Surface silane functionalized Fe₂O₃ nanoparticles for dual pickering emulsion stabilization and fenton Type catalytic oxidation


Authors

DOI:

https://doi.org/10.22517/23447214.26487

Keywords:

Fe₂O₃ nanoparticles, Catalytic oxidation, Surface functionalization, Pickering emulsions, Silane coupling agents, Catalytic oxidation; Fe₂O₃ nanoparticles; Pickering emulsions; Silane coupling agents; Surface functionalization.

Abstract

Enhanced thermal recovery of heavy crude oils requires multifunctional nanomaterials capable of stabilizing interfaces and catalyzing oxidation reactions under reservoir conditions. Fe2O3 nanoparticles (Fe2O3-NPs) are promising candidates due to their redox activity and potential as Pickering emulsion stabilizers, although their dual performance depends on precise control of surface chemistry. The objective was to design and characterize dual-function Fe2O3-NPs, active as Pickering emulsion stabilizers and Fenton-type catalysts, through controlled surface functionalization with silane coupling agents (SiCAs). Fe2O3-NPs were functionalized with propyltrimethoxysilane (C3), octyltriethoxysilane (C8), and hexadecyltrimethoxysilane (C16) via hydrolysis of alkoxy groups and condensation with surface –OH groups, characterizing BET surface area, particle size (DLS), contact angle, and surface chemistry (XPS, FTIR-ATR); the nanoparticles were used to formulate polar and nonpolar nanofluids, evaluating their interfacial activity in water/hydrocarbon Pickering emulsions at different particle loadings. Functionalization modulated interfacial activity, with contact angles ranging from 20° to 167°, without significant loss of active surface area or multilayer formation; emulsion stability and type (O/W or W/O) correlated with the particles' hydrophilic–hydrophobic balance. Fe2O3 active sites were preserved after functionalization, enabling dual performance as an interfacial stabilizer and heterogeneous oxidation catalyst, with potential application in in-situ combustion processes for thermal recovery. This work was funded by Colciencias-ANH, project "Preparation of transition metal-based nanomaterials for processes related to thermal recovery of Colombian crude oils and analysis of their catalytic behavior in in-situ combustion processes."

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Author Biographies

Wilson German Oyola Naranjo, Industrial University of Santander

Wilson G. Oyola was born in Oiba, Santander, Colombia in 1977. He received the B.S. and M.S. degrees in Chemistry from the Industrial of Santander University, in 2006 and 2015. From 2008 to 2016, he was a Research Professional with the T.I.P Ltda. From 2017 to 2019, he was a Professor with the Basic Science Department, Santo Tomás University. He is the author of three inventions registered to Ecopetrol. His research interests include spectroscopic analytical, in Oil&Gas Upgrading of heavy crudes, synthesis of additives, heterogeneous catalysis, gold and silver purity processes, and chemical recycling of polymers in pyrolysis process in the ICPET Instituto Colombiano del Petróleo y Energías de la Transición

Victor Gabriel Baldovino Medrano, Industrial University of Santander

Víctor Gabriel Baldovino Medrano Associate Professor at the School of Chemical Engineering at Universidad Industrial de Santander, Colombia. He completed undergraduate studies in Engineering (1998 – 2003) and a PhD in Chemical Engineering (2004 – 2009) at t Universidad Industrial de Santander. Subsequently, he was a postdoctoral researcher (2009 – 2014) at the Université catholique de Louvain (UC Louvain) in Belgium. He has taught courses on Applied Statistics and Design of Experiments, Transport Phenomena, Catalysis, and Surface Science. His research focuses on the synthesis and properties of materials and catalytic processes involving solids at various scales, with a particular emphasis on applications in hydrogenation and oxidation. His publication record is available on Google Scholar. He is the author of three patents and has published book chapters on Janus nanoparticles for catalytic applications and on the analysis of metal oxides using X-ray photoelectron emission spectroscopy. Recently, he published a book on Design of Experiments, featuring illustrative examples in catalysis. He has also served as a guest editor for journals such as Catalysis Today and ChemCatChem, and was the editor-in-chief of Revista ION. Currently, he is a member of the editorial committees of Molecular Catalysis and ChemCatChem. He has held leadership positions as Director of the Centro de Investigaciones en Catálisis (CICAT-UIS) and Scientific Coordinator of the Laboratorio Central de Ciencia de Superficies (SurfLab-UIS). Additionally, he served as President of the Colombian Society of Catalysis (2019–2023) and has been a member of the Ibero-American Federation of Catalysis Societies (FiSoCat) since 2019. He currently represents FiSoCat before the International Association of Catalysis Societies (IACS). 

Fernando Martínez Ortega, Industrial University of Santander

Fernando Martínez Ortega received the B.S. degree in chemistry and the M.S. degree in chemistry from the Universidad Industrial de Santander, Bucaramanga, Colombia, in 1989 and 1992, respectively, and the Ph.D. degree in chemistry from the Université de Poitiers, Poitiers, France, in 2000. He completed postdoctoral research in chemistry at the Université de Poitiers from 2010 to 2011. Since 1990, he has been with the School of Chemistry, Universidad Industrial de Santander, Bucaramanga, where he is currently a Full Professor. He is a member of the Catalysis Research Center (CICAT). His research interests include environmental catalysis, photocatalysis, selective oxidation by oxygen-atom transfer, catalyst heterogenization, oleochemistry, and the synthesis of metal nanoparticles. 

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V. G. Baldovino-Medrano, V. Niño-Celis, and R. Isaacs Giraldo, “Systematic Analysis of the Nitrogen Adsorption–Desorption Isotherms Recorded for a Series of Materials Based on Microporous–Mesoporous Amorphous Aluminosilicates Using Classical Methods,” J. Chem. Eng. Data, vol. 68, no. 9, pp. 2512–2528, Sep. 2023, https://doi.org/10.1021/ACS.JCED.3C00257.

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J. Rodríguez-Pereira, R. Valderrama-Zapata, L. J. Hoyos-Marín, and V. G. Baldovino-Medrano, “Surface Composition–Performance Relationships in Pt-Re/γ-Al₂O₃ for Catalytic Alkane Reforming and Aromatization,” ChemCatChem, vol. 18, no. 1, p. e00569, Jan. 2026, https://doi.org/10.1002/CCTC.202500569

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[13] S. Batool and Z. Hussain, “Diospyros lotus-mediated synthesis of iron oxide nanoparticles and their application as a catalyst in fenton reaction,” Curr. Nanosci., vol. 16, no. 1, pp. 91 – 100, 2020, https://doi.org/10.2174/1573413715666191023103729

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[15] C. Sanchez, B. Julián, P. Belleville, and M. Popall, “Applications of hybrid organic–inorganic nanocomposites,” J. Mater. Chem., vol. 15, no. 35–36, pp. 3559–3592, 2005, https://doi.org/10.1039/B509097K.

[16] X. Huang et al., “Magnetic nanoparticles with functional silanes: Evolution of well-defined shells from anhydride containing silane,” J. Mater. Chem., vol. 19, no. 24, pp. 4231–4239, 2009, https://doi.org/10.1039/b821917f.

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[18] X. Song and J.-F. Boily, “Water vapor interactions with FeOOH particle surfaces,” Chem. Phys. Lett., vol. 560, pp. 1–9, 2013, https://doi.org/10.1016/j.cplett.2012.12.048.

[19] B. P. Binks and S. O. Lumsdon, “Influence of Particle Wettability on the Type and Stability of Surfactant-Free Emulsions†,” Langmuir, vol. 16, no. 23, pp. 8622–8631, Nov. 2000, https://doi.org/10.1021/LA000189S.

[20] B. P. Binks and A. T. Tyowua, “Oil-in-oil emulsions stabilised solely by solid particles,” Soft Matter, vol. 12, no. 3, pp. 876–887, 2016, https://doi.org/10.1039/C5SM02438B.

[21] B. P. Binks, “Colloidal Particles at a Range of Fluid–Fluid Interfaces,” Langmuir, vol. 33, no. 28, pp. 6947–6963, Jul. 2017, https://doi.org/10.1021/ACS.LANGMUIR.7B00860.

K. Wang, J. Davies-Jones, A. Graf, M. Carravetta, P. R. Davies, and M. Pera-Titus, “Amphiphilic Janus Particles for Aerobic Alcohol Oxidation in Oil Foams,” ACS Catal., vol. 14, no. 15, pp. 11545–11553, Aug. 2024, https://doi.org/10.1021/acscatal.4c00909.

S. Zhang, D. Dedovets, A. Feng, K. Wang, and M. Pera-Titus, “Pickering Interfacial Catalysis for Aerobic Alcohol Oxidation in Oil Foams,” J. Am. Chem. Soc., vol. 144, no. 4, pp. 1729–1738, Feb. 2022, https://doi.org/10.1021/JACS.1C11207.

R. Massart, “Preparation of aqueous magnetic liquids in alkaline and acidic media,” IEEE Trans. Magn., vol. 17, no. 2, pp. 1247–1248, 1981, https://doi.org/10.1109/TMAG.1981.1061188.

R. M. Cornell and U. Schwertmann, “The Iron Oxides,” The Iron Oxides, Jul. 2003, https://doi.org/10.1002/3527602097.

V. G. Baldovino-Medrano, V. Niño-Celis, and R. Isaacs Giraldo, “Systematic Analysis of the Nitrogen Adsorption–Desorption Isotherms Recorded for a Series of Materials Based on Microporous–Mesoporous Amorphous Aluminosilicates Using Classical Methods,” J. Chem. Eng. Data, vol. 68, no. 9, pp. 2512–2528, Sep. 2023, https://doi.org/10.1021/ACS.JCED.3C00257.

A. A. Bunaciu, E. G. Udriştioiu, and H. Y. Aboul-Enein, “X-Ray Diffraction: Instrumentation and Applications,” Crit. Rev. Anal. Chem., vol. 45, no. 4, pp. 289–299, 2015, https://doi.org/10.1080/10408347.2014.949616.

M. Thommes et al., “Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report),” Pure and Applied Chemistry, vol. 87, no. 9–10, pp. 1051–1069, Oct. 2015, https://doi.org/10.1515/PAC-2014-1117.

J. Rodríguez-Pereira, R. Valderrama-Zapata, L. J. Hoyos-Marín, and V. G. Baldovino-Medrano, “Surface Composition–Performance Relationships in Pt-Re/γ-Al₂O₃ for Catalytic Alkane Reforming and Aromatization,” ChemCatChem, vol. 18, no. 1, p. e00569, Jan. 2026, https://doi.org/10.1002/CCTC.202500569

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J. J. Pignatello, E. Oliveros, and A. MacKay, “Advanced Oxidation Processes for Organic Contaminant Destruction Based on the Fenton Reaction and Related Chemistry,” Crit. Rev. Environ. Sci. Technol., vol. 36, no. 1, pp. 1–84, Jan. 2006, https://doi.org/10.1080/10643380500326564.

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[33] V. K. LaMer and R. H. Dinegar, “Theory, Production and Mechanism of Formation of Monodispersed Hydrosols,” J. Am. Chem. Soc., vol. 72, no. 11, pp. 4847–4854, Nov. 1950, https://doi.org/10.1021/ja01167a001.

S. Menchaca-Nal, C. L. Londoño-Calderón, D. C. Pardo-Saavedra, L. G. Pampillo, L. M. Socolovsky, and R. Martínez-García, “Estudio del efecto del tamaño en la estructura cristalina de nanopartículas de CoFe2O4 study of the effect of the size in the crystalline structure of CoFe2O4 nanoparticles”. An. AFA, vol. 25, no. 1, Aug. 2014, https://doi.org/10.31527/analesafa.2014.25.1.42.

A. L. Patterson, “The Scherrer Formula for X-Ray Particle Size Determination,” Physical Review, vol. 56, no. 10, p. 978, Nov. 1939, https://doi.org/10.1103/PhysRev.56.978.

B. D. Cullity and S. R. Stock, “Elements of x-ray diffraction,” p. 664, 2001.

S. A. Hassanzadeh-Tabrizi, “Precise calculation of crystallite size of nanomaterials: A review,” J. Alloys Compd., vol. 968, p. 171914, Dec. 2023, https://doi.org/10.1016/J.JALLCOM.2023.171914.

S. Nasiri et al., “Modified Scherrer equation to calculate crystal size by XRD with high accuracy, examples Fe2O3, TiO2 and V2O5,” Nano Trends, vol. 3, Sep. 2023, https://doi.org/10.1016/j.nwnano.2023.100015.

C.-J. Jia et al., “Large-Scale Synthesis of Single-Crystalline Iron Oxide Magnetic Nanorings,” J. Am. Chem. Soc., vol. 130, no. 50, pp. 16968–16977, Dec. 2008, https://doi.org/10.1021/ja805152t.

E. J. W. Verwey, “The Crystal Structure of γ-Fe2O3 and γ-Al2O3,” vol. 91, no. 1–6, pp. 65–69, 1935, https://doi.org/10.1524/zkri.1935.91.1.65.

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2026-09-30

How to Cite

Oyola Naranjo, W. G., Baldovino Medrano, V. G., & Ortega, F. M. . (2026). Surface silane functionalized Fe₂O₃ nanoparticles for dual pickering emulsion stabilization and fenton Type catalytic oxidation . Scientia Et Technica, 31(03), 124–138. https://doi.org/10.22517/23447214.26487

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Vol. 31 No. 03 (2026): Julio-Septiembre 2026

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Ciencias Básicas

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Copyright (c) 2026 Wilson German Oyola Naranjo, Victor Gabriel Baldovino Medrano

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