Microwave Synthesis of Transition Metal (Fe, Co, Ni)-Supported Catalysts for CO2 Hydrogenation
Abstract
1. Introduction
2. Results and Discussion
2.1. Physicochemical Properties of the Catalysts
2.2. Catalytic Activity
3. Materials and Methods
3.1. Catalyst Preparation
- (i)
- DPU method: The reactor for sample synthesis was a 250 mL round-bottomed flask placed in a water bath with a thermocouple between the walls of the bath and the reactor. A magnetic stirrer was placed into the reactor for the uniform stirring of the suspension, and simultaneously an aqueous solution of metal nitrate precursor at the required concentration (1 M) and the required volume of distilled water were introduced. Then we introduced a calcined SiO2 carrier and stirred the suspension for 15 min. After that, a weight of urea was added to the obtained suspension, and the suspension was heated to 92 °C, then thermostated under constant stirring for 9 h. Then the suspension was cooled, the precipitate was separated from the mother liquor by centrifugation, and the sample was dried under a vacuum on a rotary evaporator at 40 °C for 2 h. The dry sample was additionally calcined in an air atmosphere at 300 °C for 3 h. The catalysts were denoted as 5Fe/SiO2-DP, 5Co/SiO2-DP, and 5Ni/SiO2-DP, respectively [29,31].
- (ii)
- MW method: For microwave synthesis, the Multiwave Pro (Anton Paar GmbH, Graz, Austria) microwave oven equipped with four autoclave-type beakers was used in the preparation of catalysts. A magnetic stirrer was placed in each beaker, then the SiO2 carrier was added, and an equal amount of the prepared solution was introduced, as in the DPU method (i). Next, the beakers were sealed and placed in a microwave reactor. The process of hydrothermal synthesis was carried out under the following conditions: temperature—92 °C (measured in each beaker by an IR sensor), pressure—9 bar, time of synthesis—5 h, and microwave radiation power—100 W. Upon completion of the process, the resulting suspension was washed three times with distilled water, centrifuged and dried under a vacuum for 3 h. Dry samples were additionally calcined in an air atmosphere at a temperature of 300 °C for 3 h. The catalysts were denoted as 5Fe/SiO2-MW, 5Co/SiO2-MW, and 5Ni/SiO2-MW, respectively [31].
- (iii)
- IP method: For comparison, samples were synthesized by the carrier impregnation method. The pre-vacuumed SiO2 carrier (2 g) was impregnated for 2 h with aqueous solutions of nitrates of the corresponding salts (Fe(NO3)3, Co(NO3)2, and Ni(NO3)2), with periodic shaking for uniform distribution, then the samples were dried in an oven at 110 °C and calcined at 300 °C in air for 3 h. The calcined catalysts obtained by the IP method were designated 5Fe/SiO2-IP, 5Co/SiO2-IP, and 5Ni/SiO2-IP, respectively.
3.2. Catalyst Characterization
3.3. Catalyst Activity Test
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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| Sample | XRD | SBET, m2/g | Vtot, cm3/g | Vmeso, cm3/g | Dpor, Micro/Meso, nm |
|---|---|---|---|---|---|
| 5Ni/SiO2-IP | NiO | 218 | 0.80 | 0.72 | 1–2/5–35 |
| 5Ni/SiO2-DP | Ni3Si4O10(OH)2 | 281 | 0.72 | 0.65 | 1–2/3–30 |
| 5Ni/SiO2-MW | Ni3Si4O10(OH)2 | 256 | 0.85 | 0.85 | 1–2/3–30 |
| 5Fe/SiO2-IP | Fe2O3 | 234 | 0.93 | 0.92 | 1–2/5–35 |
| 5Fe/SiO2-DP | - | 243 | 0.94 | 0.93 | 1–2/5–40 |
| 5Fe/SiO2-MW | - | 237 | 0.93 | 0.92 | 1–2/5–40 |
| 5Co/SiO2-IP | Co3O4 | 237 | 0.93 | 0.92 | 1–2/5–40 |
| 5Co/SiO2-DP | - | 246 | 0.93 | 0.92 | 1–2/5–40 |
| 5Co/SiO2-MW | - | 244 | 0.93 | 0.92 | 1–2/5–40 |
| SiO2 | - | 244 | 0.78 | 0.77 | 1–2/6–18 |
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Strekalova, A.A.; Shesterkina, A.A.; Beresnev, K.A.; Pribytkov, P.V.; Kapustin, G.I.; Mishin, I.V.; Kustov, L.M.; Kustov, A.L. Microwave Synthesis of Transition Metal (Fe, Co, Ni)-Supported Catalysts for CO2 Hydrogenation. Catalysts 2026, 16, 111. https://doi.org/10.3390/catal16010111
Strekalova AA, Shesterkina AA, Beresnev KA, Pribytkov PV, Kapustin GI, Mishin IV, Kustov LM, Kustov AL. Microwave Synthesis of Transition Metal (Fe, Co, Ni)-Supported Catalysts for CO2 Hydrogenation. Catalysts. 2026; 16(1):111. https://doi.org/10.3390/catal16010111
Chicago/Turabian StyleStrekalova, Anna A., Anastasiya A. Shesterkina, Kirill A. Beresnev, Petr V. Pribytkov, Gennadiy I. Kapustin, Igor V. Mishin, Leonid M. Kustov, and Alexander L. Kustov. 2026. "Microwave Synthesis of Transition Metal (Fe, Co, Ni)-Supported Catalysts for CO2 Hydrogenation" Catalysts 16, no. 1: 111. https://doi.org/10.3390/catal16010111
APA StyleStrekalova, A. A., Shesterkina, A. A., Beresnev, K. A., Pribytkov, P. V., Kapustin, G. I., Mishin, I. V., Kustov, L. M., & Kustov, A. L. (2026). Microwave Synthesis of Transition Metal (Fe, Co, Ni)-Supported Catalysts for CO2 Hydrogenation. Catalysts, 16(1), 111. https://doi.org/10.3390/catal16010111

