One-pot Method For Preparation Research Articles

Rod-shaped Mo(vi) trichalcogenide–Mo(vi) oxide decorated on poly(1-H pyrrole) as a promising nanocomposite photoelectrode for green hydrogen generation from sewage water with high efficiency

Abstract The synthesis of rod-shaped Mo(vi) trichalcogenide–Mo(vi) oxide, cleverly adorned on a poly(1-H pyrrole) (P1HP) matrix (MoS3–MoO3/P1HP), is achieved through a one-pot preparation method. This process occurs under the pyrrole oxidation employing the oxidizing agent Na2MoO4. Notably, this oxidation process facilitates the direct incorporation of the inorganic constituents into the polymer matrix. Of particular significance is the material’s bandgap, which is optimally situated at 1.4 eV, rendering it highly suitable for its intended applications. The material assumes a rod-like structure, characterized by an average length of 400 nm and width of 30 nm, further enhancing its desirability. In practice, this thin film serves as an exceptionally promising photoelectrode. It finds its forte in the generation of hydrogen from sewage water, achieving an impressive efficiency rate of 12.66%, specifically at 340 nm. In addition to that, it boasts a remarkable hydrogen generation rate of 1.2 moles·h−1·cm−2. Moreover, the material exhibits remarkable versatility in its response to light. Its sensitivity to monochromatic light across a broad optical spectrum (UV till IR), underscores its potential for hydrogen generation applications for industrial applications.

Thermo-compression process-mediated in-situ cellulose microfibers phosphorylation enables high performant cellulosic paper packaging

With the increasing demand for environmentally friendly alternatives to traditional plastic packaging, the development of sustainable cellulosic-based materials has become a strategic research topic. In this concept, a groundbreaking approach was adopted herein to produce phosphorylated cellulose microfibers (CMFs)-based paper packaging via a one-pot preparation step using a thermo-compression process (150 °C under pression for 45 min) in the presence of diammonium hydrogen phosphate ((NH4)2HPO4, denoted DAP) and urea. This process involves a chemical mechanism leading to the production of phosphorylated cellulosic paper with a very compacted structure induced by the hornification phenomenon. This phenomenon reveals the formation of additional and irreversible strong hydrogen bonds leading thus to an increase of the materials’ crystallinity up to 91%, and to an enhancement of their morphological, thermal stability, flame retardancy, hydrophobicity, water vapor permeability, and mechanical strength properties. To further enhance these properties, and thus their potential applications, the as-produced phosphorylated CMF paper samples were then coated with a thin layer (40 ± 1.11 µm) of poly[ethylene-co-(vinyl acetate)] (EVA) polymer. A comparison of collected properties with those from non-phosphorylated CMFs or from materials prepared using the conventional phosphorylation process clearly demonstrates that the proposed one-pot preparation method led to the production of advanced materials more effective for packaging applications. Overall, the findings associated to this work could be used as a proof-of-concept for the development of sustainable packaging materials, which could be made by following a more efficient and cost-effective manufacturing procedure than current benchmarks.

One-pot preparation of mannan-coated antigen nanoparticles using human serum albumin as a matrix for tolerance induction

Nanoparticles (NPs) for allergen immunotherapy have garnered attention for their high efficiency and safety compared with naked antigen proteins. In this work, we present mannan-coated protein NPs, incorporating antigen proteins for antigen-specific tolerance induction. The heat-induced formation of protein NPs is a one-pot preparation method and can be applied to various proteins. Here, the NPs were formed spontaneously via heat denaturation of three component proteins: an antigen protein, human serum albumin (HSA) as a matrix protein, and mannoprotein (MAN) as a targeting ligand for dendritic cells (DCs). HSA is non-immunogenic, therefore suitable as a matrix protein, while MAN coats the surface of the NP. We applied this method to various antigen proteins and found that the self-disperse after heat denaturation was a requirement for incorporation into the NPs. We also established that the NPs could target DCs, and the incorporation of rapamycin into the NPs enhanced the induction of a tolerogenic phenotype of DC. The MAN coating provided steric hindrance and heat denaturation destroyed recognition structures, successfully preventing anti-antigen antibody binding, indicating the NPs may avoid anaphylaxis induction. The MAN-coated NPs proposed here, prepared by a simple method, have the potential for effective and safe allergies treatment for various antigens.

Sample Preparation Methods for Targeted Single-Cell Proteomics.

We compared three cell isolation and two proteomic sample preparation methods for single-cell and near-single-cell analysis. Whole blood was used to quantify hemoglobin (Hb) and glycated-Hb (gly-Hb) in erythrocytes using targeted mass spectrometry and stable isotope-labeled standard peptides. Each method differed in cell isolation and sample preparation as follows: 1) FACS and automated preparation in one-pot for trace samples (autoPOTS); 2) limited dilution via microscopy and a novel rapid one-pot sample preparation method that circumvented the need for the solid-phase extraction, low-volume liquid handling instrumentation and humidified incubation chamber; and 3) CellenONE-based cell isolation and the same one-pot sample preparation method used for limited dilution. Only the CellenONE device routinely isolated single-cells from which Hb was measured to be 540-660 amol per red blood cell (RBC), which was comparable to the calculated SI reference range for mean corpuscular hemoglobin (390-540 amol/RBC). FACSAria sorter and limited dilution could routinely isolate single-digit cell numbers, to reliably quantify CMV-Hb heterogeneity. Finally, we observed that repeated measures, using 5-25 RBCs obtained from N = 10 blood donors, could be used as an alternative and more efficient strategy than single RBC analysis to measure protein heterogeneity, which revealed multimodal distribution, unique for each individual.

Glucose oxidase-loaded colloidal stable WS2 nanobowls for combined starvation/photothermal therapy of colorectal tumors

Glucose is used as an important nutrient to support cell growth. The glucose oxidase (GOx) can transform glucose into gluconic acid and toxic H2O2, which can be used for tumor starvation therapy. However, the leakage of GOx may cause severe side effects to the normal tissue. To prevent the accidental leakage of GOx, this study proposes the chemical modification of GOx on the photothermal transducing agent surface, to realize the safe and combined starvation and photothermal therapy of colorectal tumors. Polyvinylpyrrolidone (PVP)-modified WS2 nanobowls (WS2-PVP) as a photothermal transducing agent were produced using a one-pot preparation method. Then, α-lipoic acid (LA) molecules were immobilized at the sulfur-deficient sites on the surface of WS2 nanobowls to afford the chemical loading of GOx through amide bonds. Under the irradiation of a near-infrared laser (808 nm), thermal energy is generated by WS2 to kill colorectal cancer cells locally. The photothermal conversion efficiency of WS2-PVP-LA was 27.2%. This study is anticipated to open up an alternative avenue for the rational design of multifunctional nanotherapeutics for tumor therapy.

Studying the optical and thermal properties of Cs/ZnO and Cs/ZnO/GO hybrid nanocomposites

Green nanotechnology, defined as the synthesis or hybridization of nanomaterials with natural bioactive compounds, is a low-cost, eco-friendly, easy-to-manage and non-toxic technology. Nanocomposites have recently gained attention due to their unique characteristics and applications in the fabrication of microelectronic circuits, sensors, piezoelectric devices, optoelectronic components, fuel cells, corrosion surface passivation coatings, and catalysts. Accordingly, chitosan (Cs), a bioactive polymer, was hybridized with nanomaterials including ZnO and graphene oxide (GO) utilizing two easy, eco sustainable, and low-cost methods of preparation. All samples were analyzed using different analytical techniques. The FTIR and NMR results confirmed that the interaction between Cs, ZnO and GO occurs through the NH2 function group of Cs with ZnO and the O of the carboxyl group COOH of GO. Furthermore, the SEM data show the agglomeration generated by ZnO and GO on the Cs surface. According to the optical characterization of hybrid Cs/ZnO/GO, the one-pot preparation method achieves the lowest indirect and direct optical band gap values of 0.176 and 3.18 eV, respectively. Furthermore, it has a larger Eu = 5.46 eV value than the other samples, indicating a higher degree of disorder and high conductivity. Finally, the TGA results showed that hybridization of Cs with ZnO and Go improved the temperature decomposition and degradation of Cs by 79.9%. As a result, the one-pot approach for creating CS/ZnO/GO hybrid nanocomposite is effective for preparing Cs/ZnO/GO as an optoelectronic material.

Development of an enrichment-free one-pot sample preparation and ultra-high performance liquid chromatography-tandem mass spectrometry method to identify Immunoglobulin A1 hinge region O-glycoforms for Immunoglobulin A nephropathy

Immunoglobulin A nephropathy (IgAN) is a highly prevalent autoimmune renal disease. Human IgA1 with galactose deficiency in the hinge region (HR) has been identified as an autoantigen for this disease. Therefore, analyzing IgA1 HR glycoforms in biofluids is important for biomarker discovery. Herein, an analytical method that includes one-pot sample preparation with unbiased plasma IgA purification, dual internal standard addition, and sensitive ultra-high-performance liquid chromatography-triple quadrupole tandem mass spectroscopy (UHPLC-QqQ-MS/MS) was developed. Targeted O-glycopeptides detection was performed in pooled plasma with the validation of theoretical retention times, enzymatic treatment outcomes, product ion scans, and signal repeatability. A total of 42 IgA1 O-glycopeptides with N-acetylgalactosamines, galactoses, and sialic acids were determined from 8 µL of plasma. The newly developed method was applied to plasma samples from 16 non-IgAN controls and 19 IgAN patients. Comparing the 42 targets, 16 IgA1 HR O-glycopeptides were statistically different between the two groups (p<0.05). Decreased sialylation was identified in the IgA1 hinge region of IgAN patients, which was also correlated with the estimated glomerular filtration rate (eGFR). The developed method is sensitive and precise and can be used to identify plasma biomarkers for IgA nephropathy.

One-pot production of a graft copolymer of cationic starch and cationic polyacrylamide applicable as flocculant for wastewater treatment

A newly developed, high-performance, and environmentally friendly flocculant, i.e., a graft copolymer of cationic starch and cationic polyacrylamide (SC-CPAM), is synthesized via a single-step pathway in which the cationic agent is incorporated onto the starch backbone and into the polyacrylamide grafted branch simultaneously. One-pot preparation method is quick, reproducible, and easily scalable, which yields high-quality products with better flocculation performance than conventional cationic starch (SC) and starch-graft-polyacrylamide (S-PAM). The synthesized samples are characterized by physicochemical techniques, namely Fourier Transform Infrared Spectroscopy (FTIR), elemental analysis, H1 Nuclear Magnetic Resonance (H1NMR) Spectroscopy, Zeta Potential (ZP), and Dynamic light scattering (DLS). The application as a flocculant for wastewater treatment is investigated by flocculation of kaolinite suspension and analysis of turbidity (UV-Vis and NTU), ZP, and floc size in neutral pH. A high clarification of 97.8%, low turbidity of 1.97 NTU, and large floc size of 136 µm, obtained by SC-CPAM, are believed to result from dual flocculation mechanisms, i.e., polymer charge patch and particle bridging, enabled by the cationic high molecular weight branched bio-based flocculant for wastewater purification applications.

One-pot Preparation of CoS/CuS Nanocomposite-sensitized TiO2 Nanorod Arrays with Enhanced Photoelectrochemical Performance

Transition metal sulfides are widely used for the modification of TiO2 to improve its light absorption range due to their small bandgaps. In this work, novel CoS/CuS/TiO2 was synthesized via a simple one-pot hydrothermal preparation method. Using various characterization techniques, CoS/CuS/TiO2 was found to demonstrate excellent photoelectrochemical performance and photocatalytic activity for the degradation of tetracycline hydrochloride. The CoS/CuS/TiO2 catalyst showcased a maximum photocurrent density of 55 μA cm−2, which was 7.8 times higher than that of unmodified TiO2 nanorods. Under visible light irradiation using Xe lamp, the photocatalytic degradation efficiency of CoS/CuS/TiO2 on tetracycline hydrochloride was found to be significantly improved, where it recorded an excellent degradation rate of 64.0% at 90 min. The charge transfer mechanism of the proposed material was also investigated.

Potential one-pot synthesis of spherical magnesium silicate powder by mechanical milling

Synthetic magnesium silicate finds applications in adsorbents, catalysis, pharmaceuticals, foods, cosmetics, and in oil industry. This study introduces a method for potential one-pot preparation of narrowly sized, spherical magnesium silicate powders. After initial synthesis by precipitation from magnesium sulphate and sodium metasilicate solutions, the magnesium silicate precursor was ball-milled with two immiscible liquids, forming a particle-loaded emulsion. Hexane formed the continuous phase; the droplet phase was formed by either acetonitrile, methanol, or water-methanol mixtures. Suspended precursor particles were refined, their fragments became trapped in the droplets, where they were eventually compacted into composite spheres. Prepared spherical powders were characterized using scanning electron microscopy, nitrogen sorption, and low angle laser light scattering. The synthesized powders exhibited narrow size distributions with modes from 3.3 to 92 μm. The spherical powders showed an enhanced flowability and had specific surface areas comparable to or higher than the precipitated precursor powders.

High-performance FeOOH quantum dots: A novel one-pot microemulsion method for fast preparation and adsorption kinetics

As an emerging material, FeOOH quantum dots (QDs) are being used for their applications in the photodegradation of organic pollutants. However, as a promising adsorbent for the removal of dyes from aqueous solution, their adsorption performance has not yet been studied, and the fabrication of FeOOH QDs typically involves a time-consuming process. To improve its preparation efficiency, a one-pot microemulsion method for the fast fabrication of FeOOH quantum dots was successfully developed, by which FeOOH QDs of approximately 5 nm were successfully prepared within 30 min. The as-synthesized FeOOH QDs were characterized by XRD, XPS, BET, HR-TEM, and AFM. The adsorption properties of the FeOOH QDs for methyl orange (MO) were investigated, and the adsorption mechanism was studied via adsorption kinetics and adsorption isotherms. The results indicated that the adsorption of MO onto FeOOH QDs was a chemisorption process that follows the Langmuir isotherm. The FeOOH QDs possess a high BET surface area of 97.24 m2/g and can achieve a maximum adsorption capacity (qm) of 167.22 mg/g for MO, as estimated by the Langmuir isotherm. The adsorption performance of FeOOH QDs is better in acidic solution than it is in basic solution, and the FeOOH QDs show good stability and reusability.

A facile one-pot method for preparation of succinic esters containing several functional groups

A facile one-pot method for preparation of succinic esters containing several functional groups

One-pot method for preparation of capsaicin-containing double-network hydrogels for marine antifouling.

Marine biofouling which interferes with normal marine operation and also causes huge economic loss has become a worldwide problem. With the development of society, there is an urgent need to develop non-toxic and efficient anti-fouling strategies. Capsaicin is an environmentally friendly antifouling agent, but controlling the stable release of capsaicin from the coating is still a challenge to be solved. To achieve long-lasting antifouling property, in this work, we incorporate a derivative of capsaicin N-(4-hydroxy-3-methoxybenzyl)acrylamide (HMBA) to prepare double network (DN) hydrogels and make HMBA a part of the polymer network. Polyvinyl alcohol (PVA) has good hydrophilicity, and as a soft and ductile network, acrylamide (AM) and HMBA can polymerize to generate a rigid and brittle network. By adjusting the content of HMBA in the DN hydrogels, we can obtain a PVA–PAHX hydrogel with high mechanical strength, low swelling rate, and excellent antifouling effect, which provides a feasible way for the practical application of a hydrogel coating in long-term marine antifouling.

Solution combustion derived oxygen vacancy-rich Co3O4 catalysts for catalytic formaldehyde oxidation at room temperature.

Fabricating abundant oxygen vacancies is crucial for non-noble metal oxides to catalyze formaldehyde (HCHO) oxidation at room temperature. Here, a simple one-pot preparation method via solution combustion was found to produce oxygen vacancy-rich Co3O4 catalysts, avoiding delicate defect engineering. The catalyst was evaluated to result in 52% HCHO conversion in a dynamic flow reaction with ∼6 ppm HCHO, which was higher as compared to some other Co3O4 catalysts prepared in three methods of sol–gel, deposition precipitation and thermal decomposition. The optimal catalyst also exhibited high durability with steady HCHO conversion (∼47%) for more than 50 h. The catalyst characterizations revealed that the explosive solution combustion brought out two particular features of Co3O4, namely, the porous network structure with nano-holes and the abundant oxygen vacancies. The latter was demonstrated to increase the reactive oxygen species and to improve the reducibility and the oxygen transport capacity of Co3O4. The two features and the derived properties are beneficial to the activity and durability of Co3O4. The solution combustion method can serve as a simple and feasible way to fabricate abundant oxygen vacancies to provide room-temperature activity of Co3O4 for HCHO elimination at room temperature.

Safe, Flexible, and High-Performing Gel-Polymer Electrolyte for Rechargeable Lithium Metal Batteries

The use of gel polymer electrolytes (GPEs) is of great interest to build high-performing rechargeable lithium metal batteries (LMBs) owing to the combination of good electrochemical properties and improved safety. Herein, we report a facile and scalable one-pot preparation method of a GPE based on highly safe polyethylene glycol dimethyl ether (PEGDME) plasticizer in a poly(vinylidenefluoride-co-hexafluoropropylene) (PVDF-HFP) polymer matrix. The prepared GPE exhibits excellent safety (nonflammability and thermal stability up to 250 °C) and outstanding electrochemical properties at room temperature (high ionic conductivity of 3.4 × 10–4 S cm–1 and high lithium transference number). Moreover, high loading LiFePO4 (6–7 mg cm–2) LMB using such GPE delivers a good C-rate response and high capacity (ca. 1 mAh cm–2 at C/10) with an excellent retention of 98% after 60 cycles in coin cell configuration. Notably, the prototype pouch cell (ca. 19 mAh at C/10) provides remarkable safety, mechanical flexibility, and strong tolerance toward bending and cutting. These results suggest that the prepared GPE is a promising candidate for the development of high performance, flexible, and safe LMBs that operate at room temperature, as well as for other energy storage systems beyond lithium-ion technologies.

Influence of Carbon Content in Ni-Doped Mo2C Catalysts on CO Hydrogenation to Mixed Alcohol

Herein, we synthesize the Ni-doped Mo2C catalysts by a one-pot preparation method to illuminate the effect of the number of carbon atoms in Mo2C lattice on CO hydrogenation to mixed alcohol. The Ni doping inhibits the agglomeration of Mo2C crystals into large particles and the surface carbon deposition, which increase the active surface area. In addition, the interaction between Ni and Mo increases the electron cloud density of Mo species and promotes the non-dissociative adsorption and insertion of CO. Especially, our results indicate that with the increase of the nickel content, the number of carbon atoms in Mo2C lattice on the surface of the catalyst shows a volcano type variation. The low carbon content induces the formation of coordination unsaturated molybdenum species which exhibit the higher catalytic activity and mixed alcohol selectivity than other molybdenum species. Among the catalysts, the MC-Ni-1.5 catalyst with Ni/Mo molar ratio of 1.5:8.5, which has the largest amount of coordination unsaturated molybdenum species, shows the highest space-time yield of mixed alcohols, which is three times higher than that of the Mo2C catalyst.

Facile synthesis of muscovite–supported Fe3O4 nanoparticles as an adsorbent and heterogeneous catalyst for effective removal of methyl orange: Characterisation, modelling, and mechanism

The discharge of organic pollutants including dyes into the aquatic system represents a main source of environmental contamination. Decontamination of dye molecules from polluted water bodies through adsorption process is reported to be an effective and economic technology. Herein, a one-pot preparation method was used to decorate the available and low-cost layered silicate muscovite (MUS) mica by iron oxide (Fe3O4) nanoparticles. The new Fe3O4@MUS composite was characterised by XRD, FTIR, SEM, and TEM techniques and tested for the adsorption and Fenton-like degradation of hazardous methyl orange (MO). The results of experimental parameters such as reaction time, Fe3O4@MUS mass, MO concentration, solution pH, H2O2 concentration, and temperature indicated that Fenton-like oxidation process was rapid (i.e., around 98 % of MO removal was achieved after 60 min). The pseudo-first-order for kinetics and Langmuir for equilibrium models fitted the MO adsorption data. The maximum Langmuir uptake capacity of Fe3O4@MUS presented the value of 149.25 mg/g at 25°C. Fenton-like degradation data followed the first-order removal rate at varied initial concentrations (i.e., 50, 100, and 150 mg/L) of MO dye. Electrostatic interactions, hydrogen bonding, and the π-π bond (i.e., dye‒dye interaction) were involved during MO adsorption onto Fe3O4@MUS surface. Degradation of MO was mainly associated with the generation of •OH radicals through H2O2 catalytic decomposition using Fe3O4@MUS composite. The synthetic catalyst was reused up to five runs without an apparent decrease in its removal efficiency even after 5th use, reflecting the high stability of Fe3O4@MUS.

Morphology controlled synthesis of 2D heterostructure Ag/WO3 nanocomposites for enhanced photoelectrochemical CO2 reduction performance

Supporting nanomaterials having strong metal-support interaction is the key to an efficient catalyst. The present paper describes a morphology-controlled synthesis of silver (Ag) nanoparticles supported on nanostructured tungsten oxide (WO3) for selective photoelectrocatalytic carbon dioxide reduction reactions (CO2RR) under visible light irradiation. Highly dispersed Ag on WO3 nanorod was synthesized by a one-pot preparation method in the presence of cetyltrimethylammonium bromide (CTAB). The synthesis strategy remained intact and reproduced by varying loading of Ag, which was further confirmed by various characterization techniques like XRD, SEM, TEM, STEM elemental mapping, Raman, XPS, FT-IR, and BET analysis. The morphological growth of the WO3 nanorod (NR) and the related mechanism was studied and discussed in the paper. 1.5 wt % Ag showed optimum loading for high dispersion over WO3-NR and efficient CO2RR with high current density (0.4 mA cm−2), towards the desired selective product formation (formic acid). The efficiency of the catalyst was further correlated with cluster vacancies on the interface of Ag particle and WO3 nanorod by positron doppler broadening (DB) spectroscopy.

ZnO@graphene oxide core@shell nanoparticles prepared via one-pot approach based on laser ablation in water

Core-shell nanoparticles (NPs) have attracted tremendous attention due to their tunable properties and numerous potential applications. However, preparation of uniform and size-controlled core-shell nanomaterials of ZnO with graphene oxide (GO) is still considered as a challenging task even after years of research. In this work, we report on a facile one-pot organics-free method for preparation of GO-wrapped ZnO NPs. Laser ablation of zinc and carbon targets in water medium at ambient atmosphere resulted in formation of spherical ZnO core and GO shell, respectively. According to Raman active modes, the GO shell was layered and the ZnO core was polycrystalline. Both Raman spectra and X-ray diffraction patterns revealed that formation of layered GO increased stress inside the ZnO core. Surface layers reduced the density of defects and disorders in the ZnO crystal lattice and enhanced the phonon lifetime. Also, the minimal interfacial disorder between the layered GO and ZnO core resulted in continuous formation of a GO layer. Thus, laser ablation in liquid is demonstrated to provide stable and uniform core-shell GO@ZnO NPs with controlled GO layer that can find applications in biomedical and sensing fields.

Metal ion-promoted fabrication of melanin-like poly(L-DOPA) nanoparticles for photothermal actuation

Melanin-inspired polymers are currently the focus of growing interest for a wide range of applications ranging from energy to biomedical area. Whilst researchers have made numerous attempts to prepare and utilize polydopamine nanoparticles (PDA NPs), they have made limited progress in developing and discovering another typical functional mimic of natural melanin, poly (levodopa) (P(L-DOPA)) NPs, probably due to the lack of facile synthetic strategies towards satisfactory structural and functional control of melanin-like NPs. Herein, we reported a one-pot preparation method towards P(L-DOPA) NPs with good yields and controllable size/property in an aqueous solution assisted by various metal ions (i.e., Ni(II), Mg(II), Ca(II), Fe(III), Mn(II), Co (II), Zn(II) and Cd(II)). Interestingly, the resulting P(L-DOPA) NPs exhibited enhanced light absorption and photothermal behaviors compared with well-established PDA NPs, which can be employed to further fabricate kinds of photothermal composite actuators with promising performances such as folding, switching, and forward-moving. This study offers a facile and robust way to synthesize new synthetic melanins beyond PDA, and facilitates further functional discovery and evolution of melanin-inspired polymers and composites.