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Volume 6
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Article

MOF-Derived TiO2 Photocatalysts for Hydrogen Production Coupled to Selective Glycerol Oxidation at Near-Neutral pH

by
Emerson Faustino
1,†,
Priscila Sabioni Cavalheri
2,†,
Emmanuel da Silva Côgo Miguel
2,
Thalita Ferreira da Silva
3,
Gabriel Henrique Diniz Manicoba
4,
Ana Beatriz Saldanha da Silva Ezequiel
4,
Luiz Eduardo Gomes
2,
Heberton Wender
2,
Anderson Rodrigues Lima Caires
2,
Rodrigo Pereira Cavalcante
5 and
Amilcar Machulek Junior
4,*
1
Institute of Chemistry, Federal University of Mato Grosso do Sul, Senador Filinto Muller Ave., 1555, Campo Grande 79070-900, MS, Brazil
2
Institute of Physics, Federal University of Mato Grosso do Sul, Senador Filinto Muller Ave., 1555, Campo Grande 79070-900, MS, Brazil
3
São Carlos Institute of Chemistry, University of São Paulo, Trab. São Carlense Ave., 400, São Carlos 13566-590, SP, Brazil
4
Institute of Chemistry, Federal University of Rio Grande do Norte, Senador Salgado Filho Ave., s/n, Natal 59078-970, RN, Brazil
5
Institute of Chemistry, Federal University of Alfenas, Alfenas 37130-001, MG, Brazil
*
Author to whom correspondence should be addressed.
†
These authors contributed equally to this work.
Nanomanufacturing 2026, 6(2), 7; https://doi.org/10.3390/nanomanufacturing6020007
Submission received: 29 November 2025 / Revised: 17 January 2026 / Accepted: 17 March 2026 / Published: 26 March 2026
(This article belongs to the Topic Innovative Synthesis and Applications of Functional Nanomaterials)
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Abstract

Simultaneous hydrogen fuel and value-added chemical production from renewable resources is a key strategy in sustainable catalysis. This work presents a novel strategy employing metal–organic frameworks (MOFs) as precursors for synthesizing advanced titanium dioxide (TiO2) photocatalysts with enhanced structural and optical properties. Two photocatalysts, M-BDC and M-2,5PDC, were synthesized via controlled calcination of MIL-125(Ti) using terephthalic and 2,5-pyridinedicarboxylic acids, respectively. Characterization confirmed the formation of mixed anatase/rutile TiO2 phases with mesoporous structures. Notably, nitrogen incorporation in M-2,5PDC reduced the optical band gap to 2.94 eV compared with 3.08 eV for M-BDC, enhancing visible-light absorption. Photocatalytic experiments conducted at near-neutral pH (6.0) demonstrated effective simultaneous glycerol oxidation and hydrogen evolution without the use of alkaline additives. M-BDC achieved 30% glycerol conversion with 78.85% selectivity toward dihydroxyacetone and 21.15% toward glyceraldehyde, while M-2,5PDC exhibited selectivities of 71.55% and 28.45%, respectively. Glycerol underwent partial oxidation without complete mineralization, generating high-value products in parallel with hydrogen production. Both catalysts displayed excellent reuse stability across three consecutive cycles, with M-BDC showing enhanced dihydroxyacetone selectivity (78.85% to 84.42% between cycles). This MOF-derived TiO2 platform integrates controlled synthesis, near-neutral pH operation, high selectivity, and catalytic stability, thereby establishing a viable strategy for the simultaneous production of clean fuel and value-added chemicals from renewable resources.
Keywords: metal–organic frameworks; photocatalysis; hydrogen production; glycerol oxidation; dihydroxyacetone; sustainable catalysis metal–organic frameworks; photocatalysis; hydrogen production; glycerol oxidation; dihydroxyacetone; sustainable catalysis

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MDPI and ACS Style

Faustino, E.; Cavalheri, P.S.; Miguel, E.d.S.C.; da Silva, T.F.; Manicoba, G.H.D.; Ezequiel, A.B.S.d.S.; Gomes, L.E.; Wender, H.; Caires, A.R.L.; Cavalcante, R.P.; et al. MOF-Derived TiO2 Photocatalysts for Hydrogen Production Coupled to Selective Glycerol Oxidation at Near-Neutral pH. Nanomanufacturing 2026, 6, 7. https://doi.org/10.3390/nanomanufacturing6020007

AMA Style

Faustino E, Cavalheri PS, Miguel EdSC, da Silva TF, Manicoba GHD, Ezequiel ABSdS, Gomes LE, Wender H, Caires ARL, Cavalcante RP, et al. MOF-Derived TiO2 Photocatalysts for Hydrogen Production Coupled to Selective Glycerol Oxidation at Near-Neutral pH. Nanomanufacturing. 2026; 6(2):7. https://doi.org/10.3390/nanomanufacturing6020007

Chicago/Turabian Style

Faustino, Emerson, Priscila Sabioni Cavalheri, Emmanuel da Silva Côgo Miguel, Thalita Ferreira da Silva, Gabriel Henrique Diniz Manicoba, Ana Beatriz Saldanha da Silva Ezequiel, Luiz Eduardo Gomes, Heberton Wender, Anderson Rodrigues Lima Caires, Rodrigo Pereira Cavalcante, and et al. 2026. "MOF-Derived TiO2 Photocatalysts for Hydrogen Production Coupled to Selective Glycerol Oxidation at Near-Neutral pH" Nanomanufacturing 6, no. 2: 7. https://doi.org/10.3390/nanomanufacturing6020007

APA Style

Faustino, E., Cavalheri, P. S., Miguel, E. d. S. C., da Silva, T. F., Manicoba, G. H. D., Ezequiel, A. B. S. d. S., Gomes, L. E., Wender, H., Caires, A. R. L., Cavalcante, R. P., & Machulek Junior, A. (2026). MOF-Derived TiO2 Photocatalysts for Hydrogen Production Coupled to Selective Glycerol Oxidation at Near-Neutral pH. Nanomanufacturing, 6(2), 7. https://doi.org/10.3390/nanomanufacturing6020007

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