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. 2025 Jan 10;12(9):2413203. doi: 10.1002/advs.202413203

Catalytic Hydrolysis of Perfluorinated Compounds in a Yolk–Shell Micro‐Reactor

Jialin Zheng 1,2, Xiaojian Wang 1,2, Xin Zi 1, Hang Zhang 1, Heping Chen 3, Evangelina Pensa 4, Kang Liu 1, Junwei Fu 1, Zhang Lin 2, Liyuan Chai 2, Emiliano Cortés 4,✉, Min Liu 1,2,✉
PMCID: PMC11884611  PMID: 39792599

Abstract

Perfluorinated compounds (PFCs) are emerging environmental pollutants characterized by their extreme stability and resistance to degradation. Among them, tetrafluoromethane (CF4) is the simplest and most abundant PFC in the atmosphere. However, the highest C─F bond energy and its highly symmetrical structure make it particularly challenging to decompose. In this work, a yolk–shell Al2O3 micro‐reactor is developed to enhance the catalytic hydrolysis performance of CF4 by creating a local autothermic environment. Finite element simulations predict that the yolk–shell Al2O3 micro‐reactor captures the heat released during the catalytic hydrolysis of CF4, resulting in a local autothermic environment within the yolk–shell structure that is 50 °C higher than the set temperature. The effectiveness of this local autothermic environment is experimentally confirmed by in situ Raman spectroscopy. As a result, the obtained yolk–shell Al2O3 micro‐reactor achieves 100% CF4 conversion at a considerably low temperature of 580 °C for over 150 h, while hollow and solid Al2O3 structures required higher temperatures of 610 and 630 °C, respectively, to achieve the same conversion rate, demonstrating the potential of yolk–shell Al2O3 micro‐reactor to significantly reduce the energy requirements for PFCs degradation and contribute to more sustainable and effective environmental remediation strategies.

Keywords: catalytic hydrolysis, environmental chemistry, perfluorocarbons, thermal effects, yolk–shell

The yolk–shell micro‐reactor captures the heat released during the catalytic hydrolysis of tetrafluoromethane (CF4) to create a local autothermic environment between the yolk and the shell, increasing the local temperature by 50 °C. As a result, the yolk–shell micro‐reactor achieved 100% CF4 degradation at a considerably low temperature of 580 °C for over 150 h.

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1. Introduction

Perfluorinated compounds (PFCs) are among the most persistent environmental pollutants, known for their extreme resistance to decompose, which has garnered global attention.[ 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 ] Tetrafluoromethane (CF4), the simplest PFCs, features highly symmetrical C─F with a bond energy of up to 543 ± 4 kJ mol−1, and an atmospheric lifetime exceeding 50 000 years, making it exceptionally challenging to break down naturally.[ 9 , 10 , 11 , 12 , 13 , 14 ] Therefore, developing an efficient method for CF4 catalytic hydrolysis is highly desirable for a sustainable future.

Thermocatalytic hydrolysis is regarded as one of the most effective techniques for CF4 treatment, but its high‐temperature requirements and significant energy consumption pose substantial challenges for industrial applications.[ 15 , 16 , 17 , 18 , 19 , 20 , 21 , 22 ] To enhance catalytic activity and reduce energy consumption, researchers are actively optimizing the Al2O3 catalyst.[ 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 , 31 ] For example, Zhang et al. reported the preparation of various crystalline phases of Al2O3, in which γ‐Al2O3 could degrade CF4 100% at 650 °C.[ 22 ] EI‐Bahy et al. found that a Ga‐Al catalyst could achieve 100% conversion of CF4 at 630 °C.[ 23 ] Despite these results demonstrating the efficient CF4 conversion, the high temperatures required resulted in significant energy consumption. Recently, Lai et al. discovered that utilizing thermal cycling within a porous media structure can improve the reaction conversion rate and reduce energy consumption.[ 32 ] Consequently, energy consumption during hydrolysis can be minimized by precisely adjusting the catalyst's local autothermic environment to harness the energy released by CF4 conversion, an exothermic reaction that releases a large amount of energy (168 KJ mol−1).[ 33 , 34 , 35 , 36 ]

Herein, we developed a yolk–shell Al2O3 micro‐reactor to create a local autothermic environment, thereby enhancing the catalytic hydrolysis performance of CF4. Finite element simulations using COMSOL demonstrated that the yolk–shell Al2O3 catalyst can effectively utilize the heat released by CF4 catalytic hydrolysis to establish a local autothermic environment, increasing the reaction temperature by 50 °C. In contrast, hollow and solid Al2O3 catalysts could only achieve temperature increases of 15 and 0 °C, respectively, under the same conditions. The successful preparation of yolk–shell, hollow, and solid structured catalysts was confirmed through scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X‐ray powder diffraction (XRD) analyses proved that all catalysts were indeed Al2O3. Furthermore, in situ Raman spectroscopy experimentally confirmed the generation of a local autothermic environment. The catalytic hydrolysis performance tests showed that the yolk–shell Al2O3 micro‐reactor achieved a 100% CF4 conversion rate at 580 °C for over 150 h, whereas hollow and solid Al2O3 catalysts required temperatures of 610 and 630 °C, respectively, to achieve the same conversion rate. This work presents a novel catalyst design that effectively harnesses reaction heat to create a local autothermic environment, offering a new strategy for the low‐temperature, high‐efficiency catalytic hydrolysis of PFCs.

2. Results and Discussion

2.1. Finite Element Simulations

To validate the feasibility of constructing a local autothermic environment utilizing the heat released by CF4 catalytic hydrolysis reaction, we conducted simulations using COMSOL for yolk–shell, hollow, and solid Al2O3 catalysts (Figure 1a).[ 37 , 38 , 39 , 40 ] Spherical models of these catalysts were constructed to simulate the temperature distributions during the catalytic hydrolysis of CF4. Using 580 °C as the baseline catalytic hydrolysis temperature, the simulation revealed that the yolk–shell Al2O3 catalyst exhibited a higher internal temperature of 630 °C within its cavity (Figure 1c–f), while the hollow Al2O3 catalyst only reached an internal temperature of 595 °C (Figure 1d–g). In contrast, the solid Al2O3 shows no significant temperature difference (Figure 1b–e). These indicate that the yolk–shell Al2O3 catalyst can utilize the energy released during CF4 catalytic hydrolysis to create a local autothermic environment, raising the local temperature by 50 °C.

Figure 1.

Figure 1

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Finite element simulations. a) Schematic illustration of the direction of heat generated by catalytic hydrolysis of CF4 in different catalyst structures. COMSOL simulates the temperature distribution for b,e) solid, c,f) yolk–shell, and d,g) hollow Al2O3 catalysts during the catalytic hydrolysis of CF4.

2.2. Synthesis and Characterizations of Catalysts

To validate the simulation prediction, a yolk–shell Al2O3 catalyst was synthesized by a sol‐gel method with aging time adjustment (Figure 2a). X‐ray diffraction (XRD, Figure S1, Supporting Information) confirmed that the obtained yolk–shell, hollow, and solid Al2O3 all correspond to the γ‐Al2O3 phase (PDF#79‐1558). Scanning electron microscopy (SEM) images showed that the prepared catalysts exhibited a sea urchin‐like morphology, with an external surface composed of randomly assembled and interconnected nanosheets (Figure 2b–d and S2, Supporting Information). Transmission electron microscopy (TEM) images further revealed that the yolk–shell, hollow, solid Al2O3 catalysts had diameters in the range of 2–3 µm, with the yolk in the yolk–shell structure measuring ≈ 1.5 µm, consistent with SEM results (Figure 2e–g). Energy‐dispersive spectroscopy (EDS) mapping illustrated uniform distributions of Al and O across the catalyst (Figure S3, Supporting Information). Al 2p X‐ray photoelectron spectroscopy (XPS) spectra demonstrated the chemical valence states of Al in the yolk–shell, hollow, and solid Al2O3 catalysts are consistent (Figure S4, Supporting Information). Brunauer–Emmett–Teller (BET) analyses revealed that the specific surface areas of yolk–shell, hollow, and solid Al2O3 catalysts were 305.3, 331.4, and 283.6 m2 g−¹, respectively (Figure S5 and Table S1, Supporting Information), excluding the effect of specific surface area. These results confirmed the successful preparation of yolk–shell, hollow, and solid Al2O3 catalysts with identical physical and chemical properties.

Figure 2.

Figure 2

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Characterization of yolk–shell, hollow, and solid catalysts. a) Schematic illustration of the preparation process for three catalysts. b–d) SEM images of yolk–shell, hollow, and solid Al2O3 catalysts respectively. e–g) TEM images of yolk–shell, hollow, and solid Al2O3 catalysts respectively.

2.3. Local Thermal Field Effect

To experimentally validate the creation of a local thermal environment, we employed in situ Raman spectroscopy to monitor temperature changes of the catalyst during CF4 catalytic hydrolysis (Figure 3a; Figure S6, Supporting Information).[ 41 ] During the CF₄ catalytic hydrolysis reaction, the tensile vibration of the Al─O bond is affected by temperature changes, resulting in a shift of the Raman peak toward lower wavenumbers (Figure 3b). The results showed that the Raman peak of the yolk–shell Al2O3 catalyst shifted from 405.7 to 401.4 cm−¹, corresponding to an offset of 4.3 cm−¹. In comparison, the offsets for the hollow and solid Al2O3 catalysts were only 2.1 and 1.4 cm−¹, respectively (Figure 3d–f; Figure S7, Supporting Information).

Figure 3.

Figure 3

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Local thermal field effect. a,b) Schematic diagram of Raman test mechanism. c) The difference between the actual temperature and the setting temperature of yolk–shell, hollow, and solid Al2O3 catalysts is calculated by fitting. d–f) Shift of Raman peak with increasing temperature during a reaction of yolk–shell, hollow, and solid Al2O3 catalysts.

Based on the linear relationship between Raman frequency shift and temperature,[ 42 ] the actual temperatures could be calculated, allowing us to determine the difference (Δ°C) between the set and actual temperatures (Figure 3c). As shown in the figure, when the external temperature was set to 580 °C, the actual temperature in the yolk–shell catalyst reached 627 °C, resulting in a Δ°C of 47 °C. In contrast, the hollow and solid catalysts exhibited Δ°Cs of 24 and 12 °C, respectively. These Δ°Cs demonstrated that the yolk–shell catalyst has a superior capacity to accumulate and retain heat compared to the hollow and solid structures, thereby creating a localized thermal field during the catalytic process.

2.4. CF4 Catalytic Hydrolysis Performance

To demonstrate the effectiveness of the local autothermal environment, we evaluated the CF4 hydrolysis activities of yolk–shell, hollow, and solid Al2O3 catalysts over a temperature range of 500 –580 °C (Figure 4a; Figure S8, Supporting Information). Through this temperature range, the yolk–shell Al2O3 catalyst consistently exhibited higher CF4 conversion rates than those for the hollow and solid Al2O3 catalysts, further confirming the effectiveness of the local autothermal environment. As a result, the yolk–shell Al2O3 catalyst achieved 100% CF4 conversion at 580 °C, while temperatures of 610 and 630 °C are required to achieve the same conversion rates over hollow and solid Al2O3 catalysts, respectively (Figure 4b). This significant reduction in required temperature underscores the effectiveness of the yolk–shell structure in enhancing catalytic performance.

Figure 4.

Figure 4

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Catalytic stability and performance characterizations. a) CF4 conversion (%) during CF4 catalytic hydrolysis reaction at different reaction temperatures for yolk–shell, hollow, and solid Al2O3 catalysts. b) Temperature at 100% catalytic hydrolysis of the three samples and TOF calculation for catalytic conversion of CF4. c) Arrhenius plots obtained for the CF4 conversion rates at 500–580 °C for the three catalysts. d) The stability test of yolk–shell, hollow, and solid Al2O3 catalysts at 580 °C. (Reaction condition: 2500 ppm of CF4 and 10% of H2O, balanced with Ar, total flow rate of 33.3 mL min−1, and weight hourly space velocity (WHSV) of 1000 mL g −1 h−1).

To rule out potential influences from the number and properties of acidic sites or CF4 adsorption capabilities, temperature‐programmed desorption of NH3 (NH3‐TPD), pyridine‐infrared (py‐IR), and CF4‐TPD was conducted. The NH3‐TPD and Py‐IR analyses indicated that only L‐acid sites on the catalyst surfaces (Figures S9 and S10, Supporting Information). CF4‐TPD results showed that the CF4 adsorption capacity of hollow Al2O3 was higher than those of yolk–shell and solid Al2O3 (Figure S11, Supporting Information), indicating that the enhancement of CF4 conversion over yolk–shell Al2O3 was not caused by its adsorption capacity but its local autothermic nature.

To investigate the intrinsic activity of the catalysts, the turnover frequency (TOF) of the catalysts was calculated at 500 °C based on surface acidity test results. The yolk–shell Al2O3 catalyst exhibited a TOF of 4.4 × 10− 3 s−¹, which was 1.5 and 2.7 times higher than those of hollow and solid Al2O3 catalyst, respectively (Figures S12 and Table S2, Supporting Information). The calculated apparent activation energies for the yolk–shell, hollow, and solid Al2O3 catalysts are 84.2, 97.0, 111.9 kJ mol−¹, respectively (Figure 4c; Figures S8 and S13, Supporting Information), further proving the enhanced catalytic activity by the local autothermic environment created in the yolk–shell structure.

Next, the stability of the catalysts was assessed at 580 °C. The results showed that the yolk–shell Al2O3 catalyst maintained a 100% CF4 conversion for over 150 h (Figure 4d; Figure S14, Supporting Information), significantly outperforming 75% CF4 conversion for 80 h and 60% CF4 conversion for 75 h over hollow and solid Al2O3 respectively. These results demonstrate that the yolk–shell Al2O3 catalyst offers both superior catalytic activity and stability, and has certain advantages compared with the reported catalyst (Table S3, Supporting Information).

In order to understand the different stability of the catalysts, we performed XRD and SEM characterizations of the catalysts after a long reaction time. The XRD results show that all the catalysts change from the γ‐Al2O3 phase to the inactive α‐Al2O3 phase, accounting for the decrease in catalyst stability (Figure S15, Supporting Information). In addition, during CF4 catalytic hydrolysis, fluorine is adsorbed on the Al active sites, resulting in catalyst fluorine poisoning and reduced stability. The higher temperature is conducive to breaking the Al─F bonds, realizing the regeneration of the Al active sites, and improving the stability of the catalyst. Finite element simulations and in situ Raman spectroscopy indicate that the yolk–shell Al2O3 catalyst creates the local autothermic environment, which makes the cavity temperature higher than that of hollow and solid Al2O3 catalysts, and is conducive to the regeneration of the Al active sites (Figure S16a, Supporting Information). Although the hollow Al2O3 catalyst also has a local autothermic environment (weaker than the yolk–shell Al2O3), the hollow Al2O3 catalyst is more prone to collapse, hindering the regeneration of the Al active sites, so the activity of the hollow Al2O3 catalyst begins to decline at 80 h (Figure S16b, Supporting Information). The solid structure lacks a local autothermic environment, so the stability decreases due to the fluorine poisoning of the Al active sites after a 75 h reaction (Figure S16c, Supporting Information).

3. Conclusion

In summary, we developed a yolk–shell Al2O3 micro‐reactor catalyst that leverages the cavity between the yolk and shell to trap the heat released during the reaction, creating a localized autothermic environment that enhances CF4 catalytic hydrolysis. COMSOL simulations demonstrated that the yolk–shell Al2O3 catalyst effectively utilizes the heat from CF4 catalytic hydrolysis to establish a local autothermic environment, raising the reaction temperature by 50 °C. In contrast, hollow and solid Al2O3 catalysts exhibited much smaller temperature increases of 15 and 0 °C, respectively, under the same conditions. In situ Raman spectroscopy confirmed the creation of this localized autothermic environment. Performance tests revealed that the yolk–shell Al2O3 catalyst achieved 100% CF4 conversion at 580 °C and maintained this activity for over 150 h. This work introduces a novel approach for designing low‐temperature, high‐activity catalysts for the catalytic hydrolysis of PFCs.

Conflict of Interest

The authors declare no conflict of interest.

Supporting information

Supporting Information

ADVS-12-2413203-s001.docx (9.7MB, docx)

Acknowledgements

J. Z. and X. W. contributed equally to this work. The authors thank the Foundation for Innovative Research Groups of the National Natural Science Foundation of China (Grant No. 52121004), the National Natural Science Foundation of China (Grant No. 22376222, 22002189, 52202125, and 52372253), the Science and Technology Innovation Program of Hunan Province (Grant No. 2023RC1012), the Central South University Research Programme of Advanced Interdisciplinary Studies (Grant No. 2023QYJC012), the Central South University Innovation‐Driven Research Programme (Grant No. 2023CXQD042), the Natural Science Foundation of Hunan Province for Excellent Youth Scholars (Grant No. 2024JJ4051) and the Natural Science Foundation of Hunan Province (Grant No. 2024JJ6484). The authors also acknowledge funding and support from the Deutsche Forschungsgemeinschaft (DFG) under Germany´s Excellence Strategy – EXC 2089/1 – 390776260, the Bavarian program Solar Technologies Go Hybrid (SolTech), the Center for NanoScience (CeNS) and the German Federal Ministry of Education and Research (BMBF) under the project NANOBAT. The authors are grateful for the technical support from the High Performance Computing Center of Central South University.

Zheng J., Wang X., Zi X., Zhang H., Chen H., Pensa E., Liu K., Fu J., Lin Z., Chai L., Cortés E., Liu M., Catalytic Hydrolysis of Perfluorinated Compounds in a Yolk–Shell Micro‐Reactor. Adv. Sci. 2025, 12, 2413203. 10.1002/advs.202413203

Contributor Information

Emiliano Cortés, Email: emiliano.cortes@lmu.de.

Min Liu, Email: minliu@csu.edu.cn.

Data Availability Statement

The data that support the findings of this study are available from the corresponding author upon reasonable request.

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Supporting Information

ADVS-12-2413203-s001.docx (9.7MB, docx)

Data Availability Statement

The data that support the findings of this study are available from the corresponding author upon reasonable request.

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