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.

We report a visible-light-activated nanobioherbicide based on the conjugated polymer poly(2,5-di(hexyloxy)cyanoterephthalylidene) (CNPPV) for the controlled delivery of the natural bioherbicide usnic acid (UA). The nanostructures were fabricated by an adapted nanoprecipitation method, yielding spherical nanoparticles with a mean hydrodynamic diameter of 162 ± 76 nm, polydispersity index < 0.25, and encapsulation efficiency > 80%. Photophysical studies demonstrated strong optical absorption and efficient photoresponsiveness under blue-light irradiation (450 nm). Light-triggered release experiments revealed non-Fickian transport behavior characterized by a Super Case II mechanism. The nanobioherbicide exhibited adequate colloidal stability during 90 days of protected storage and showed light-triggered release of UA, inducing a concentration-dependent photoinhibitory response in Lemna minor. This work demonstrates a visible-light-responsive nanoplatform for usnic acid delivery and provides proof-of-concept evidence of its phytotoxic effects in Lemna minor, supporting further investigation of conjugated polymers for agrochemical delivery.