The role of p-benzoquinone (BQ) as a photocatalyst in the synthesis of solketal under UV irradiation has been studied, along with the combined use of BQ/TiO₂ P25 as a photocatalytic system for the process. The presence of the O₂/O₂^−• redox couple is essential for the reaction to take place. However, experiments with p-benzoquinone as a superoxide radical scavenger failed, with the opposite effect of enhancing the reaction being observed. It was found that p-benzoquinone and oxygen compete for photogenerated electrons in the conduction band of titania. A redox equilibrium between p-benzoquinone and hydroquinone (H₂Q), mediated by the O₂/O₂^−• system, was identified as a key factor in enabling the reaction. Furthermore, EPR spin-trapping experiments confirmed the presence of the carbon-centered radical 2-hydroxypropan-2-yl, which was determined to be the main radical species involved in the process. Either acetone or 2-propanol can generate this radical, with the BQ/H₂Q redox system being pivotal in the formation of the hemiacetal intermediate. This intermediate is subsequently converted into the final acetal (solketal), with H₂Q acting as a photoacid through an excited-state proton transfer (ESPT) mechanism. The photoacid behavior of hydroquinone was confirmed using pyridine as a basic probe, as the formation of hydroquinone–pyridine adducts was detected by Raman spectroscopy.

Pt-TiO₂ systems are the most widely used photocatalysts in the production of green hydrogen from glycerol photoreforming. To incorporate metals on the surface of materials, photodeposition is the most used method because it employs mild conditions. However, despite its use, there are some parameters that have not been deeply studied, such as the appropriate metal loading and the method itself, to obtain a better dispersion of Pt. In this work, six Pt-TiO₂ catalysts were synthesized by a classical photodeposition method employing UV radiation. The studied Pt wt.% range was 0.15–0.60 wt.%, being incorporated in one step or in subsequent ones. HRTEM analyses showed that both methods allowed a homogeneous distribution of Pt, and in both, the particle size was around 2.3–3.6 nm, increasing with metal loading. The photocatalytic activity of materials was tested in glycerol photoreforming under UV radiation, and the 0.45 wt.% Pt-containing solid that had been synthesized in one step was the one that allowed the highest hydrogen production. This might suggest that around 0.40% is the appropriate metal loading for hydrogen production under these conditions and that incorporating the desired metal percentage in one step is the most efficient method in terms of energy and time savings.

Biotemplating technique allows the synthesis of catalysts, recreating the sophisticated structure of nature templates. In this work, some biotemplated TiO₂ semiconductors were synthesized using Olea europaea leaves as templates. Then, g-C₃N₄ was coupled to materials to later incorporate Pt on the surface or as dopant in the structure to evaluate the efficiency of the solids in two photocatalytic applications to valorize biomass: hydrogen production through glycerol photoreforming, and photoacetalization of cinnamaldehyde with 1,2-propanediol. In glycerol photoreforming, the presence of Pt (superficial or dopant) enhanced hydrogen production, being Pt@AOLCN (a heterojunction containing biotemplated TiO₂, g-C₃N₄, and Pt) the system that exhibited the highest efficiency (3053.4 µmol·g_cat⁻¹·h⁻¹). For photoacetalization, while Pt reduced cinnamaldehyde conversion, it improved selectivity when incorporated on TiO₂. Notably, carbon nitride (CN) exhibited the highest yield after 16 h of testing. The study emphasizes the importance of tailoring catalyst selection to specific reactions, as efficiency is closely tied to the structural and chemical properties of the materials. These findings contribute to the development of efficient photocatalysts for sustainable biomass valorization processes.

Biotemplated strategies inspired by natural architecture have emerged as an effective strategy to improve the performance of photocatalytic materials. In this work, TiO₂-based photocatalysts were synthesized using olive leaves as a biological template to reproduce their hierarchical microstructure and enhance photocatalytic hydrogen production. The artificial olive leaf (AOL) support was obtained through a biotemplated ion-exchange process followed by hydrolysis and calcination. It was then modified by photodeposition of Au or Pt nanoparticles. The materials were characterized by SEM, XRD, N₂ adsorption–desorption, UV–Vis spectroscopy, and XPS to evaluate their structural and optical properties. SEM confirmed the successful replication of both the external morphology and internal architecture of the olive leaf, while XRD revealed low crystallinity with anatase as the only TiO₂ phase. Optical characterization showed a reduced band gap (~2.97 eV), and extended absorption toward the visible region, with Au nanoparticles exhibiting a plasmonic band at ~550 nm, whereas Pt enhanced light-harvesting efficiency. XPS indicated the presence of oxygen vacancies and Ti³⁺ species that promote metal–support interactions. Photocatalytic glycerol photoreforming showed a strong enhancement in hydrogen production after noble metal incorporation, reaching up to 14-fold under UV irradiation and 23-fold under simulated solar light for the Pt-modified catalyst, highlighting the synergy between biotemplated structuring and noble metal deposition.

The global proliferation of plastic waste has made the search for sustainable chemical recycling strategies imperative to transition toward a circular bioeconomy. This study presents a dual-valorization approach for polylactic acid (PLA) waste, utilizing it both as a sustainable precursor for g-C₃N₄ catalyst synthesis and as a sacrificial agent for green hydrogen production via photoreforming. Platinum-modified graphitic carbon nitride catalysts were synthesized and evaluated using pure lactic acid and commercial PLA waste under solar-simulated irradiation. Results identified C₃N₄-NaOH-Pt as the most active material, while the simultaneous one-pot depolymerization/photoreforming of macroscopic PLA fragments exhibited a peak H₂ production rate of 1.5 mmol·h⁻¹·g⁻¹, remarkably surpassing both the pure monomer model and pre-depolymerized solutions. This enhanced performance is tentatively attributed to a “controlled release” mechanism that prevents catalyst surface saturation and minimizes light scattering effects inherent to fine powders. The study concludes that maintaining the macroscopic integrity of PLA waste provides a strategic advantage for chemical reforming by eliminating energy-intensive grinding and pretreatment. Future research into diverse operational and chemical parameters, including temperature and base-addition strategies, will be essential for scaling solar-driven upcycling technologies.