The escalating demand for fertilizers and the scarcity of natural potassium (K) reserves highlight the need for sustainable recovery strategies. Vinasse, a by-product of sugarcane ethanol, contains exceptionally high organic loads (>100 g L-1 COD) and is discharged from the process at elevated temperature, conditions that enable efficient persulfate thermal activation (TAP) and justify its treatment with a combined TAP-Fenton process. Using substoichiometric doses of persulfate and hydrogen peroxide, the combined treatment promoted partial oxidation and coagulation, generating an iron-rich sludge (50 % Carbon) suitable for valorization. This sludge was transformed into hydrochar via hydrothermal carbonization (HTC) and subsequently activated with NaOH (HTC-A), which increased surface reactivity via deprotonated oxygenated groups. The activated hydrochar displayed strong K+ retention (up to 14.5 mg g-1) with pseudo-second-order kinetics (R2 > 0.99), indicating chemisorption by oxygenated functional groups. The spent hydrochar (HTC-S) also co-adsorbed phosphorus, supporting its use as a slow release, multinutrient soil amendment. Carbon retention analysis indicated a net sequestration potential of 1.25-1.45 t CO2 eq per ton of hydrochar. This combined functionality, namely nutrient recovery and carbon retention, supports the potential of the TAP-Fenton/HTC route as a circular strategy for the treatment and valorization of high-load agro-industrial effluents.

NO2-, a toxic and potentially carcinogenic nitrogen compound, poses serious risks to water quality and human health. Although several physicochemical treatments have been developed, many convert NO2- into NH4+ rather than N-2(g), limiting their environmental effectiveness. This study investigates the catalytic photo-reduction of NO2- using C(2)O(4)(2-)as a reducing agent and Fe3+ as a homogeneous catalyst under UV irradiation. The mechanism, intermediate species, and reaction kinetics were investigated by varying the concentration of the reactants and iron species. Complete NO2- conversion was achieved within 60 min under optimized conditions, with negligible NH4+ generation and transient detection of NOX gases only in the early reaction stages. Reaction mechanism follows a dual pathway, with contribution of NO2- disproportionation reactions which generate NO, NO2 and NO3-. NO and NO2 can further react with H2O producing HNO2 and HNO3. On the other hand, the photo-assisted catalytic decomposition of C2O42- yields CO2 center dot- radicals, which are responsible for the sequential NO2- reduction to NO center dot and N2O, ultimately achieving N-2 (g). Kinetic analysis showed that NO3- and NO2- reduction follow an apparent pseudo-first order kinetic model, with higher apparent rate constants at lower initial NO2- concentration. In contrast, C2O42- consumption follows a zero-order kinetic model. These findings provide mechanistic and kinetic insights into the selective photo-assisted reduction of NO2-, contributing to the development of advanced water treatment strategies targeting nitrogenous contaminants.

This study investigates a combined advanced oxidation process (AOP) utilizing UVA-LED irradiation (365 nm) for the degradation of sucralose (SUC), a complex artificial sweetener that poses a challenge for wastewater treatment due to its resistance to conventional methods. A sequential treatment strategy was employed. The initial step utilized UVA-activated persulfate (PS) at varying dosages (0.12-0.5 g/L) and UVA fluence rate (ranging from 20 to 100% of nominal output). The influence of natural water components (bicarbonate, chloride, sulfate, and nitrate) on PS activation was systematically analyzed. Notably, the substantial pH decrease during oxidation opened the possibility of replacing an amount of PS with the less expensive and more environmentally friendly hydrogen peroxide (H2O2) in the subsequent Fenton reaction. This second step employed a stoichiometric dosage of H2O2 (2.12 g/g COD) and varying Fe2+ concentrations (0.05-0.2 g/L), achieving a 95% overall mineralization within 60 min. The combined process incurred an approximate cost of 2.5 & euro; per m3. This research contributes to the development of more effective and environmentally friendly wastewater treatment strategies for emerging contaminants.

Wastewater treatment plants (WWTPs) generate large volumes of anaerobically digested sludge, whose high-water content (95 - 97 wt%) continues to pose major operational and economic burdens. Although anaerobic digestion reduces sludge organic load, it does not sufficiently improve dewaterability, creating a need for more effective conditioning strategies. In this study, thermally activated potassium persulfate (PS-H) is proposed as an efficient, catalyst-free method to enhance sludge dewatering under moderate mild conditions. Frist of all, a parametric study was conducted by varying oxidant concentration (0.25 - 2.0 mmol g(vs)(-1)), temperature (25 - 80 degrees C) and pH(0) (3 - 9). Under optimal conditions ([K2S2O8](0) = 1.0 mmol g(vs)(v-1); T = 60 degrees C; pH(0) = 5), PS-H achieved 54.4 % centrifuge weight reduction and a 78.6 % decrease in capillary suction time. These improvements clearly surpass those obtained with persulfate alone (10 % and 25.6 %, respectively), demonstrating a strong synergistic effect between persulfate and thermal activation. Mechanistically, the process promoted a > 50 % reduction in bound water, a marked decrease in viscosity, and pronounced floc disintegration. The transformation of tightly bound extracellular polymeric substances (EPS) into soluble fractions confirmed the effective structural disruption underlying the enhanced water release. Beyond dewatering performance, the treatment maximized nutrient release into the liquid phase, representing a promising and innovative strategy to simultaneously improve sludge dehydration and foster resource recovery in WWTPs.

The homogeneous Fe3+/oxalate system was examined as a Metal-Acid Light Induced (MALI) cycle for the photo-assisted reduction of nitrate (NO3-). A linear correlation between NO3-concentration removal and C2O42-con-sumption, at stoichiometric conditions, was obtained. This confirmed that CO2 center dot- radicals generated through ferrioxalate photolysis are the primary reductive species, enabling complete NO3 - conversion with no detectable accumulation of NH4+ or gaseous NOX and only minor transient NO2- formation. Time-resolved kinetic experiments demonstrated that NO3-undergo pseudo-first order, whereas oxalate decomposition follows zero-order behavior governed exclusively by the photon flux. A study has been conducted on the influence of the different variables affecting the Fe-Oxalate-UV cycle. A photonic operational window was identified in Fe-oxalate systems, delineating the transition from reagent-controlled to photon-limited regimes. Outside this window, excess oxalate activated competing oxidative pathways that re-oxidized nitrogenated byproduct and decreased NO3 - removal rate, thereby elucidating inconsistencies previously reported in the literature. Application to a real groundwater matrix revealed that Ca2+ induced CaC2O4 precipitation, markedly lowering UV transmittance and slowing the reaction. Mild acidification effectively suppressed precipitation restored photon utilization and produced NO3-reduction rates comparable to, and initially exceeding, those obtained in ultrapure water. These results close critical mechanistic and operational gaps in homogeneous photo-assisted NO3 - reduction. The integrated kinetic, photonic and matrix-dependence framework developed here provides quantitative design guidelines for reagent dosing, light delivery and water-quality conditioning. Collectively, these insights advance the rational scale-up of the MALI cycle as a selective and practical technology for NO3-remediation.

Reliable quantification of microplastics in wastewater is hindered by current particle-based methods. A novel gravimetric approach (Captoplastic) provides rapid, cost-effective mass-based metrics for monitoring and regulation.

This study systematically evaluates the impact of water-matrix complexity on the photo-Fenton oxidation of polystyrene (PS) nanoplastics (NPs), using operating conditions previously optimized for ultrapure water ([PS NPs]0 = 20 mg L−1, [Fe3+] = 1 mg L−1, pH0 = 3, and [H2O2]0 = 130 mg L−1 with sequential dosing). Degradation kinetics followed the Prout-Tompkins model, revealing an anionic inhibition trend (H2PO4− ≫ NO3− ≈ SO42− > Cl−). Phosphate was the main bottleneck due to iron complexation, whereas counter-cations showed negligible effects. The full inorganic matrix reduced the reaction rate by 45% through catalyst complexation and radical scavenging. Dissolved organic matter (DOM) further decreased the kinetic rate constant by 38–44%. Ultimately, the full complex matrix (ions + DOM) induced a 68% reduction in the reaction rate. Despite these constraints, complete mineralization of PS NPs was achieved within 40–140 min. Proof-of-concept applications in real matrices (bottled, tap, reclaimed water, and wastewater effluent) confirmed organic load as the primary kinetic driver, reducing the rate constant by up to 49%. Additionally, expanded polystyrene microplastics (MPs) removal in different real matrices exhibited significant weight loss (50–74%) with negligible final total organic carbon, indicating effective mineralization despite lower specific surface areas. SEM and TEM analyses confirmed a surface-driven degradation pathway for both NPs and MPs, progressing from the particle surface toward the core. Overall, these findings demonstrate the viability of the photo-Fenton process for removing persistent plastic contaminants in water reuse schemes.

The widespread occurrence of cyanotoxins in water bodies presents a significant health risk due to their high toxicity and persistence in the environment. Exposure to these toxins can lead to severe health issues, from gastrointestinal distress to organ failure, underscoring the urgent need for advanced water treatment methods. Catalytic Wet Peroxide Oxidation (CWPO) has proven effective for cyanotoxin removal; however, the specific degradation pathways during CWPO remain unclear. This study elucidates the possible degradation pathways of some of the most globally prevalent cyanotoxins, including microcystin-LR (MC-LR) and cylindrospermopsin (CYN), through CWPO using magnetite as a catalyst. These pathways involve hydroxylation, dehydrogenation, decarboxylation, functional group substitution, and ring opening, identifying new degradation by-products. The evolution of ecotoxicity during CWPO was also examined, revealing an initial increase in effluent toxicity under sub-stoichiometric H2O2 conditions, but eventually declines below the toxicity of the original cyanotoxins. Raising the oxidant concentration to stoichiometric levels efficiently eliminates cyanotoxins, yielding primarily short-chain organic acids in a completely non-toxic effluent. These findings are critical for optimizing CWPO as a safe, efficient, and sustainable approach for treating cyanotoxins in water, marking important progress towards cost-effective and environmentally friendly water treatment solutions.

Microplastics (MPs) are persistent pollutants of growing environmental concern, and advanced oxidation processes (AOPs) have been increasingly investigated as promising routes to accelerate their transformation beyond conventional treatments. In this study, homogeneous photo-Fenton oxidation was applied to cryo-milled commercial MPs (50-100 & micro;m) of polyethylene terephthalate (PET), low-density polyethylene (LDPE), polycarbonate (PC), polyvinyl chloride (PVC), and expanded polystyrene (EPS) to assess polymer-dependent degradation under controlled conditions. Degradation was quantified through a combined solid-liquid carbon assessment based on gravimetric weight loss (solid-phase removal) and aqueous Total Organic Carbon (TOC) (mineralization yield). Scanning Electron Microscopy (SEM) provided insights into particle morphology and surface damage, while Energy-Dispersive X-ray Spectroscopy (EDS) and Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR) were employed to track elemental and chemical changes, respectively. Finally, elemental analysis was used to assess bulk compositional shifts during oxidation. A polymer-dependent degradation trend was observed after 8 h of photo-Fenton treatment, EPS (approximate to 74 %) > LDPE > PC > PET approximate to PVC (approximate to 40 %), accompanied by extensive mineralization (aqueous TOC < 1 mg L-1). Clear oxidation signatures were also found on MPs surfaces, including the emergence of surface pitting, cavities, and microcracks in SEM, together with increased oxygenated functionalities detected by ATR-FTIR/EDS. The degradation kinetics of EPS and PET were successfully described by the Shrinking Core Model (SCM) for spherical particles (R-2 > 0.99), indicating ash-layer diffusion behavior for EPS and surface chemical control behavior for PET.

Nanoparticles based on Fe, Ni and Pd (Fe_100, Ni_100, Pd_100, PdFe_5050 y PdNi_5050) were synthesized via chemical reduction with NaBH4 and their catalytic activity was evaluated in the hydrodehalogenation (HDH) of diclofenac in aqueous phase in batch experiments. The results demonstrated the higher catalytic activity of Pd-based systems. Monometallic Ni_100 and Fe_100 showed low catalytic activity. In Fe_100 system, the degradation followed an oxidative pathway dependent on dissolved oxygen, in addition to significant metal leaching due to Fe-0 oxidation. Conversely, although PdFe_5050 proves to be highly active, the high Fe leaching limited its long-term viability. In contrast, both Pd_100 and PdNi_5050 nanoparticles achieved complete diclofenac (DFC) dechlorination within 60 min, effectively suppressing the accumulation of chlorinated intermediates. The high efficiency of PdNi_5050 was attributed to the surface enrichment of Pd within the bimetallic system. This synergy allowed PdNi_5050 to match the activity of Pd_100, despite the lower content of the precious metal. Finally, PdNi_5050 proved to be a promising alternative, maintaining high catalytic activity and stability over 10 consecutive cycles. This, coupled with the significant reduction in the associated material costs, positions PdNi_5050 as a promising option for HDH process.

This work is focused on developing and evaluating structured catalytic membranes for the degradation of micropollutants via catalytic wet peroxide oxidation (CWPO). A simple, flow-through deposition method was developed to incorporate five different minerals (Fe3O4, Fe2O3, FeOOH, CuO and MnO2) onto a propylene microfiltration membrane. The resulting catalytic membranes (PP_Mineral) were extensively characterized, confirming the successful incorporation of the active phases onto their surface. These materials also exhibited high mineral retention, with magnetite showing the highest retention efficiency (99.3%). The catalytic performance was assessed using sulfamethoxazole (SMX) as target pollutant. Among the prepared structured catalysts, PP_Fe3O4 demonstrated the highest catalytic efficiency, achieving a significant 73% SMX removal after 3 h of reaction. Furthermore, the PP_Fe3O4 structured catalyst showed an outstanding stability through a continuous flow experiment lasting over 100 h, maintaining constant activity with negligible metal leaching and catalyst particle loss. These results demonstrate the potential of the structured catalytic membranes developed in this work for water treatment applications.

Catalytic wet peroxide oxidation (CWPO) is introduced as a novel advanced oxidation process (AOP) for treating microwave-activated microplastics (MPs), specifically LDPE and PP. Graphite was used as a metal-free catalyst to promote H2O2 decomposition into reactive oxygen species (HO· and HOO·) that drive plastic oxidation in aqueous phase.The effects of H2O2 dosage, temperature, reaction time, MP concentration and graphite loading were evaluated in terms of plastic conversion, morphological changes, carbon distribution in gas and aqueous phases and the nature of oxidation by-products. Without H2O2, plastic transformation mainly produced gaseous compounds, whereas H2O2 shifted the pathway toward oxygenated water-soluble products, including ketones, aldehydes, alcohols, and short-chain carboxylic acids. Higher temperatures increased MP conversion, while shorter reaction times limited over-oxidation of dissolved organic carbon.At high MP concentration (8 g L−1) under 180 °C, 2 h, MP:graphite = 8:2 c c−1, MP:H2O2 = 8:40 c c−1, up to 40 wt% of the initial carbon (2725 mg C L−1) was recovered in the aqueous phase (∼25 wt% as short-chain carboxylic acids). At lower MP concentration (1 g L−1) with MP:graphite = 1:1 c c−1 and MP: H2O2 = 1:5 c c−1, complete MP conversion was achieved under the same temperature and time.Overall, CWPO stands out among AOPs by operating under realistic conditions (180 °C, 2 h) for scalability and efficiently treating high MP loadings. These results highlight CWPO as a versatile process that can be directed toward either the complete MP removal or selective production of value-added chemical products.

Nanoparticlesbased on Fe, Ni and Pd (Fe_100, Ni_100, Pd_100, PdFe_5050 y PdNi_5050) were synthesized via chemical reduction with NaBH4 and their catalytic activity was evaluated in the hydrodehalogenation (HDH)of diclofenac in aqueous phase in batch experiments. The results demonstrated the higher catalytic activity of Pd-based systems. Monometallic Ni_100 and Fe_100 showed low catalytic activity. In Fe_100 system, the degradation followed an oxidative pathway dependent on dissolved oxygen, in addition to significant metal leaching due to Fe0oxidation.Conversely, although PdFe_5050 proves to be highly active, the high Fe leaching limited its long-term viability. In contrast, both Pd_100 and PdNi_5050 nanoparticlesachieved complete diclofenac (DFC)dechlorination within 60 min, effectively suppressing the accumulation of chlorinated intermediates. The high efficiency of PdNi_5050 was attributed to the surface enrichment of Pd within the bimetallic system. This synergy allowed PdNi_5050 to match the activity of Pd_100, despite the lower content of the precious metal.Finally, PdNi_5050 proved to be a promising alternative, maintaining high catalytic activity and stability over 10 consecutive cycles. This, coupledwith the significant reduction in the associated material costs, positions PdNi_5050 as a promising option for HDH process.

The increasing occurrence of toxic cyanobacteria blooms in drinking water sources poses a global health risk, underscoring the need for new, economically viable, and eco-friendly treatments. Catalytic Wet Peroxide Oxidation (CWPO), using natural magnetite, has shown strong potential for degrading cyanobacteria and cyanotoxins, though scaling it up for continuous, large-scale treatment remains challenging. This study evaluated the CWPO process at pilot scale using a continuous stirred slurry tank reactor (3 L) coupled with continuous magnetite recovery to degrade microcystin-LR (MC-LR), one of the most prevalent cyanotoxin worldwide, under ambient conditions. Key operational variables (including magnetite concentration, initial H2O2 concentration, and pH) were optimized. Under optimal conditions ([Fe3O4] = 8 g L-1; [H2O2](0) = 12.6 mg L-1; flow rate = 50 mL min(-1); pH(0) = 3.5), the process achieved up to 90% MC-LR degradation. Simultaneous elimination of cyanobacteria (>99.9%) and 85% cyanotoxin reduction was achieved in the presence of Microcystis aeruginosa cells (50 mu g L-1, measured as chlorophyll-a). A slight process intensification ([Fe3O4] = 10 g L-1; [H2O2](0) = 15 mg L-1) allowed increasing to 95% the cyanotoxin degradation, resulting in a fully non-toxic effluent (Daphtoxkit-F ISO standard 6341 procedure). Finally, an industrial-scale design was proposed for a Drinking Water Treatment Plant (DWTP) designed for 10,000 population equivalent, with estimated costs of 0.19 per treated cubic meter after economical optimization. Electricity for aeration, hydrogen peroxide consumption and pH adjustment were identified as the main contributors to the overall operating cost. This approach offers a safe and sustainable, advancing innovative water treatment technologies.

Urban stormwater runoff is increasingly recognized as a valuable alternative water source, yet its reuse is hindered by emerging pollutants such as microplastics. Among these, tire-wear particles (TWP) represent a major concern due to their ubiquity and potential toxicity. This study explores ballasted flocculation (BF) as a compact and high-rate physicochemical treatment for the targeted removal of TWP from urban runoff. Natural magnetite was selected as ballast material, as it enhances floc density and settling while offering magnetic properties that enable easy separation and recovery for reuse, supporting a circular treatment approach. To simulate stormwater conditions, aged TWPs were prepared in the laboratory by oxidative aging (UV/PMS). BF experiments demonstrated faster clarification compared to conventional flocculation, exhibiting nearly two-fold higher apparent first-order clarification rate constants and achieving up to 94% turbidity removal within 15 s when using magnetite fraction of 32-50 mu m. Operational parameter analysis confirmed robust performance across variations in coagulant dose, ballast concentration, and TWP levels, while pH adjustment to neutrality proved crucial. Under these conditions, effluent turbidity was reduced to 2.3 NTU and particle size analysis of the effluent revealed a clear shift toward particles <50 mu m, confirming effective removal of the added TWP (similar to 130 mu m). Additional removal of bulk organic matter was evidenced by reductions of 61% TOC and 44.5% UV254. Zeta potential measurements showed a change from -20.30 mV to -6.50 mV, indicating charge neutralization and floc consolidation. BF process produces compact sludge and clarified effluent, supporting decentralized stormwater treatment under short effective treatment times.

This work examines the application of active learning methodologies, including interactive platforms and project-based learning (PBL), in the subject "Bases de la Ingenier & iacute;a Ambiental" (Fundamentals of Environmental Engineering, FEE) at the Universidad Autonoma de Madrid. Over five academic years (2019/20-2023/24), student response systems (SRSs) such as Kahoot! and Edpuzzle were implemented to foster participation and improve conceptual understanding through gamified quizzes and video-based problem-solving. Additionally, PBL was introduced to promote hands-on learning, teamwork, and critical thinking. The intervention involved approximately 130 students per academic year. Comparative analysis of academic performance showed an increase in average final grades from 4.81 (pre-intervention period) to 5.62 in the two most recent academic years, along with higher scores in continuous assessment activities. Student satisfaction indicators remained consistently high, with institutional surveys showing no negative deviations even during pandemic-related disruptions. Professors reported a positive perception of the methodology, highlighting improved student engagement without loss of control over class dynamics. These findings support the value of combining SRS tools and PBL as a robust framework to enhance motivation and academic achievement in environmental engineering education.

Cyanuric acid (CYA) is widely used as a chlorine stabilizer in swimming pools, but concentrations above 75 mg L−1 cause overstabilization and loss of disinfection capacity. This study evaluated CYA removal by advanced oxidation processes, including heterogeneous photocatalysis, photo-Fenton, photo-persulfate, and anodic oxidation (AO). AO with boron-doped diamond anodes proved most effective, achieving up to 90% total organic carbon removal in ultrapure water. When applied to real swimming pool samples (118 and 251 mg L−1 CYA), the process achieved significant CYA abatement, demonstrating its potential as a practical strategy to control overstabilization without additional chemicals.

Microplastic fibers (MFs) from synthetic garments pose a growing environmental challenge, as their release during domestic laundry cycles and persistence in wastewater have facilitated their dispersion in aquatic ecosystems, as well as their accumulation along the food chain. In this context, advanced oxidation processes (AOPs), capable of breaking down refractory organic pollutants, emerge as a promising alternative to mitigate this issue. In this study, the effectiveness of photo-Fenton to remove PET MFs was evaluated by quantifying their weight loss. Physical and chemical changes in the fibers were followed using scanning electron microscopy coupled to energy-dispersive X-ray spectroscopy (SEM-EDS) and Fourier transform infrared spectroscopy (ATR-FTIR). Total organic carbon (TOC) of the effluents obtained after the photo-Fenton treatment was also measured to determine the degree of mineralization achieved. Moreover, the effect of hydrogen peroxide concentration and reaction time was investigated. A starting H2O2 concentration of 500 mg L-1 was identified as optimal, yielding 40.6 % mass loss of PET MFs after 4 h. Under these conditions, 16 h tests resulted in 99 % mass loss, with high mineralization yields (TOC < 0.5 mg L-1) . The degradation was successfully described by a cylindrical Shrinking Core Model (R2 > 0.99). Progressive cavity and hole formation, and the appearance of oxygenated functionalities, were also observed upon treatment. Finally, the degradation of MFs fragments was examined to evaluate the role of morphology, and the effect of real fibers obtained from a washing cycle was also assessed.

The degradation of the UV filter benzophenone-3 (BP-3) by low-frequency ultrasound was investigated in different aqueous matrices. BP-3 sonodegradation followed pseudo-first-order kinetics, achieving >97 % removal of 500 μg L-1 of BP-3 within 120 min in ultrapure water (UPW), using a 20 kHz ultrasound horn at 71 W L-1. Varying the initial pH from 3 to 6 and 9 had only a slight effect on the process efficacy, with corresponding kinetic constant rates of 0.029, 0.030, and 0.041 min-1, respectively. Experiments conducted in different water matrices showed a decrease in the apparent rate constant from 0.030 min-1 in ultrapure water to 0.027 min-1 in drinking water and 0.015 min-1 in secondary effluent. Similarly, the presence of 250 mg L-1 of chlorides or 10 mg L-1 of humic acid reduced the degradation rate to 0.016 and 0.020 min-1, respectively, while 250 mg L-1 of hydrogen carbonate had no significant effect. The presence of nano- or microplastics led to a moderate decrease in BP-3 removal, particularly with smaller particles. Electron paramagnetic resonance (EPR) spectroscopy confirmed that fewer hydroxyl radicals were available in the presence of plastics. Twelve transformation products were identified by UHPLC-TOF/MS, resulting mainly from hydroxylation, demethylation, and ring-cleavage. According to the ecotoxicity analysis using the ECOSAR software, most of the transformation products were less toxic than the parent compound, enhancing the environmental feasibility of the process.

Formic acid (FA) is a promising liquid organic hydrogen carrier for safe and efficient hydrogen handling. FA dehydrogenation occurs under near‐ambient conditions using palladium/activated carbon (Pd/AC) catalysts, but aspects like high Pd loading and gradual catalyst deactivation remain key challenges. This study investigates how the physicochemical properties of Pd nanoparticles and support characteristics influence the continuous process performance including FA conversion, evolved gas flow rate, total hydrogen production, and catalyst durability. Pd catalysts were prepared via wet impregnation using various precursors, powdered supports, and Pd loadings and evaluated in a fixed‐bed reactor. The findings reveal that Pd/AC catalysts prepared with PdCl₂ precursor and nanopowdered AC are the most efficient. Strong electrostatic interactions between negatively charged PdCl₄ 2 ⁻ species and the positively charged AC surface during impregnation enhance nanoparticle support interactions, resulting in small (∼2 nm), highly dispersed Pd nanoparticles with a high Pd 2 ⁺/Pd⁰ atomic surface ratio. Metal dispersion is the dominant factor influencing hydrogen production, surpassing the effects of both particle size and electronic state. Higher Pd loadings also increased catalyst durability, reducing regeneration frequency. This study provides valuable insights into the rational design of Pd/AC catalysts, paving the way for efficient FA utilization as a hydrogen carrier.