Mechanism study on the influence of surface properties on the synthesis of dimethyl carbonate from CO2 and methanol over ceria catalysts

doi:10.1016/S1872-2067(24)60091-4

Abstract

Abstract:

The direct synthesis of dimethyl carbonate (DMC) from CO₂ and methanol has attracted much attention as an environmentally benign and alternative route for conventional routes. Herein, a series of cerium oxide catalysts with various textural features and surface properties were prepared by the one-pot synthesis method for the direct DMC synthesis from CO₂ and methanol, and the structure-performance relationship was investigated in detail. Characterization results revealed that both of surface acid-base properties and the oxygen vacancies contents decreased with the rising crystallinity at increasingly higher calcination temperature accompanied by an unexpectedly volcano-shaped trend of DMC yield observed on the catalysts. In situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) studies indicated that the adsorption rate of methanol is slower than that of CO₂ and the methanol activation state largely influences the formation of key intermediate. Although the enhanced surface acidity-basicity and oxygen vacancies brought by low-temperature calcination could facilitate the activation of CO₂, the presence of excess strongly basic sites on low-crystallinity sample was detrimental to DMC synthesis due to the preferred formation of unreactive mono/polydentate carbonates as well as the further impediment of methanol activation. Moreover, with the use of 2-cyanopyridine as a dehydration reagent, the DMC synthesis was found to be both influenced by the promotion from the rapid in situ removal of water and the inhibition from the competitive adsorption of hydration products on the same active sites.

Key words: CeO₂, Dimethyl carbonate, Surface property, Methanol activation, 2-Cyanopyridine

Lei Dong, Shengjie Zhu, Yangyang Yuan, Xiaomin Zhang, Xiaowei Zhao, Yanping Chen, Lei Xu. Mechanism study on the influence of surface properties on the synthesis of dimethyl carbonate from CO₂ and methanol over ceria catalysts[J]. Chinese Journal of Catalysis, 2024, 65: 138-152.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60091-4

https://www.cjcatal.com/EN/Y2024/V65/I10/138

Figures/Tables 14

Fig. 1. XRD patterns of CeO2-T catalysts synthesized at various calcination temperatures.

Table 1 Textural properties and surface concentrations of Ce3+ and oxygen vacancies of CeO2-T samples.

Catalyst	BET surface area ^a(m² g^-1)	Pore volume ^b(cm³ g^-1)	Crystal size ^c(nm)	Surface content of Ce^{3+ d}(%)	Surface content of O_V^e(%)
CeO₂-400	90	0.24	10.0	29.6	18.5
CeO₂-500	83	0.23	11.0	28.5	17.9
CeO₂-600	60	0.18	13.9	27.8	17.2
CeO₂-700	30	0.10	22.6	25.9	16.5
CeO₂-800	5	0.03	46.8	24.9	15.4

Fig. 2. SEM and TEM images of CeO2-400 (a,b), CeO2-500 (c,d), CeO2-600 (e,f), CeO2-700 (g,h) and CeO2-800 (i,j).

Fig. 3. Raman spectra of CeO2-T catalysts.

Fig. 4. XPS spectra of Ce 3d (a) and O 1s (b) of CeO2-T catalysts.

Fig. 5. (a) NH3- and (b) CO2-TPD profiles of CeO2-T catalysts.

Table 2 Basicity and acidity of CeO2-T catalysts determined from NH3- and CO2-TPD profiles.

Catalyst	NH₃ adsorption (μmol g^-1)				CO₂ adsorption (μmol g^-1)
	Weak	Moderate	Strong	Total	Weak	Moderate	Strong	Total
	(< 200 °C)	(200-400 °C)	(> 400 °C)	Total	(< 200 °C)	(200-400 °C)	(> 400 °C)	Total
CeO₂-400	30.1	194.9	252.6	477.6	222.7	49.2	89.9	361.8
CeO₂-500	20.7	108.9	200.9	330.5	192.3	50.6	61.6	304.5
CeO₂-600	18.6	102.6	104.1	225.3	183.9	31.4	55.2	270.5
CeO₂-700	16.6	40.7	76.0	133.3	123.6	23.1	16.2	162.9
CeO₂-800	5.7	19.9	4.1	29.7	3.0	13.1	17.2	33.3

Fig. 6. (a) Catalytic performance of CeO2-T catalysts for DMC synthesis in the absence of dehydrating agents. Reaction conditions: 0.1 g catalyst, 15 mL CH3OH, 120 °C, 3.0 MPa (initial pressure), 2 h. (b) Catalytic performance of CeO2-T catalysts for DMC synthesis in the presence of 2-CP. Reaction conditions: 0.1 g catalyst, 15 mL CH3OH, 50 mmol 2-CP, 120 °C, 3.0 MPa (initial pressure), 2 h. (c) Arrhenius plots of direct DMC synthesis in the absence and presence of 2-CP on CeO2-600. (d) Catalytic activity of CeO2-T catalysts for the hydrolysis of 2-CP. Reaction conditions: 0.01 g catalyst, 15 mL CH3OH, 30 mmol 2-CP, 30 mmol H2O, 120 °C, 3.0 MPa (initial pressure), 2 h. It should be noted that the interference of DMC synthesis reaction on the hydration process could be ignored since no trace amount of DMC was detected under above reaction conditions.

Fig. 7. (a) The relationship among the CO2 adsorption amount, surface content of OV and the space-time yield of DMC. (b) The correlation among the space-time yield, total acidity and basicity.

Fig. 8. DRIFTS spectra of CO2 (a) and methanol (b) adsorbed on CeO2-T (T = 400, 500 and 600 °C) catalysts at 120 °C. DRIFTS spectra of CeO2-T (T = 400, 500 and 600 °C) catalysts pre-adsorbed with CO2 followed by introducing methanol (c) and pre-adsorbed with methanol followed by introducing CO2 at 120 °C (d). The spectra (c) and (d) were both difference spectra referenced to the corresponding spectrum collected at 120 °C after pre-adsorption with CO2 or methanol and subsequent Ar purging.

Table 3 The proportion of various carbonates in total surface carbonates species a.

Catalyst	Bicarbonates content (%)	Bridged carbonates content (%)	Bidentate carbonates content (%)	Mono- and polydentate carbonates content (%)
CeO₂-400	31.1	14.6	30.4	23.9
CeO₂-500	31.2	15.0	33.6	20.2
CeO₂-600	26.8	14.6	41.2	17.4

Fig. 9. (a) The effect of the addition of 2-PA to ‘CeO2 + 2-CP’ reaction system on DMC synthesis. (b) The relationship among 2-PA adsorption amount, acidity/basicity ratio and activity dropping degrees. Reaction conditions: 0.1 g (0.58 mmol) catalyst, 15 mL CH3OH, 50 mmol 2-CP, 2.9 mmol 2-PA, 120 °C, 3.0 MPa (initial pressure), 2 h.

Fig. 10. Reusability of CeO2-600 for the direct DMC synthesis from CO2 and methanol with the assistance of 2-CP. Reaction conditions: 0.2 g catalyst, 30 mL methanol, 100 mmol 2-CP, 3.0 MPa (initial pressure), 120 °C, 2 h. The ‘R’ and ‘RC’ within the parenthesis represented the recycled catalyst treated without and with further calcination, respectively.

Scheme 1. Proposed reaction mechanism for the direct DMC synthesis from CO2 and methanol over CeO2-T catalysts.

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Mechanism study on the influence of surface properties on the synthesis of dimethyl carbonate from CO₂ and methanol over ceria catalysts

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