for comparison in this work.

Fig. 5. TEM images of CeO2-IL-M-Ace catalyst prepared with (CH3CO2)3Ce·xH2O (a-c), CeO2-IL-M-Chl catalyst prepared with CeCl3·6H2O (d-f), and CeO2-IL-M-Amm catalyst prepared with H8CeN8O18 (g-i).

Fig. 6. N2 adsorption-desorption isotherms (a) and BJH pore size distribution curves (b) of CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples.

Table 1 Physical and chemical properties of the samples.

Sample	Surface area ^a (m² g^-1)	Pore diameter ^b (nm)	Pore volume ^c (cm³ g^-1)
CeO₂-M	29.343	3.394	0.019
CeO₂-IL-M	57.000	3.063	0.117
CeO₂-IL-W	57.340	3.073	0.081
CeO₂-IL-M-All	80.952	3.064	0.116

Fig. 7. XPS spectra of CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples. (a) Survey; (b) Ce 3d; (c) O 1s; (d) C 1s.

Fig. 8. Raman spectra (a) and EPR spectra (b) of the CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples.

Fig. 9. (a) CO2-TPD profiles of the CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples. (b) Partially enlarged profiles of 50-200 °C in (a). (c) CO2-TPD profiles of the CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples. (d) The integral area of the zone in the temperature range of 50-150 °C in (a) and 50-200 °C in (c).

Fig. 10. (a,b) The catalytic activities of commercial CeO2 and CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All samples for the reaction of CO2 and EG to produce EC. (c) The catalytic activities of CeO2-ILx-M samples prepared with different ILs. (d) The cycling performance of catalyst CeO2-IL-M.

Fig. 11. The different influences of experiment parameters the reaction temperature (a), the pressure of CO2 (b), reaction time (c), and catalyst usage (d) of CeO2-IL-M mesocrystalline nanoparticles.

Fig. 12. React-IR spectra during the catalytic production of EC from CO2 and EG by the CeO2-M (a), CeO2-IL-M (b), CeO2-IL-W (c), and CeO2-IL-M-All (d) catalysts.

Fig. 13. The rate of group change over time, k = ΔIntensity/Δt (a.u./min), monitored via React-IR spectra during the catalytic production of EC from CO2 and EG by the CeO2-M, CeO2-IL-M, CeO2-IL-W, and CeO2-IL-M-All catalysts. (a) Changes of groups over time in catalytic processes of CeO2-IL-M; (b) the k of O=C-NH2 group; (c) the k of O=C group; (d) the k of O=C-R group.

Fig. 14. Isotope labelling experiments and analysis of GC-MS test results (a and b), and formation pathways of EC and?2-picolinamide on the CeO2-IL-M catalysts (c).

Scheme 2. The main reaction route of the carbonylation of EG and CO2 over the mesoporous CeO2 single-crystal catalysts.

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Constructing mesoporous CeO₂ single-crystal particles in ionic liquids for enhancing the conversion of CO₂ and alcohols to carbonates

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