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Article

Synthesis of Alpha Ferrous Oxalate Dihydrate from Ferrotitaniferous Mineral Sands via Hot Pressurized Aqueous Oxalic Acid: Kinetics and Characterization

by
Carla S. Valdivieso-Ramírez
1,
Salomé Galeas
1,2,
Marleny D. A. Saldaña
3,
Patricia I. Pontón
1,
Víctor H. Guerrero
1,*,
Karla Vizuete
4,
Alexis Debut
4 and
Bojan A. Marinkovic
5,*
1
Department of Materials, Escuela Politécnica Nacional, Quito 170525, Ecuador
2
Doctoral School Energy and Environment, University of Perpignan Via Domitia (UPVD), 52 Avenue Paul Alduy, 66100 Perpignan, France
3
Faculty of Agricultural, Life and Environmental Sciences, University of Alberta, Edmonton, AB T6G 2P5, Canada
4
Centro de Nanociencia y Nanotecnología, Universidad de Las Fuerzas Armadas (ESPE), Sangolquí 171103, Ecuador
5
Department of Chemical and Materials Engineering, Pontifical Catholic University of Rio de Janeiro (PUC-Rio), Rio de Janeiro 22453-900, Brazil
*
Authors to whom correspondence should be addressed.
Minerals 2024, 14(9), 891; https://doi.org/10.3390/min14090891
Submission received: 9 July 2024 / Revised: 19 August 2024 / Accepted: 28 August 2024 / Published: 30 August 2024
(This article belongs to the Section Mineral Processing and Extractive Metallurgy)

Abstract

Ferrous oxalate dihydrate is a versatile organic mineral with applications across fields. However, little is known about the feasibility of its synthesis directly from iron-bearing minerals using binary subcritical water (sCW) systems and its associated kinetics. In this study, the sCW+oxalic acid system at either 115 °C or 135 °C was investigated as a reaction medium for ferrous oxalate dihydrate (α-FeC2O4∙2H2O) synthesis, starting from ferrotitaniferous sands. The kinetics of the synthesis reaction were studied, and the physicochemical characterization of the as-synthetized ferrous oxalates was performed. Overall, the sCW synthesis was temperature-dependent, following second-order reaction kinetics according to the proposed precipitation pathway. A high reaction rate constant, significantly high yields (up to 89%), and reduced reaction times (2–8 h) were evident at 135 °C. The as-synthetized product corresponded to the monoclinic α-FeC2O4∙2H2O, showed relatively high specific surface areas (from 31.9 to 33.7 m2∙g−1), and exhibited band gap energies within the visible light range (~2.77 eV). These results suggest that α-FeC2O4∙2H2O can be synthesized using an organic dicarboxylic acid and iron-rich, widely available, low-cost mineral precursors. In addition, the as-prepared α-FeC2O4∙2H2O could be further optimized and tested for catalytic and visible light photocatalytic applications.
Keywords: α-FeC2O4∙2H2O; synthesis methods; oxalic acid; subcritical water; iron-rich minerals; photocatalyst α-FeC2O4∙2H2O; synthesis methods; oxalic acid; subcritical water; iron-rich minerals; photocatalyst

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MDPI and ACS Style

Valdivieso-Ramírez, C.S.; Galeas, S.; Saldaña, M.D.A.; Pontón, P.I.; Guerrero, V.H.; Vizuete, K.; Debut, A.; Marinkovic, B.A. Synthesis of Alpha Ferrous Oxalate Dihydrate from Ferrotitaniferous Mineral Sands via Hot Pressurized Aqueous Oxalic Acid: Kinetics and Characterization. Minerals 2024, 14, 891. https://doi.org/10.3390/min14090891

AMA Style

Valdivieso-Ramírez CS, Galeas S, Saldaña MDA, Pontón PI, Guerrero VH, Vizuete K, Debut A, Marinkovic BA. Synthesis of Alpha Ferrous Oxalate Dihydrate from Ferrotitaniferous Mineral Sands via Hot Pressurized Aqueous Oxalic Acid: Kinetics and Characterization. Minerals. 2024; 14(9):891. https://doi.org/10.3390/min14090891

Chicago/Turabian Style

Valdivieso-Ramírez, Carla S., Salomé Galeas, Marleny D. A. Saldaña, Patricia I. Pontón, Víctor H. Guerrero, Karla Vizuete, Alexis Debut, and Bojan A. Marinkovic. 2024. "Synthesis of Alpha Ferrous Oxalate Dihydrate from Ferrotitaniferous Mineral Sands via Hot Pressurized Aqueous Oxalic Acid: Kinetics and Characterization" Minerals 14, no. 9: 891. https://doi.org/10.3390/min14090891

APA Style

Valdivieso-Ramírez, C. S., Galeas, S., Saldaña, M. D. A., Pontón, P. I., Guerrero, V. H., Vizuete, K., Debut, A., & Marinkovic, B. A. (2024). Synthesis of Alpha Ferrous Oxalate Dihydrate from Ferrotitaniferous Mineral Sands via Hot Pressurized Aqueous Oxalic Acid: Kinetics and Characterization. Minerals, 14(9), 891. https://doi.org/10.3390/min14090891

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