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- Apósitos absorbentes a base de sericina de seda para la liberación de fármacos en el tratamiento de heridas cutáneas(2026) Arango Sánchez, Camila; Cháfer Ortega , Amparo; Cerisuelo i Feriols, Josep Pasqual; Álvarez-López, Catalina; Escola de DoctoratLa prevalencia de heridas crónicas y úlceras patológicas representa un desafío importante para los sistemas de salud debido a las limitaciones de los tratamientos actuales. Estas afecciones, presentan lenta cicatrización, inflamación persistente y alta susceptibilidad a infecciones. En este contexto, los apósitos avanzados con liberación controlada de fármacos han surgido como una alternativa prometedora. Sin embargo, muchos biomateriales presentan dificultades para controlar simultáneamente propiedades como absorción, estabilidad en medios húmedos y liberación sostenida de fármacos, además de requerir agentes reticulantes químicos potencialmente tóxicos. El objetivo principal de esta tesis doctoral fue desarrollar apósitos absorbentes a base de sericina (SS) para la incorporación y liberación controlada de sulfato de gentamicina en heridas cutáneas infectadas. Para ello, se utilizó SS, extraída de capullos defectuosos, un subproducto de la industria serícola colombiana, debido a sus propiedades antioxidantes, biocompatibles y con alta capacidad de absorción. La investigación se desarrolló mediante metodologías físicas, incluyendo liofilización, secado por atomización y métodos de reticulación física verde. Inicialmente, se evaluó el efecto de tratamientos físicos con etanol sobre estructuras porosas basadas únicamente en SS, con el fin de comprender los cambios inducidos en estabilidad acuosa, organización estructural y comportamiento mecánico. Posteriormente, se estudió el efecto de incorporar alcohol polivinílico (PVA) y diferentes métodos de reticulación física verde en mezclas SS/PVA, buscando mejorar la estabilidad estructural, la absorción y las propiedades mecánicas. A partir de estos fundamentos, se aplicó una metodología de superficie de respuesta para optimizar membranas basadas en mezclas ternarias de sericina, gelatina y PVA, utilizando glicerol como plastificante y modulador estructural. El objetivo fue obtener membranas flexibles, absorbentes, estables en medios fisiológicos simulados y con propiedades adecuadas de transmisión de vapor de agua. Asimismo, se desarrollaron micropartículas de sericina/sulfato de gentamicina mediante secado por atomización como sistema de liberación. El proceso de encapsulación fue optimizado y posteriormente se evaluó la cinética de liberación y el coeficiente de difusión mediante modelado matemático. Las micropartículas optimizadas fueron incorporadas en la membrana optimizada para desarrollar un sistema compuesto multifuncional, evaluando sus propiedades estructurales, fisicoquímicas, biológicas y antibacterianas. Los estudios biológicos demostraron que el sistema desarrollado no presentó citotoxicidad sobre queratinocitos y fibroblastos humanos, preservando la actividad metabólica celular sin inducir respuestas proinflamatorias. Además, exhibió una rápida actividad antibacteriana frente a bacterias Gram-positivas y Gram-negativas de relevancia clínica, alcanzando una reducción completa de los recuentos viables bacterianos y confirmando un efecto bactericida asociado a la difusión localizada de gentamicina desde la membrana. Los resultados obtenidos permitieron establecer una ruta tecnológica integral y prometedora para la obtención de un prototipo de apósito multifuncional basado en sericina, con capacidad de absorción, control de humedad y liberación localizada de antibiótico para el tratamiento de heridas cutáneas infectadas.
- Polyproline based drug-delivery platform for targeted cell penetration: platform screening and industrial insights towards scale-up(2026) Karpova, Ekaterina; Duro Castaño, Aroa; Vicent Docón, María Jesus; Felip León, Carles; Escola de DoctoratNanomedicine offers new opportunities to improve drug delivery through targeted and polymer-based nanocarriers. However, clinical translation remains limited by insufficient subcellular targeting and the lack of robust, scalable manufacturing processes. This thesis addresses both challenges by developing novel poly(amino acid)-based carriers for mitochondrial targeting and establishing reproducible synthesis protocols using a Quality-by-Design approach. First, poly(L-proline)-based cell-penetrating diblock copolymers were synthesized by N-carboxyanhydride ring-opening polymerization. The developed platform enabled the preparation of well-defined polyornithine–polyproline copolymers together with lysine, arginine, histidine, and hydroxyproline analogues. Biological evaluation demonstrated that mitochondrial localization strongly depended on the block composition, with only specific polyornithine-to-polyproline ratios exhibiting selective mitochondrial targeting while maintaining acceptable cytotoxicity. The hydroxyproline analogue further expanded the versatility of the platform by introducing reactive hydroxyl groups for future functionalization. To support future translation, the synthesis of the lead mitochondrial-targeting copolymer was optimized using Design of Experiments. Critical process parameters were identified, statistically validated, and used to establish a design space and proven acceptable ranges according to ICH Q8/Q11 principles. The optimized process enabled reproducible scale-up from laboratory synthesis to gram-scale production while maintaining polymer quality and batch-to-batch consistency. Finally, polyproline was explored as a structural component of amphiphilic PEG-based triblock copolymers for nanoparticle drug delivery. Histidine- and glutamate-containing copolymers were synthesized, characterized, and evaluated for self-assembly. Histidine-based random copolymers formed stable micelles capable of encapsulating hydrophobic drugs such as doxorubicin and paclitaxel with high encapsulation efficiencies. The resulting nanoparticles showed controlled physicochemical properties and preliminary evidence of pH-responsive drug release. Overall, this work establishes versatile synthetic methodologies for proline-based polymer therapeutics, demonstrates the first statistically optimized NCA polymerization process for scalable manufacturing of mitochondrial-targeting copolymers, and introduces new amphiphilic polymer platforms for drug delivery. These findings provide a foundation for the future development of clinically translatable polymer nanomedicines for cancer, neurodegenerative, and metabolic diseases.
- A novel [GO-Fe(II) macrocycle@Fe₃O₄] nanocomposite with enhanced surface area, stability, and electrochemical performance for next-generation supercapacitors(2026) Hassouna, Chaima; Agren, Soumaya; El Haskouri, Jamal; Menéddez, Nicolás; Culebras, Mario; Baouab, Mohamed Hassen V.Supercapacitors are emerging as efficient solutions to meet growing global energy demands due to their high-power density and rapid charge-discharge capability. Graphene oxide (GO) derivatives, with their tunable physicochemical properties, are strong candidates for advanced electrode materials. This study presents a hierarchical GO-based nanocomposite integrating a tetra-aza macrocycle, Fe(II)(C40H24N4), and magnetite (Fe3O4) nanoparticles to enhance supercapacitor performance. Structural characterization confirms successful material assembly: XRD shows a crystallite size reduction from 28 nm for the GO-macrocycle system to 14 nm after Fe3O4 addition, while SEM/EDX and XPS analyses verify uniform Fe3O4 dispersion and proper elemental composition. Textural analysis reveals a fourfold increase in BET surface area, rising from 6.8 to 27.5 m²/g, along with improved mesoporosity. TGA results indicate significantly enhanced thermal stability, with Fe3O4 acting as a protective barrier. Electrochemical tests demonstrate high performance, including a specific capacitance of 750.57 F/g at 1 A/g, an energy density of 16.68 Wh/kg, and a power density of 200 W/kg. The composite retains 92.32% capacitance after 5000 cycles and shows low charge-transfer resistance. Moreover, the assembled asymmetric GO-Fe (II)(C40H24N4)@Fe₃O₄//AC supercapacitor exhibits improved energy storage performance as well as excellent cycling stability. These results demonstrate that the incorporation of Fe3O4 is an effective approach for the design of high-performance GO-based electrode materials suitable for next-generation supercapacitors
- Nanobiopesticide based on Cry3Aa@mesoporous silica: improving stability and pesticide activity via support engineering(2026) Estacio-Honrubia, Sara; García Robles, Inmaculada; Rausell Segarra, Carolina; Real García, María Dolores; Robles-Fort, Aida; MLópez-Galiano, María José; Benitez, Miriam; El Haskouri, Jamal; Amorós del Toro, Pedro José; Ros Lis, José VicenteIn this study, a nanobiopesticide based on mesoporous silica was prepared as a support for the Bacillus thuringiensis Cry3Aa protein. The selected support material was UVM-7 silica, which has been demonstrated to possess high accessibility due to its hierarchical bimodal porosity. The functionalisation of the silica with Ce as a heteroelement was achieved through incorporation using the atrane method, resulting in a final molar ratio of Si/Ce =16. The modified support material exhibited a high BET surface area (747 cm3/g) and pore volume (1.02 cm3/g). Ce, which generates CeO2-type nanodomains detected by RAMAN, has a dual role: to increase the local isoelectric point to promote interaction with the Cry3Aa protein and to protect the latter from UV radiation. The nanoencapsulation of the protein does not result in alterations to the organisation and morphology of the support, and is achieved through electrostatic interactions. The efficacy of the material as a biopesticide has been substantiated through experimental testing on the potato pest Leptinotarsa decemlineata (Colorado potato beetle, CPB). It has been observed that materials containing cerium (Ce) have the capacity to retain a greater amount of protein and to provide protection against the degradation of the Cry3Aa protein caused by UV radiation. Consequently, these nanobiopesticides have been demonstrated to result in elevated mortality rates (50 ±7%).
- Azadirachtin-based formulation in combination with mesoporous silica materials as a plague control agent(2025) Benitez, Miriam; El Haskouri, Jamal; Montesinos, Carlos; Amorós del Toro, Pedro José; Ros Lis, José VicenteAzadirachtin is the most important active ingredient of neem oil, a standout product among essential oils. These substances are an interesting family of active products because of their non-toxicity to vertebrates, their specificity against certain pests and the fact that they do not induce resistance. The encapsulation of essential oils and insecticides of natural origin is a widely used strategy to improve their properties. In this work, the ability of silica materials with different topologies and functionalizations to encapsulate and release neem oil and an azadirachtin-based formulation was evaluated. A material containing titanium has also been prepared as a potential protector against UV radiation. It is observed that the presence of the textural pores of the UVM-7 material favors the capture and modulates the release. On the other hand, the mesopores offer a minor contribution. Regarding functionalization, coatings with amine and alkane groups were tested, which did not improve their properties. The UVM-7 material with and without titanium loaded with Zenith A26 was tested in the field against E. banksi in citrus, showing values of incidence and severity close to the conventional treatment with citrulline. Conversely the presence of titanium offered only a minor improvement. Thus, these types of materials could be an interesting approach towards more sustainable agriculture.
- Reproducible strategy to generate ultra-large mesopores in spherical silica particles by chemical etching with triethanolamine(2025) Garrido, M. Dolores; El Haskouri, Jamal; Ros Lis, José Vicente; Amorós del Toro, Pedro JoséThis work presents a simple and reproducible method for obtaining spherical silica particles with expanded mesopores. Porosity can be modulated gradually from small mesopores generated by surfactant micelles (around 2-3 nm) to ultra-large mesopores (ca. 14-15 nm). The methodology is based on a chemical attack of Stöber-type mesoporous silica particles (obtained with CTAB as surfactant) with triethanolamine. The control of simple parameters such as triethanolamine concentration and aging time allows for the modulation of porosity. In the case of short reaction times and/or low triethanolamine concentrations, silicas with hierarchical bimodal porosity are obtained, and a portion of the original mesopores are preserved. However, as the chemical degradation progresses, the original mesopore disappears, and mesoporous silicas with ultra-large pores are obtained. The process occurs without a significant decrease in particle size, accompanied by a degradation in volume, which also exhibits high homogeneity. The underlying principle of the process is the combination of a moderately basic pH generated by triethanolamine and its capacity to interact with Si. The successful expansion of the mesopores facilitates the adsorption of substantial quantities (ca. 400 mg/g) of medium-sized proteins, such as hemoglobin.
- Theoretical study of potential noncanonical photosensitizers of nucleic acids working under hypoxia conditions(2026) Abdelgawwad, Abdelazim; Francés Monerris, Antonio; Roca Sanjuán, Daniel; Escola de DoctoratTraditional anticancer startegies based on chemotherapy and radiotherapy are prone to general and systemic side effects. One strategy to increase selectivity is to use an external stimulus such as light or neutrons to activate the anticancer agent through the so-called photodynamic therapy (PDT), photoactivated chemotherapy (PACT), and boron neutron capture therapy (BNCT) approaches. The molecular mechanisms of these emergent therapies at the atomic and electronic levels, and the key role of dynamic and environmental effects are, however, not completely understood. In this context, the present Thesis contributes to advances the molecular-level understanding of photoinduced DNA damage processes through the application of quantum chemistry, multiscale simulations, molecular dynamics (MD), and QM/MM methodologies. Particular attention was devoted to elucidating the mechanisms of DNA damage induced by organic and metal-based photoactive compounds under biologically relevant conditions. The first system consists of a nitroimidazole derivative which releases a chemotherapeutic agent upon light absorption. The mechanistic investigation of the oxygen-independent pathways for photoinduced DNA damage under hypoxic conditions was performed through multiscale simulations. These demonstrated that these systems are activated either through direct photochemical pathways or via guanine-assisted photoreduction, leading to the formation of highly reactive carbocation intermediates capable of inducing DNA interstrand cross-links. This Thesis has also developed an automated tool to parameterize metal-containing molecules by combining the Amber general force field and quantum-mechanical descriptions. The program, named easyPARM, was developed and extended for the automated parametrization of transition-metal complexes, metalloproteins, Fe-S clusters, and metal-organic polyhedra. It is published free of charge as open source in a GitHub repository. These methodological developments were subsequently applied to investigate the DNA reactivity of Ru(II)-Pt(II) and Os(II)-Pt(II) bimetallic assemblies designed as dual PDT/PACT anticancer agents. QM/MM free-energy calculations demonstrated that photoexcitation significantly accelerates platinum coordination to DNA by lowering the activation barriers associated with Pt–DNA bond formation. Additionally, the interaction mechanism between the boron-rich metallacarborane o-[COSAN]- and DNA was characterized, providing molecular insight into its potential application in BNCT. Finally, modified gemcitabine derivatives incorporating photoactive functionalities were investigated as potential dual chemo-photodynamic agents. The obtained results demonstrated that structural modifications involving heavy atoms and aromatic substituents red-shift the absorption spectrum, enhance intersystem crossing, and increase the population of reactive triplet states. The obtained results not only provide fundamental insight into photo-induced oxygen-independent DNA damage processes, but also in the description of metal-containing molecules, establishing computational protocols and design principles that may facilitate the future development of more selective and effective anticancer therapies.
- Tosylate as a Counter Ion in a Tetra-Aza Macrocycle Complexed by Fe(II) and Co(II) Ions: Spectroscopic Characterization and Modelling by DFT Calculation(2025) Hassouna, Chaima; Agren, Soumaya; Ben Khalifa, Maryem; El Haskouri, Jamal; Ben Chaabane, Rafik; Baouab, Mohamed Hassen V.Herein, we detail the design of a novel tetra-aza macrocyclic Schiff base ligand (A) and its corresponding iron (B, C) and cobalt (D, E) complexes, where chloride (B, D) and tosylate (C, E) counter ions were introduced via streamlined synthetic routes. Comprehensive structural, thermal, and optical characterization revealed the profound influence of metal coordination and counterion substitution on material properties. FTIR and 1H NMR spectra confirmed successful synthesis, while XRD analysis demonstrated enhanced crystallinity in tosylate derivatives (C, D). TGA/DSC studies indicated superior thermal stability in tosylate-substituted complexes (C, E). Theoretical validation via TD-DFT simulations corroborated the structures of (C) and (E), with excellent agreement between experimental and simulated absorption spectra and frontier molecular orbitals (FMOs). MEP analysis further localized nucleophilic density around the metal-nitrogen core due to strong electron withdrawal, while electrophilic regions concentrated on the aromatic rings. Electrochemical data proved that the cobalt-tosylate complex (E) emerged as the most electroactive and reversible species, underscoring its potential utility in redox-active applications.
- Amphoteric Halloysite and Sepiolite Adsorbents by Amino and Carboxy Surface Modification for Effective Removal of Cationic and Anionic Dyes from Water(2025) Boumhidi, Boutaina; Katir, Nadia; El Haskouri, Jamal; Draoui, Khalid; El Kadib, AbdelkrimSurface functionalization is a key enabler that imparts solid materials with excellent chemoselectivity. With this aim, halloysite and sepiolite clay particles were functionalized with carboxyethylsilanetriol sodium salt (CES) and 3-aminopropyltriethoxysilane (APTES), affording carboxy-terminated and amino-terminated clay, respectively. In the case of halloysite, the grafting occurs at Al-OH groups of the lumen surface (tube inner surface) and Al-OH and Si-OH groups at the edges and external surface defects of the nanotubes. For sepiolite, silanol groups located on the edges of the structural channels were at the origin of a chemical reaction between this fibrous clay and the terminal alkoxysilane. The resulting modified clays were examined for removal of Congo red (CR) and malachite green (MG) as anionic and cationic dyes, respectively. Clay bearing only carboxylic groups display more affinity towards cationic dye (MG), recording 926 mgg-1 and 387 mgg-1 for HNT-CES and SEP-CES, respectively, while amino-functionalized clays show very high adsorption for anionic dye (CR), reaching 1232 and 1228 mgg-1 for HNT-APTES and SEP-APTES, respectively. Simultaneous grafting of the two silyl coupling reagents was also attempted through one-pot and sequential grafting method, with the latter being more appropriate to access amphoteric clay featuring both carboxylic and amino groups. The behavior of the bifunctional adsorbents was investigated with respect to pristine and monofunctional clay. The obtained results provide insights to fulfill the requirement for handling complex water effluent containing both anionic and cationic pollutants, towards more sustainable development.
- Investigating the impact of substitution and metal type on the structural, morphological, thermal, and optical properties of newly substituted Schiff base g-C3N4 derivatives(2025) Abbassi, Kaouther; Agren, Soumaya; El Haskouri, Jamal; Beyou, Emmanuel; Baouab, Mohamed Hassen V.This work designs functional g-C3N4 hybrids through substituted Schiff base modification (-OH,-Br, -OCH3,-N (CH3)2) and metal complexation (Co, Cu, Ni, Zn). SEM reveals substituent-driven morphologies: bromo/hydroxy creates microtubes, while-N(CH3)2 yields smooth nanopores. FTIR confirms successful modification via new O-H (3050-3200 cm-1) and C = N (1612 cm-1) vibrations while preserving the heptazine core (1270-1750 cm-1), with metal coordination evidenced by distinct M-O/N bonds (Ni-O at 600 cm-1, Co-O at 619 cm-1). XRD confirms crystallinity enhancement (28-30 degrees peaks) for electron-donating groups, with metal integration preserving matrix integrity. UV-Vis shows substituent-dependent absorption shifts (Delta lambda=30-50 nm) and fluorescence emission modulation via metal coordination. Nickel/cobalt complexes exhibit greater thermal stability than pristine g-C3N4, while copper/zinc produce ultrasmooth surfaces ideal for interfacial applications. Elemental mapping validates uniform metal distribution, revealing metal-substituent-morphology correlations that guide the design of functional surfaces. These hybrids demonstrate how molecular engineering can tailor carbon nitride architectures for specific optoelectronic and catalytic performance
- Targeting Leishmania Fe-SOD and Glucose Metabolism with Tripodal and Pyridinacyclophane Polyamines as a Chemotherapeutic Strategy(2026) Martín Montes, Álvaro; Delgado-Pinar, E.; Bonastre Sabater, Irene; Clares Garcia, M. Paz; Verdejo Viu, Begoña; Martínez Camarena, Álvaro; Ballesteros-Garrido, Rafael; Martín Escolano, Rubén; Rosales-Lombardo, Mª José; Garcia-España Monsonis, Enrique; Marín, ClotildeBackground/Objectives: Many parasitic diseases remain without an effective treatment and cause many deaths worldwide. Leishmaniasis is a complex disease that belongs to the category of Neglected Tropical Diseases, as its treatment relies on outdated drugs that also lead to resistance and negative side-effects. To address this problem, two new chem-ical families have been tested in vitro against three of the most common parasites from the genus Leishmania. Methods: One family is formed by the polyamine tris(2-ami-noethyl)amine functionalised either in one or its three primary amines with different aryl group, and the other is a group of azamacrocyclic cyclophanes containing either one or two aromatic spacers. Results: From the first family, only one compound showed activity against Leishmania donovani, and from the second family, three compounds were selective, two of them for Leishmania braziliensis and a different one against L. donovani, another par-asite of the studied genus. Conclusions: The anti-Leishmania activity seems to be related to the compounds' ability to inhibit the iron superoxide dismutase activity and to alter the parasite metabolism by inhibiting glucose intake in L. braziliensis or by accelerating it in L. donovani and by attacking the parasite defences against ROS, both effects triggering a mitochondrial membrane depolarization that enhances damage, leading to cell death.
- Eco-friendly catalysts: Chitosan-silver hybrid nanocarriers for efficient oxidative coupling of anilines to azobenzenes(2025) Chabbi, Jamal; El Assimia, Taha; Blazic, Roko; El Haskouri, Jamal; Kaddami, Hamid; Ben Youcef, Hicham; Vidovic, Elvira; El Kadib, Abdelkrim; Lahcini, MohammedSustainable, catalytic hybrid nano-carrier (microspheres/films) were synthesized by combining polysaccharides and silver nanoparticles (AgNPs). Chitosan (CS) and microcrystalline cellulose (MCC) acted as stabilizers and reinforcements, respectively, resulting in a bio-composite support with tailored catalytic activity. The hybrid nano-carriers were characterized using various analytical techniques including, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The catalytic performance and stability of the prepared nano-carriers (both microspheres and films) were evaluated in the synthesis of azo compounds. The results demonstrated high catalytic efficiency (up to 90 % conversion) in the production of azobenzene, with good recyclability. This study highlights the potential of chitosan, silver nanoparticles and microcrystalline cellulose as effective components in the development of catalytic nano-carriers for azo compounds synthesis.
- Dual-functional hydrochar via hydrothermal carbonization for norfloxacin removal: Fractal adsorption kinetics and mechanism elucidation(2025) Yazidi, Imane; El Bardiji, Naoual; El Boundati, Youssef; El Haskouri, Jamal; Ziat, Khadija; Allali, Nabil; Sitel, Ferdaous; Chabbi, MohamedEscalating concentrations of norfloxacin (NFX) in surface and wastewaters demand sustainable remediation strategies. In this study, dual-functional hydrochars were synthesized from argan nut shells (ArNS) via hydrothermal carbonization (HTC), with process conditions optimized by varying temperature (150-200°C) and residence time (2-6h). Among the materials, H1:5@150-4-prepared at 150°C for 4h with a biomass-to-water ratio of 1:5-exhibited the best performance, achieving a monolayer NFX adsorption capacity of 27.85mgg--1 at 298K. To describe the adsorption process, equilibrium data were fitted using advanced isotherms, including Generalized Langmuir (GL), Multisite Langmuir (MSL), and the Model of Linear Adsorbates (MLA). The GL model provided the best fit (R2>0.97), reflecting heterogeneous surface binding and deviation from classical monolayer assumptions. For adsorption kinetics, the modified fractal multiexponential model (mod(f-mexp)) demonstrated superior performance, capturing a two-step mechanism with strong R2 values (0.996-0.997) across 298-318K. At 298K, a high rate constant (k1'=0.53min-(1-h)) and fractal exponent (h1=0.61) indicated rapid surface uptake followed by slower diffusion-limited adsorption. To elucidate interaction mechanisms, pH-edge, ethanol disruption, and ionic strength experiments were conducted and complemented by FTIR, XPS, UV-Vis spectroscopy, and Boehm titration. These analyses revealed multiple synergistic pathways-electrostatic attraction, hydrogen bonding, pi-pi electron donor-acceptor (EDA) interactions, and hydrophobic effects-driven primarily by surface chemistry over porosity. Finally, thermal and regeneration studies highlighted the hydrochar's stability and reusability. H1:5@150-4 retained 95% of its initial capacity after one cycle and 77% after five cycles, maintaining effectiveness in real water matrices and under ionic competition. These findings validate HTC-derived, surface-functionalized hydrochars as efficient, sustainable adsorbents for pharmaceutical removal, with broad implications for fractal kinetics and adsorption mechanism design.
- Highly efficient removal of Cr(III) and Ni(II) ions from aqueous solutions using a new hybrid [magnetic graphene oxide/Dialdehyde Nanocellulose] adsorbent(2026) Hassouna, Chaima; Agren, Soumaya; El Haskouri, Jamal; Baouab, Mohamed Hassen V.A novel ternary magnetic nanocomposite, DANC-[GO@Fe3O4], was successfully synthesized via co-precipitation and demonstrated exceptional adsorption performance for Cr(III) removal from water. Characterization confirmed the successful integration of dialdehyde nanocellulose, graphene oxide, and Fe3O4 into a stable, magnetically recoverable adsorbent. Under optimized adsorption parameters (pH 6, 25 ◦C, 6 h, 0.025 g adsorbent in 0.05 L of 250 mg/L Cr(III) solution), DANC-[GO@Fe3O4] attains a notable 98.72% removal efficacity in addition to a high adsorption capacity of 493.60 mg/g, remarkably outperforming non-combined magnetic graphene oxide and dialdehyde nanocellulose adsorbents. Cr(III) adsorption procedure follows pseudo-second- order kinetics (k2 =0.0226 g⋅mg 1⋅h 1, R2 =0.989) and displayed spontaneous character (ΔG◦= 12.48 kJ/mol at 298 K). The equilibrium findings are better fitted by the Freundlich isotherm model (R2 =0.985, KF = 84.0 mg/g, n =1.03), demonstrating multilayer adsorption on a heterogeneous surface. Moreover, DANC- [GO@Fe3O4] exhibits remarkable recyclability, retaining approximately 90% of its primary adsorption performance after six successive runs. Compared to Ni(II), DANC-[GO@Fe3O4] demonstrates better affinity for Cr(III) associated with its relatively reduced ionic radius (62 pm vs 69 pm) and higher coordination capacity with oxygen-containing functional moieties. The collected data highlights the magnetic material's promising capability as a competent, recoverable adsorbent for the depollution Cr(III)-contaminated wastewater. Environmental Implication: The synthesized DANC-[GO@Fe3O4] nanocomposite presents significant environmental benefits by enabling highly efficient removal of Cr(III) from contaminated water, thereby reducing heavy metal pollution and associated ecological risks. Its high adsorption capacity and reusability minimize secondary waste generation and lower treatment costs. The magnetic recoverability further simplifies separation processes, reducing energy and chemical inputs. By integrating sustainable components such as nanocellulose, this material supports greener remediation strategies and offers a promising, eco-friendly solution for wastewater treatment and environmental protection.
- Green synthesis and characterization of trisubstituted imidazole derivatives by an ecofriendly and efficient heterogenous nanocatalyst based on magnetite nanoparticles coated modified nanocellulose(2025) Ben Haj Fraj, Sarah; Agren, Soumaya; El Haskouri, Jamal; Fazio, Enza; Corsaro, Carmelo; Neri, Giovanni; Baouab, Mohamed Hassen V.In the present work, a nanocellulose based magnetic nanocomposite [(pH-PDA-DANC)@Fe(3)O(4)NPs] was synthesized by an ecofriendly and a simple protocol and characterized by means of different techniques such as Fourier-transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Thermal Gravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) equipped with an Energy Dispersive X-ray (EDX) probe and the Value Stream Mapping (VSM). The theoretical study of [(pH-PDA-DANC)@Fe(3)O(4)NPs] was investigated using Density Functional Theory (DFT) at the DFT-D3/ B3LYP/LanL2DZ level of theory to explore the nature of the interactions between the (pH-PDA-DANC) ligand and magnetite nanoparticles. The results indicate that the Fe3O4 nanoparticles form covalent bonds with the N-ring of the ligand. Then, it was used as a catalyst in the green and efficient procedure for one-pot multicomponent syntheses of imidazole derivatives by the condensation of benzil or 9.10-phenanthrenequinone, benzaldehyde derivatives and ammonium acetate. The catalytic reaction provided the synthesis of above imidazole derivatives with high reaction efficiency (80 %-98.1 %) in a short reaction time (3 h) and in presence of a minimum amount of ethanol. The identification and structure of imidazole derivatives was determined analyzing the H-1 NMR (Nuclear Magnetic Resonance) and FTIR spectra. This procedure has several advantages compared to the conventional method such as the high yields, short reaction times, easy separation of the nanocatayst from the reaction mixture by using a magnet, and the reusability of the catalyst.
- An innovative magnetic L-lysine-dialdehyde nanocellulose for sonochemical heterogeneous catalysis in the green synthesis of ultrapure tri-substituted imidazoles(2025) Agren, Soumaya; Mehdaoui, Rahma; Chaabene, Marwa; El Haskouri, Jamal; Beyou, Emmanuel; Baouab, Mohamed Hassen V.In this contribution, we report the first ultrasound-assisted synthesis of magnetically modified L-lysine dialdehyde nanocellulose and its use in an efficient ecological catalytic application. The structure of designed nanomaterial [Lys-g-DANC)@Fe3O4] was successfully elucidated using various structural, morphological, thermal, optical and magnetic techniques. Next, it was utilized as a heterogeneous nano-catalyst in an ecofriendly and effective process following one-pot multicomponent synthesis of tri-substituted imidazoles. The catalytic procedure afforded seven imidazole byproducts in outstanding yields (83.45-97.13 %) using ultrasound irradiation, 0.03 g of [Lys-g-DANC)@Fe3O4], 10 mL of ethanol at 45 degrees C and in limited time ranges (1.5-3 h). The structures of obtained imidazole derivatives were elucidated using FTIR and NMR spectroscopic techniques. This work proves the efficiency of magnetically L-lysine nanocellulose in catalytic procedures compared to classical heating protocols including increased yields, limited reaction time ranges, simple catalyst separation and its effective recyclability.
- Sustainable core-shell structures derived from lignin for Na ion batteries(2025) Miralda Jalle, Judith; El Haskouri, Jamal; Moraes Leite, Marina; Kennedy, Tadhg; Culebras Rubio, Mario; Collins, Maurice N.The aromatic nature of the structure of lignin enables its use as a natural and sustainable hard carbon precursor. Upon carbonisation, lignin-derived hard carbon has shown potential as a sodium-ion battery anode. In this study, we have utilised coaxial electrospinning to produce nanofibers, which undergo stabilisation and carbonisation, to analyse the influence of carbon morphology on sodium-ion storage mechanisms. Various nanostructures have been tailored to produce intricate core/shell structures with varying degrees of porosity to allow controlled Na diffusion and storage. The morphology of these unique high surface area nanostructures has been assessed by scanning electron microscopy. The optimized Core-Shell structure shows a specific capacity of 184.7mAh g(-1), with 99.7 % of coulombic efficiency. This innovative and green approach enables new strategies to obtain sustainable materials for sodium ion energy storage applications
- New Methods for the Synthesis of Highly Fluorescently Substituted Heterocyclic Boranils: Structural Identification and Photophysical Properties(2025) Agren, Soumaya; El Haskouri, Jamal; Beyou, Emmanuel; Baouab, Mohamed Hassen V.We report the synthesis, structural, thermal, and photophysical properties of six boranils ((A-F)-BF2). Compounds (A-C)-BF2 were synthesized at low temperature, while nitro and pyridine derivatives were obtained at 80°C with yields up to 66%. Tert-butyl and chloro-substituted boranils showed thermal stability up to 300 °C. All boranils were fluorescent, with properties tuned by phenyl substitution and boron difluoride complexation. The lowest energetic gap (2.210 eV) was found in (D-BF2), which exhibited a remarkable red-shift in absorption and emission due to charge transfer between donor and acceptor groups. This work is part of ongoing studies on metal cation detection and photocatalysis.
- Innovative adsorption of lead and copper using recycled concrete in aqueous solutions(2025) Ferhat, Hiba; Maachou, Radia; Benaissa, Sihem; Mebarek-Haddad, Safia; Lefkir, Abdelouahab; Gómez, Clara M.; El Haskouri, Jamal; Amrane, Abdeltif; Berrahou, GhezlaneThe main objective of this study was to investigate the potential use of concrete debris generated from construction and demolition waste at the Technical Landfill Centre (TLC) for eliminating copper and lead ions from synthetic solutions. To assess its suitability, the physicochemical characteristics of the debris were thoroughly examined, including its cation exchange capacity (CEC) and pH at the zero-charge point (pH PZC). Various characterization methods were employed, such as Fourier-transform infrared spectroscopy (FTIR) to predict the functional groups. X-ray diffraction (XRD) was applied to determine the crystalline structure of the materials and identify the phases present, while BET surface area analysis and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM/EDX) were also used to gain a comprehensive understanding of the concrete debris. Key parameters evaluated included solution pH, initial metal ion concentration, adsorbent mass, stirring speed, and temperature, all analyzed to determine their influence on adsorption capacity. Optimal removal conditions were identified as pH 5.5 for lead and pH 5 for copper, with agitation speeds of 300 and 400 rpm, contact times of 20 and 15 min, and adsorbent masses of 0.3 and 0.4 g for copper and lead, respectively. Furthermore, A kinetic analysis of adsorption was conducted to identify the mechanisms of the process by fitting experimental data to various models. Additionally, different isotherms were utilized to accurately fit the equilibrium adsorption. The results indicate that adsorption is best represented by the Langmuir model. The use of thermodynamics in the removal process revealed that this procedure was endothermic and spontaneous.
- From Structure to Signal: Optical Tuning of New g-C3N4 Schiff Bases for Metal Ion Sensing(2025) Abbassi, Kaouther; Agren, Soumaya; El Haskouri, Jamal; Beyou, Emmanuel; Baouab, Mohamed Hassen V.This study reports the design of g-C3N4-based polymeric chemosensors functionalized with Schiff base derivatives formed by condensing g-C3N4 with three structurally distinct aromatic aldehydes. The aim is to explore how aldehyde substituents and conjugation influence the structural, thermal, and optical properties of the resulting materials. FTIR confirmed imine linkage formation, while UV-Vis and fluorescence studies revealed solvent-dependent optical shifts and variable emission intensities. g-Ald-B (hydroxy-naphthalene) and g-Ald-C (pyrene) exhibited strong fluorescence, in contrast to the weakly emissive nitro-substituted g-Ald-A. All derivatives showed selective fluorogenic or colorimetric responses to Zn2+, Cu2+, Co2+, and Ni2+ ions. Notably, g-Ald-B displayed the highest affinity for Zn2+ (Ka ≈ 6.2 × 104 M-1) and the lowest detection limit (0.06 µM), demonstrating its high sensitivity. These results highlight the potential of structurally tuned Schiff base-modified g-C3N4 as versatile and efficient multi-ion sensors.
