Bryophyte-Bioinspired Nanoporous AAO/C/MgO Composite for Enhanced CO2 Capture: The Role of MgO.

A composite material composed of anodized aluminum oxide (AAO), carbon (C), and magnesium oxide (MgO) was developed for CO2 capture applications. Inspired by the bryophyte organism, the AAO/C/MgO composite mirrors two primary features of these species-(1) morphological characteristics and (2) elemental composition-specifically carbon, oxygen, and magnesium. The synthesis process involved two sequential steps: electroanodization of aluminum foil followed by a hydrothermal method using a mixture of glucose and magnesium chloride (MgCl2). The concentration of MgCl2 was systematically varied as the sole experimental variable across five levels-1 mM, 2 mM, 3 mM, 4 mM, and 5 mM-to investigate the impact of MgO formation on the samples' chemical and physical properties, and consequently, their CO2 capture efficiency. Thus, scanning electron microscopy analysis revealed the AAO substrate's porous structure, with pore diameters measuring 250 ± 30 nm. The growth of MgO on the AAO substrate resulted in spherical structures, whose diameter expanded from 15 nm ± 3 nm to 1000 nm ± 250 nm with increasing MgCl2 concentration from the minor to major concentrations explored, respectively. X-ray photoelectron spectroscopy (XPS) analysis indicated that carbon serves as a linking agent between AAO and MgO within the composite. Notably, the composite synthesized with a 4 mM MgCl2 concentration exhibited the highest CO2 capture efficiency, as determined by UV-Vis absorbance studies using a sodium carbonate solution as the CO2 source. This efficiency was quantified with a 'k' constant of 0.10531, significantly higher than those of other studied samples. The superior performance of the 4 mM MgCl2 sample in CO2 capture is likely due to the optimal density of MgO structures formed on the sample's surface, enhancing its adsorptive capabilities as suggested by the XPS results.

Al/SBA-15 Mesoporous Material: A Study of pH Influence over Aluminum Insertion into the Framework.

Herein, ordered mesoporous materials like SBA-15 and Al/SBA-15 were prepared using the pH adjustment method. Thus, these materials were developed in different pH of synthesis, from the pH adjustment method using a KCl/HCl solution and varying the Si/Al molar ratio (5, 25, and 75). All the ordered mesoporous materials were characterized by FRX, 27Al NMR, SEM, XRD, N2 adsorption/desorption, and CO2 adsorption. From the applied method, it was possible to obtain SBA-15 and Al/SBA-15 with high mesoscopic ordering based on the XRD patterns, independent of the pH employed. From the chemical composition, the insertion of higher amounts of Al into the synthesis caused a progressive improvement in the structural and textural properties of the ordered mesoporous materials. Thus, the chosen synthesis conditions can lead to different aluminum coordination (tetrahedral and octahedral), which gives these materials a greater potential to be applied. The presence of Al in high amounts provides material with the ability to form micropores. Finally, the proposed method proved to be innovative; low-cost; less aggressive to the environment, with efficient insertion of aluminum in the framework of SBA-15 mesoporous material; and practical, based on only one step.

Phase stabilization and optical response in the ultraviolet range, due to terbium concentration in hafnium oxide nanoparticles.

This work reports the influence of terbium trivalent ions on growing kinetics and the phase in hafnium oxide nanoparticles, as well as response to radiation in the range from 256 to 286. The nanoparticles were obtained by the hydrothermal route maintaining the temperature constant and varying the reaction time and the terbium concentration. The results show a gradual change in the phase with the concentration of terbium trivalent ions, going from the monoclinic phase, present at low concentrations, to the tetragonal phase, which appears from dopant concentrations greater than 5% at., increasing in amount with concentration of dopant. These phases appear as two perfectly defined morphologies. Furthermore, there is a significant change in radiative lifetimes when the tetragonal phase appears.

Facile Preparation of SrZr1-xTixO3 and SrTi1-xZrxO3 Fine Particles Assisted by Dehydration of Zr4+ and Ti4+ Gels under Hydrothermal Conditions.

In recent decades, perovskite-type compounds (ABB'O3) have been exhaustively studied due to their unique ferroelectric properties. In this work, a systematic study aiming to prepare fine particles in the binary system SrZrO3-SrTiO3 was conducted under hydrothermal conditions in a KOH (5 M) solution at 200 °C for 4 h under a constant stirring speed of 130 rpm. The precursors employed were SrSO4 powder (<38 µm size) and coprecipitated hydrous gels of Zr(OH)4•9.64 H2O (Zr-gel) and Ti(OH)4•4.5H2O (Ti-gel), which were mixed according to the stoichiometry of the SrZr1-xTixO3 in the compositional range of 0.0 > x > 100.0 mol% Ti4+. The XRD results revealed the formation of two crystalline phases rich in Zr4+, an orthorhombic structured SrZr0.93Ti0.07O3 and a cubic structured SrZr0.75Ti0.25O3 within the compositional range of 0.1-0.5 mol of Ti4+. A cubic perovskite structured solid solution, SrTi1-xZrxO3, was preferentially formed within the compositional range of 0.5 > x > 0.1 mol% Ti4+. The SrZrO3 and SrZr0.93Ti0.07O3-rich phases had particle sizes averaging 3 µm with a cubic morphology. However, a remarkable reduction in the particle size occurred on solid solutions prepared with hydrous Ti-gel over contents of 15 mol% Ti4+ in the reaction media, resulting in the formation of nanosized particle agglomerates with a cuboidal shape self-assembled via a 3D hierarchical architecture, and the sizes of these particles varied in the range between 141.0 and 175.5 nm. The limited coarsening of the particles is discussed based on the Zr-gel and Ti-gel dehydration capability differences that occurred under hydrothermal processing.

Green nanoarchitectonics of carbon quantum dots from Cinchona Pubescens Vahl as targeted and controlled drug cancer nanocarrier.

Carbon quantum dots (CQDs) are a new carbon-based nanomaterial that has attracted tremendous attention due to their excellent fluorescent properties, chemical stability, water solubility, and biocompatibility features. Here, fluorescent CQDs synthesized by a green nanoarchitectonic method using Cinchona Pubescens Vahl extract were evaluated as drug nanocarriers for carboplatin (CBP) delivery. The characterization methods showed CQDs with semispherical shapes and sizes around 5 nm, temperature- and pH-dependent functional groups that interact with the CBP molecule adding specificity to the drug-delivery system. Based on the load efficiency results, it seems that the CQDs can carry almost 100 µg of carboplatin for every 1 mg of CQDs. This is possible due to the self-assembly process that takes place through the interaction between the protonation/deprotonation functional groups of CQDs and the hydrolyzed CBP molecule. Through this process, it is created spherical nanoparticles with an average size of 77.44 nm. The CQDs-CBP nanoparticles release the drug through a diffusion-controlled release mechanism where the acidic media is preferred, and the EPR effect also plays a helpful role. Besides, the viability test shows that the CQDs have almost null cytotoxicity suggesting that they could be used as a promising cancer treatment, improving the efficiency of cell internalization and significantly increasing their drug delivery.

From Waste to Added-Value Product: Synthesis of Highly Crystalline LTA Zeolite from Ore Mining Tailings.

The use of wastes is necessary to contribute to environmental sustainability. In this study, ore mining tailings were used as the raw material and precursor for the synthesis of LTA zeolite, a value-added product. Pre-treated mining tailings were submitted to the synthesis stages under specific established operational conditions. The physicochemical characterization of the synthesized products was performed with XRF, XRD, FTIR and SEM, to identify the most cost-effective synthesis condition. The LTA zeolite quantification and its crystallinity were determined as effects of the SiO2/Al2O3, Na2O/SiO2 and H2O/Na2O molar ratios used, as well as the influence of the synthesis conditions: mining tailing calcination temperature, homogenization, aging and hydrothermal treatment times. The zeolites obtained from the mining tailings were characterized by the LTA zeolite phase accompanied by sodalite. The calcination of mining tailings favored the production of LTA zeolite, and the influence of the molar ratios, aging and hydrothermal treatment times were determined. Highly crystalline LTA zeolite was obtained in the synthesized product at optimized conditions. Higher methylene blue adsorption capacity was associated with the highest crystallinity of synthesized LTA zeolite. The synthesized products were characterized by a well-defined cubic morphology of LTA zeolite and lepispheres of sodalite. The incorporation of lithium hydroxide nanoparticles over LTA zeolite synthesized (ZA-Li+) from mining tailings yielded a material with improved features. The adsorption capacity towards cationic dye was higher than for anionic dye, especially for methylene blue. The potential of using ZA-Li+ in environmental applications related to methylene blue deserves detailed study.

Hydrothermal Synthesis and Properties of Nanostructured Silica Containing Lanthanide Type Ln-SiO2 (Ln = La, Ce, Pr, Nd, Eu, Gd, Dy, Yb, Lu).

The nanostructured lanthanide-silica materials of the Ln-SiO2 type (Ln = La, Ce, Pr, Nd, Eu, Gd, Dy, Yb, Lu) were synthesized by the hydrothermal method at 100 °C, using cetyltrimethylammonium as a structural template, silica gel and sodium silicate as a source of silicon, and lanthanide oxides, with Si/Ln molar ratio = 50. The resulting materials were calcined at 500 °C using nitrogen and air, and characterized by X-ray diffraction (XRD), Fourier-Transform infrared absorption spectroscopy, scanning electron microscopy, thermogravimetry (TG), surface area by the BET method and acidity measurements by n-butylamine adsorption. The XRD and chemical analysis indicated that the SiO2 presented a hexagonal structure and the incorporation of lanthanides in the structure changes the properties of the Ln-SiO2 materials. The heavier the lanthanide element, the higher the Si/Ln ratio. The TG curves showed that the decomposition of the structural template occurs in the materials at temperatures below 500 °C. The samples showed variations in specific surface area, mean pore diameter and silica wall thickness, depending on the nature of the lanthanide. The incorporation of different lanthanides in the silica generated acid sites of varied strength. The hydrothermal stability of the Ln-SiO2 materials evaluated at high temperatures, evidenced that the properties can be controlled for application in adsorption and catalysis processes.

Chitosan-Based Carbon Dots with Applied Aspects: New Frontiers of International Interest in a Material of Marine Origin.

Carbon dots (CDs) have attracted significant research attention worldwide due to their unique properties and advantageous attributes, such as superior optical properties, biocompatibility, easy surface functionalization, and more. Moreover, biomass-derived CDs have attracted much attention because of their additional advantages related to more environmentally friendly and lower-cost synthesis. In this respect, chitosan has been recently explored for the preparation of CDs, which in comparison to other natural precursors exhibited additional advantages. Beyond the benefits related to the eco-friendly and abundant nature of chitosan, using it as a nanomaterial precursor offers additional benefits in terms of structure, morphology, and dopant elements. Furthermore, the high content of nitrogen in chitosan allows it to be used as a single carbon and nitrogen precursor for the preparation of N-doped CDs, significantly improving their fluorescent properties and, therefore, their performances. This review addresses the most recent advances in chitosan-based CDs with a special focus on synthesis methods, enhanced properties, and their applications in different fields, including biomedicine, the environment, and food packaging. Finally, this work also addresses the key challenges to be overcome to propose future perspectives and research to unlock their great potential for practical applications.

Boosting photovoltaic performance for Sb2S3solar cells by ionic liquid-assisted hydrothermal synthesis.

Bulk and surface trap-states in the Sb2S3films are considered one of the crucial energy loss mechanisms for achieving high photovoltaic performance in planar Sb2S3solar cells. Because ionic liquid additives offer interesting physicochemical properties to control the synthesis of inorganic material, in this work we propose the addition of 1-Butyl-3-methylimidazolium hydrogen sulfate (BMIMHS) into a Sb2S3hydrothermal precursor solution as a facile way to fabricate low-defect Sb2S3solar cells. Lower presence of small particles on the surface, as well as higher crystallinity are demonstrated in the BMIMHS-assisted Sb2S3films. Moreover, analyses of dark current density-voltageJ-Vcurves, surface photovoltage transient and intensity-modulated photocurrent spectroscopy have suggested that adding BMIMHS results in high-quality Sb2S3films and a successful defect passivation. Consequently, the best-performing BMIMHS-assisted device exhibits a 15.4% power conversion efficiency enhancement compared to that of control device. These findings show that ionic liquid BMIMHS can effectively be used to obtain high-quality Sb2S3films with low-defects and improved optoelectronic properties.

Advances in Engineered Metal Oxide Thin Films by Low-Cost, Solution-Based Techniques for Green Hydrogen Production.

Functional oxide materials have become crucial in the continuous development of various fields, including those for energy applications. In this aspect, the synthesis of nanomaterials for low-cost green hydrogen production represents a huge challenge that needs to be overcome to move toward the next generation of efficient systems and devices. This perspective presents a critical assessment of hydrothermal and polymeric precursor methods as potential approaches to designing photoelectrodes for future industrial implementation. The main conditions that can affect the photoanode's physical and chemical characteristics, such as morphology, particle size, defects chemistry, dimensionality, and crystal orientation, and how they influence the photoelectrochemical performance are highlighted in this report. Strategies to tune and engineer photoelectrode and an outlook for developing efficient solar-to-hydrogen conversion using an inexpensive and stable material will also be addressed.

Hydrothermal Synthesis of Silicoaluminophosphate with AEL Structure Using a Residue of Fluorescent Lamps as Starting Material.

Silicoaluminophosphate molecular sieves of SAPO-11 type (AEL structure) were synthesized by the hydrothermal method, from the residue of a fluorescent lamp as a source or Si, Al, and P in the presence of water and di-propyamine (DPA) as an organic template. To adjust the P2O5/SiO2 and Si/Al and ratios, specific amounts of silica, alumina, or alumina hydroxide and orthophosphoric acid were added to obtain a gel with molar chemical composition 1.0 Al2O3:1.0 P2O5:1.2 DPA:0.3 SiO2:120 H2O. The syntheses were carried out at a temperature of 473 K at crystallization times of 24, 48, and 72 h. The fluorescent lamp residue and the obtained samples were characterized by X-ray fluorescence, X-ray diffraction, scanning electron microscopy, and BET surface area analysis using nitrogen adsorption isotherms. The presence of fluorapatite was detected as the main crystalline phase in the residue, jointly with considered amounts of silica, alumina, and phosphorus in oxide forms. The SAPO-11 prepared using aluminum hydroxide as Al source, P2O5/SiO2 molar ratio of 3.6 and Si/Al ratio of 0.14, at crystallization time of 72 h, achieves a yield of 75% with a surface area of 113 m2/g, showing that the residue from a fluorescent lamp is an alternative source for development of new materials based on Si, Al, and P.

One-Pot Hydrothermal Synthesis of Victoria Green (Ca3Cr2Si3O12) Nanoparticles in Alkaline Fluids and Its Colour Hue Characterisation.

One-pot hydrothermal preparation of Ca3Cr2Si3O12 uvarovite nanoparticles under alkaline conditions was investigated for the first time. The experimental parameters selected for the study considered the concentration of the KOH solvent solution (0.01 to 5.0 M), the agitation of the autoclave (50 rpm), and the nominal content of Si4+ (2.2-3.0 mole). Fine uvarovite particles were synthesised at 200 °C after a 3 h interval in a highly concentrated 5.0 M KOH solution. The crystallisation of single-phase Ca3Cr2Si3O12 particles proceeded free of by-products via a one-pot process involving a single-step reaction. KOH solutions below 2.5 M and water hindered the crystallisation of the Ca3Cr2Si3O12 particles. The hydrothermal treatments carried out with stirring (50 rpm) and non-stirring triggered the crystallisation of irregular anhedral particles with average sizes of 8.05 and 12.25 nm, respectively. These particles spontaneously assembled into popcorn-shaped agglomerates with sizes varying from 66 to 156 nm. All the powders prepared by the present method exhibited CIE-L*a*b* values that correspond to the Victoria green colour spectral space and have a high near infrared reflectance property. The particle size and structural crystallinity are factors affecting the Victoria pigment optical properties, such as CIE-L*a*b* values, green tonality, and near-infrared reflectance.

Fabrication of electrospun poly(lactic acid) nanoporous membrane loaded with niobium pentoxide nanoparticles as a potential scaffold for biomaterial applications.

Tissue engineering aims to regenerate and restore damaged human organs and tissues using scaffolds that can mimic the native tissues. The requirement for modern and efficient biomaterials that are capable of accelerating the healing process has been considerably increased. In this work, a novel electrospun poly(lactic acid) (PLA) nanoporous membrane incorporated with niobium pentoxide nanoparticles (Nb2 O5 ) for biomaterial applications was developed. Nb2 O5 nanoparticles were obtained by microwave-assisted hydrothermal synthesis, and different concentrations (0, 1, 3, and 5% wt/wt) were tested. Chemical, morphological, mechanical, and biological properties of membranes were evaluated. Cell viability results demonstrated that the membranes presented nontoxic effects. The incorporation of Nb2 O5 improved cell proliferation without impairing the wettability, porosity, and mechanical properties of membranes. Membranes containing Nb2 O5 nanoparticles presented biocompatible properties with suitable porosity, which facilitated cell attachment and proliferation while allowing diffusion of oxygen and nutrients. This study has demonstrated that Nb2 O5 nanoparticle-loaded electrospun PLA nanoporous membranes are potential candidates for drug delivery and wound dressing applications.

Electrochemical Hydrogen Evolution over Hydrothermally Synthesized Re-Doped MoS2 Flower-Like Microspheres.

In this research, we report a simple hydrothermal synthesis to prepare rhenium (Re)- doped MoS2 flower-like microspheres and the tuning of their structural, electronic, and electrocatalytic properties by modulating the insertion of Re. The obtained compounds were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Structural, morphological, and chemical analyses confirmed the synthesis of poorly crystalline Re-doped MoS2 flower-like microspheres composed of few stacked layers. They exhibit enhanced hydrogen evolution reaction (HER) performance with low overpotential of 210 mV at current density of 10 mA/cm2, with a small Tafel slope of 78 mV/dec. The enhanced catalytic HER performance can be ascribed to activation of MoS2 basal planes and by reduction in charge transfer resistance during HER upon doping.

Síntese hidrotérmica de zeólitas a partir de cinza volante de carvão mineral: aplicação na adsorção de íon amônio / Hydrothermal synthesis of zeolites from fly ash of mineral coal: application of ion ammonium adsorption

RESUMO A cinza volante é o principal resíduo industrial do uso de carvão mineral na geração de vapor e energia. No Brasil, são produzidas 1,4 milhão toneladas ao ano. Essas cinzas podem ser convertidas em produtos zeolíticos por tratamento hidrotérmico alcalino. Este trabalho teve como objetivo principal realizar essa conversão hidrotérmica, a fim de obter unicamente fases cristalinas zeolíticas para a adsorção de íon amônio. Realizaram-se diversas sínteses alterando o método utilizado (clássico ou de duas fases), o tempo de reação (24 ou 30 h) e a massa de NaOH. A caracterização dos produtos e da cinza (in natura e calcinada) foi realizada por difratometria de raios X, microscopia eletrônica de varredura e, em alguns casos, análises térmica diferencial e gravimétrica (ATD-TG). Os resultados demonstraram que é possível sintetizar as zeólitas hidroxissodalita e cancrinita a partir da cinza estudada. O produto obtido pelo método de duas etapas foi utilizado na adsorção de íon amônio em solução, sendo, neste processo, o modelo isotérmico de Sips o mais adequado; alcançando um valor de capacidade máxima de adsorção de 2,71 mg.g-1.

ABSTRACT Fly ash is the main industrial waste generated by coal in steam and power plans. In Brazil, 1,4 million tons are produced every year. These ashes can be converted into zeolite products by alkaline hydrothermal treatment. The main objective of this paper was to induce this reaction which produces only zeolitic crystalline phases for ammonium ion absorption. So, some syntheses were done by different hydrothermal method (classical or two stages), work time (24 or 30 h) and many NaOH bulks. The characterization of ash (in natura and calcined) and products was performed by X-ray diffraction method, scanning electron microscopy and, in some cases, differential thermal and thermogravimetric analysis The product by two stages method was used in ammonium ion absorption in solution at Sips Mathematic Model: the highest capacity of 2,71 mg.g-1.

Blue or red photoluminescence emission in α-Bi2 O3 needles: Effect of synthesis method.

Monoclinic bismuth oxide (α-Bi2 O3 ) has attractive optical properties and, therefore, its photoluminescence (PL) behavior has been increasingly explored. Besides this fact, the influence of synthesis methods on PL properties of α-Bi2 O3 still requires research. This paper describes the influence of precipitation (PPT) and microwave-assisted hydrothermal (MAH) methods on PL properties of acicular α-Bi2 O3 microcrystals. The synthesis method promoted structural modifications on α-Bi2 O3 , in particular PPT increased the density of oxygen vacancies significantly. As a result, the PL properties of samples were different depending on the method of synthesis. PPT samples presented their maximum PL emission at 1.91 eV (red), while MAH samples had their maximum at 2.61 eV (blue). These results indicate the possibility of controlling PL properties of α-Bi2 O3 by simply choosing the adequate synthesis method.

Modulation of antibiotic effect by Fe2(MoO4)3 microstrutures.

In this study, we report the antibacterial activity and modulation of antibiotic activity by Fe2(MoO4)3 microstructures obtained by the hydrothermal route without use of surfactants or organic additives. This material was characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM) images. The XRD pattern showed that the Fe2(MoO4)3 crystallize in a monoclinic structure without secondary phases. Raman spectroscopy confirms the formation of Fe2(MoO4)3. SEM images show that the Fe2(MoO4)3 obtained have ball-of-yarn shaped morphology. In the antibacterial assays, strains of Escherichia coli, Pseudomonas aeruginosa and Staphylococcus aureus were assayed by microdilution method to evaluate the antibacterial and modulatory-antibiotic activity with antibiotics as gentamicin, norfloxacin and imipenem. Against all bacteria, the Minimum Inhibitory Concentration (MIC) was Fe2(MoO4)3 ≥ 1024 µg/mL. This high MIC result must be associated with the fact of the iron be an essential microelement to the bacterial growth. However, when the Fe2(MoO4)3 was assayed in association with the antibiotics was observed an antagonistic effect demonstrated by an enhance of the MIC. This fact is associated directly with the pro-oxidative properties of metallic oxides. These compounds enhance the production of free radicals, as H2O2 and superoxide ions that can affect the cell structures as cell membrane and cell wall. Other effect is associated with the possible coordination of the metal, performing bonds with the chemical structure of the antibiotics, reducing their activity. Our results indicated that nanocompounds as Fe2(MoO4)3 can not be used as antimicrobial products for clinical usage, neither directly and neither in association with antibiotics.

Antiangiogenic evaluation of ZnWO4 nanoparticles synthesised through microwave-assisted hydrothermal method.

Angiogenesis, the complex process of formation of new blood vessels from pre-existing blood vessels, which involves the participation of several pro- and anti-angiogenic factors, is implicated in many physiological and pathological conditions. Nanoparticle-based anti-angiogenic activity at the tumour tissue, harnessed by the Enhanced Permeability and Retention Effect (EPR effect), could potentially become a breakthrough therapy to halt tumour progression. Herein, we evaluate the anti-angiogenic effect of ZnWO4 nanoparticles (NPs). The nanoparticles were obtained by microwave-assisted hydrothermal synthesis (MAHS) at 120 °C for 60 min and were structurally characterised by X-ray diffraction (XRD) and micro-Raman (MR) spectroscopy. The mean size and polydispersity index were estimated by Zeta potential analysis. The XRD analysis revealed structural organisation at a long-range order, with an average crystallite size of around 3.67 nm, while MR revealed short-range order for ZnWO4. The anti-angiogenic potential of zinc tungstate nanoparticles was investigated through the chorioallantoic membrane assay (CAM) using fertilised chicken eggs. We demonstrate, in an unprecedented way, that nanocrystalline ZnWO4 NPs obtained by MAHS, at low reaction temperatures, showed excellent anti-angiogenic properties even at low concentrations. The ZnWO4 NPs were further evaluated for its cytotoxicity in vitro.

Hybrid Organic-Inorganic Anatase as a Bifunctional Catalyst for Enhanced Production of 5-Hydroxymethylfurfural from Glucose in Water.

Hybrid organic-inorganic anatase (hybrid-TiO2 ) is prepared by a facile hydrothermal synthesis method employing citric acid. The synthetic approach results in a high surface-area nanocrystalline anatase polymorph of TiO2 . The uncalcined hybrid-TiO2 is directly studied as a catalyst for the conversion of glucose into 5-hydroxymethylfurfural (HMF). In the presence of the hybrid-TiO2 , HMF yields up to 45 % at glucose conversions up to 75 % were achieved in water at 130 °C in a monophasic batch reactor. As identified by Ti K-edge XANES, hybrid-TiO2 contains a large fraction of fivefold coordinatively unsaturated TiIV sites, which act as the Lewis acid catalyst for the conversion of glucose into fructose. As citric acid is anchored in the structure of hybrid-TiO2 , carboxylate groups seem to catalyze the sequential conversion of fructose into HMF. The fate of citric acid bound to anatase and the TiIV Lewis acid sites throughout recycling experiments is also investigated. In a broader context, this contribution outlines the importance of hydrothermal synthesis for the creation of water-resistant Lewis acid sites for the conversion of sugars. Importantly, the use of the hybrid-TiO2 with no calcination step contributes to dramatically decreasing the energy consumption in the catalyst preparation.