Facile Synthesis Research Articles

Facile synthesis of Metal-Organic Framework/Chitosan cryogel as a robust Scavenger for Diclofenac sodium

Diclofenac sodium (DS), a commonly detected contaminant in aquatic environments, poses a a significant risk to both the ecological balance and the safety of aquatic products. Therefore, efficient removal of DS from water is ergently needed but remains a major challenge. In this study, an environmentally friendly Fe-based metal–organic framework/chitosan (NH2-MIL-53(Fe)/CS) cryogel was prepared through a Schiff base condensation reaction under mild conditions. Taking advantage of the catalytic role of the MOF in accelerating the reaction between CS and 1,3,5-triformylphloroglucinol, NH2-MIL-53(Fe) powders were incorporated into the polymeric networks within 30 s. Owing to the rich binding sites, the resulting NH2-MIL-53(Fe)/CS cryogel demonstrated remarkable efficacy in eliminating DS from water. The adsorption process reached equilibrium within 120 min with a maximum adsorption capacity of 728.6 mg g−1. A comprehensive mechanistic investigation revealed that the exceptional adsorption capability of the NH2-MIL-53(Fe)/CS cryogel for DS was attributed to the synergistic effect of multiple interactions, including favorable hydrophilicity, electrostatic forces, π-π stacking, hydrogen bonding, and coordination. Thus, this study provides a straightforward and rapid synthesis route for MOF/CS cryogel, offering a promising adsorbent that combines exceptional adsorption performance with ease of separation. The resulting MOF/CS cryogel holds great potential for the treatment of DS-contaminated wastewater.

Facile synthesis of CoFe/C nanoparticle embedded in nitrogen and sulfur co-doped reduced graphene oxide nanocomposites for electromagnetic wave absorption

Three-dimensional metal–organic framework derivatives (MOFs) offer significant potential for the absorption of electromagnetic waves (EMW). However, the discrepancy in impedance matching restricts their ability to absorb EMW efficiently. This study synthesized a novel composite material, CoFe/C@N, S-rGO, by combining diazo coupling reactions, solvothermal techniques, and high-temperature pyrolysis. The composite consists of cobalt iron/carbon (CoFe/C) nanoparticles embedded in N and S co-doped reduced graphene oxide (N, S-rGO). The co-doping of N and S on graphene oxide (SGO) resulted in numerous defects and disordered sites, which generated interfacial and dipole polarization. The EMW absorption characteristics of the CoFe/C@N, S-rGO can be tuned by varying the quantity of SGO added. Notably, at an SGO concentration of 60 mg, the produced composite exhibits a minimal reflection loss of −53.8 dB, while a thickness of 4.0 mm yields an effective absorption bandwidth of 7.2 GHz. This material’s exceptional EMW absorption capabilities are primarily attributed to interface polarization, multiple reflections, dipole polarization, natural resonance, and eddy current loss. The findings of this study provide a potential solution for enhancing the impedance matching and electromagnetic wave absorption performance of MOFs.

Facile synthesis of geopolymer-based hierarchical porous materials for efficient adsorption-photocatalysis of dye wastewater

Facile synthesis of geopolymer-based hierarchical porous materials for efficient adsorption-photocatalysis of dye wastewater

Facile synthesis of substituted 2-styrylnaphthyridine and its derivatives via sp3C-H functionalization under mild conditions and their antimicrobial activity and Electrochemical properties.

Metal-free, synthetic approach for the Efficient synthesis of pyrazole, imidazopyridine based substituted 2-styryl-1,8-naphthyridines has developed via sp3 C-H activation of substituted 7-methyl-1,8-naphthyridines, with various aromatic/heteroaromatic aldehydes through knoevenagel condensation under mild basic (Piperidine) conditions. Further, the synthesized titled molecules tested their absorption and emission spectra, interestingly compound 3d was found to be that inspiring emission spectra at 626 nm (red shift) with impressive stokes shift 133 nm. Moreover, some of the best resultant conjugate scaffolds (compounds 3c, 3d, 3e, and 4e) analysed their electrochemical properties, thus, 3c, 3d, 3e, and 4e molecules respectively displaying medium to good redox potentials (compound 3e displays 0.3, -1.71 V respectively) and tested scanning rate (from 50 to 500 mV s−1) also. Furtherly, all synthsized derivatives analysed their biological activity, i.e., antifungal and antifungal. Among that, the compounds 3c, 3d, 3e, 3i, 3k, 3l, 5c, 5d and 5f were established excellent inhibition zone of activity against standard drugs.

Facile synthesis of hierarchical CuO flowers with superior photocatalytic activity and supercapacitor performance

Facile synthesis of hierarchical CuO flowers with superior photocatalytic activity and supercapacitor performance

Facile Synthesis of Highly Supercapacitive Mo‐doped Titanium Nanotube Arrays and Effect of Anodization Voltage

AbstractDesigning potential architectures by the modification of conventional electrode materials is an effective approach in the development of high performance supercapacitor electrodes. The present study investigated the effect of varying anodization voltages (50, 75, and 100 V) on the morphology and electrochemical properties of titanium nanotubes (TNT). Molybdenum was doped onto TNT using a simple hydrothermal procedure, followed by thermal treatment at 450 °C. The study effectively demonstrated control over the dimensions of the nanotube structure by adjusting the anodization voltage. Additionally, it was found that the tube diameters were increased due to etching during the hydrothermal treatment with the Mo precursor, which potentially enhanced the supercapacitive performance of Mo‐doped TNT. Further, structural analysis revealed that Mo doping improved both crystallinity and electrode stability. With an optimal anodization voltage of 100 V, TNT and Molybdenum‐doped TNT could exhibit capacitance value of 13.34 and 326.54 mF cm−2 respectively, at a current density of 1 mA cm−2. Furthermore, the electrode demonstrated good cyclic stability with 88% capacitance retention and 97% coulombic efficiency after 5000 cycles. An impressive energy density of 87.03 µWh cm−2 and a power density of 799.99 µW cm−2 could be achieved with this sample in an asymmetrical device.

Facile synthesis of polyhedral oligomeric silsesquioxanes with excellent thermosetting, fibrous and crystalline properties

The development of multifunctional polyhedral oligomeric silsesquioxanes (POSS) that are more serialized than traditional POSS is essential to reduce the economic investment and expand the category of high-performance POSS. This work employed a simple one-step method to synthesize a series of different physical states of methacryloxypropyl-phenyl POSS (AcPhPOSS). The FTIR, NMR and MS results showed that the products were mainly composed of regular T8, T10 and T12 cage-like structures, and the outer periphery of the AcPhPOSS cage carried different proportions of flexible methacryloxypropyl (R1) and rigid phenyl (R2) groups. In addition, the curable, fibrous, and crystalline properties of liquid, semi-solid, and powder AcPhPOSS were studied through thermal curing, electrospinning, and crystallization methods, respectively. The results showed that AcPhPOSS in three different states, especially AcPhPOSS@1:0 (liquid), AcPhPOSS@1:3 (semi-solid) and AcPhPOSS@0:1 (powder), exhibited good thermal curing properties, fiber and crystallization, respectively. Hence, this work proposes a facile strategy for producing multifunctional materials with good curing properties, fiber-forming properties, and crystallinity, which have broad application potential in thermosetting resins, fiber materials, and single crystal materials.

Facile synthesis of novel nitrogen-doped diamond with excellent microwave absorption and thermal conductive performance

Facile synthesis of novel nitrogen-doped diamond with excellent microwave absorption and thermal conductive performance

Lanthanide coordination polymers as luminescent laccase mimics for ratiometric sensing of dopamine

Some metal ions, with inner enzyme-like catalytic activity, could be doped into lanthanide coordination polymers (Ln CPs) through coordination, which has been proved as a facile strategy to prepare the luminescent nanozymes. In this study, Cu-doped Ln CPs with laccase-mimic activity and double luminescence were rationally designed and synthesized by self-assembly of guanine monophosphate (GMP), 2-aminoterephthalic acid (ATA), Cu2+ and Tb3+ in buffer solution at room temperature. The obtained probes Tb/Cu-GMP/ATA CPs not only emitted green fluorescence of Tb3+ and blue fluorescence of ATA simultaneously under irradiation at the same wavelength, but also processed enhanced laccase-like activity for catalyzing the oxidation of phenolic substrates. Upon dopamine (DA), the probes catalyzed the oxidation of DA to polydopamine (PDA), which effectively quenched the fluorescence of Tb3+ due to the internal filtration effect. Based on this, a ratiometric fluorescent sensor for DA was constructed accordingly, and the corresponding fluorescence intensity ratio of Tb3+to ATA (F547/F427) was linearly correlated with the DA concentration in the range of 1 to 400 μM, with a detection limit of 0.44 μM. Besides, this sensor could be used to detect DA in human serum samples with good recovery, which results were highly consistent with that of HPLC method. The constituent and luminescence tunability, as well as the extraordinarily facile synthesis, made Ln CPs a potential platform for designing and preparing the integrated multifunctional probe for special target in sensing applications.

Prussian Blue Nanocages as Efficient Radical Scavengers and Photothermal Agents for Reducing amyloid-beta Induced Neurotoxicity

The unusual accumulation of amyloid-beta 1–42 (Aβ42) is an essential pathological feature of Alzheimer’s disease (AD), and development of Aβ42 nanomodulators offers a potentially therapeutic approach to AD. Here, we report facile synthesis of the hollow mesocrystalline Prussian blue nanocages (HMPBs), which serve as versatile Aβ42 modulators. Due to the hollow nanostructures and large specific surface area, they can effectively inhibit Aβ42 aggregation by adsorption. They also exhibit robust near-infrared (NIR) photothermal effect for light-to-heat transition, which promotes the depolymerization of Aβ42 fibers. Besides, they display ROS quenching ability to scavenge hydroxyl radicals (•OH) caused by Aβ42 fibers, alleviate cellular oxidative stress, and improve cell survival. This work provides a new kind of Prussian blue nanomaterial for multimodal Aβ modulation.

Programmable Piperazine Synthesis via Organic Photoredox Catalysis.

Piperazine cores have long been identified as privileged scaffolds in the development of pharmaceutical compounds. Despite this, the facile synthesis of diverse C-substituted piperazines remains a challenge without prefunctionalized substrates/cores. Herein, we describe a programmable approach to highly diversifiable piperazine cores, which circumvents the typical need for radical precursors. The use of organic photoredox catalysis renders this method operationally simple, as direct substrate oxidation followed by 6-endo-trig radical cyclization with in situ generated imines may furnish the product. Additionally, the photoredox-catalyzed anti-Markovnikov hydroamination of readily accessible ene-carbamates provides a modular approach to functionalized diamine starting materials which are shown to generate more complex piperazine cores. A wide range of both carbonyl and amine condensation partners were shown to be compatible with this system in good to excellent yield.

Facile synthesis of novel soy protein-based flame retardant and its effects on the flame retardancy and biodegradation of polylactic acid

Facile synthesis of novel soy protein-based flame retardant and its effects on the flame retardancy and biodegradation of polylactic acid

Modification of MWCNTs with Bi2WO6 nanoparticles targeting IL-1β and NLRP3 inflammasome via augmented autophagy.

This study reports the facile hydrothermal synthesis of pure Bi2WO6 and Bi2WO6\MWCNTs nanocomposite at specific molar ratio 1:2.5 of Bi2WO6:MWCNTs and elucidates their role in modulating the NLRP3 inflammasome pathway via autophagy induction. Comprehensive characterization techniques, including XRD, Raman, UV.Vis PL,FESEM,EDS and TEM, revealed the successful incorporation of MWCNTs into the Bi2WO6 structures, leading to enhanced crystattlinity, reduced band gap energy (2.4 eV) suppressed charge carrier recombination and mitigated nanoparticles aggregation. Notably, the reduced band gap facikitaed improved visible light harvesting, a crucial attribute for photocatalytic applications. Significantly, the nanocompsoite exhibited a remarkable capacity to augment autophagy in bone marrow-derived macrophages (BMDMs), consequently down-regulating the NLRP3 inflammasom activation and IL-1β secretion upon LPS and ATP stimulation. Immunofluorescence assays unveiled increased co-localization of LC3 and NLRP3, suggestion enhanced targeting of NLRP3 by autophagy. Inhibition of autophagy by 3-MA reversed these effects, confirming the pivotal role of autophagy induction. Furthermore, the nanocomposite attenuated caspase-1 activation and ASC oligomerzation, thereby impeding inflammasome assembly. Collectively, these findings underscore the potential of Bi2WO6\MWCNTs nanocompsite as a multifaceted therapeutic platform, levering its tailored optoelectronic properties and sbility to modulate the NLRP3 infalmmasome via autophagy augmentation. This work covers the way for the development of advanced nanomaterials with tunable functionalities for combating inflammatory disorders and antimicrobial applications.

A facile one-pot synthesis of hierarchical porous carbon for supercapacitor electrodes

This study presents a facile, environmentally friendly approach to fabricate hierarchical porous carbon for supercapacitor electrodes. The one-pot synthesis of PFO/silica/PTFE via co-pyrolysis generates ideal hierarchical porous carbon. Compared with traditional methods, this method eliminates toxic solvents and complex cleaning steps. PPC-2 obtained under the optimized activation time has the highest specific surface area (2657 m2 g−1) and a remarkable total pore volume (2.96 cm3 g−1). These properties result in a remarkable specific capacitance of 335.9–210.8 F g−1 at current densities of 0.5–10 A g−1 in KOH electrolyte. The electrochemical performance of the PPC-2 electrode in a symmetric supercapacitor device was measured in aqueous (6 M KOH) and ionic liquid (EMIM-TFSI) electrolytes. In EMIM-TFSI, PPC-2//PPC-2 provides an energy density of 48.5 Wh/kg even at a power density of 750 W kg−1. This facile one-pot synthesis method offers a sustainable and scalable approach to produce high-performance hierarchical porous carbon for supercapacitor applications.

Green solvents assisted de-novo synthesis and defect-engineered UiO-66 for improved CO2 adsorption and kinetics- experimental and DFT approach

The CO2 concentration in the atmosphere is increasing at an alarming rate, which is causing distress to human society and the natural environment. Adsorption is one of the most widely used methods of removing CO2 from flue gases, which reduces its adverse effects on our environment. For adsorption purposes, a facile green solvent-assisted de-novo synthesis approach was developed to construct a UiO-66′s structure to target CO2 at low pressure due to the partial pressure of CO2 in flue gases in the atmosphere (0.01⁓0.02 MPa). In the de-novo synthesis approach, a combination of various types of modulators and deep eutectic solvents (DES) are utilized to graft structural defects and induce quantitative and dispersive deep eutectic solvents onto the UiO-66 structure, respectively. The green solvent-assisted de-novo synthesis approach helped to tune all three structural parameters and preserve extra open metal sites (Lewis acid and Bronsted basis sites) with active NH2 and OH groups for improved CO2 adsorption and kinetics under flue gas conditions (CO2/N2=15/85 %). In comparison to the parent UiO-66, de-novo synthesized ChClPropx5@UiO-66 showed increased CO2 uptake (65.04 mg g-1) by 73 % at 0.15 bar and 25 °C, and the cyclic capacity remained almost similar over 10 consecutive cycles with an almost 94 % retention rate. After 3 times of regeneration at 105 °C under N2 atmosphere, the sample reserved almost similar adsorption capacity and could be recycled without dropping CO2 uptake. The strong and rapid interaction between guest CO2 and de-novo synthesized UiO-66 was confirmed by pseudo-first-order and second-order kinetics with reaction rate constants of 0.00026 and 0.00259, respectively. Furthermore, through periodic Density Functional Theory (DFT) calculations, a variety of linker defects are engineered onto the UiO-66 structure to preserve more open metal sites. For each of the engineering defects, free energies, adsorption energies, and the interaction of CO2 molecules on defect structures with bond length (Ɩ, Å) and bond angle (θ˚) are calculated for the most stable structures of UiO-66.

Experimental Realization of Fluoroborophene.

Borophene, an anisotropic metallic Dirac material exhibits superlative physical and chemical properties. While the lack of bandgap restricts its electronic chip applications, insufficient charge carrier density and electrochemical/catalytically active sites, restricts its energy storage and catalysis applications. Fluorination of borophene can induce bandgap and yield local electron injection within its crystallographic lattice. Herein, a facile synthesis of fluoroborophene with tunable fluorine content through potassium fluoride-assisted solvothermal-sonochemical combinatorial approach is reported. Fluoroborophene monolayers with lateral dimension 50 nm-5 µm are synthesized having controlled fluorine content (12-35%). Fluoroborophene exhibits inter-twinned crystallographic structure, with fluorination-tunable visible-range bandgap ≈1.5-2.5 eV, and density functional theory calculations also corroborate it. Fluoroborophene is explored for electrocatalytic oxygen evolution reaction in an alkaline medium and bestow a good stability. Tunable bandgap, electrophilicity and molecular anchoring capability of fluoroborophene will open opportunities for novel electronic/optoelectronic/spintronic chips, energy storage devices, and in numerous catalytic applications.

Phenacyl bromide as Norrish type I photoinitiator for the facile synthesis of chain-end functional PMMA and polystyrene

Phenacyl bromide has been explored as a new Norrish Type I photoinitiator for radically polymerizing methyl methacrylate and styrene monomers. A straightforward radical photopolymerization method using UVA light for the synthesis of chain-end functional poly(methyl methacrylate) and polystyrene has been developed. The process has been refined for both bulk and solution photopolymerizations. Chain-end functionalization was demonstrated by the formation of block-copolymers of the bromine-ended homopolymers, utilized as macroinitiators, resulting in an increase in the molecular weight of the corresponding precursor, observed by gel permeation chromatography (GPC). Block copolymerization was initiated by radicals generated at the chain-ends by a halogen-atom transfer reagent, namely, dimanganese decacarbonyl (Mn2(CO)10). This simple light-induced method is promising for the additive manufacturing field such as vat photopolymerization, stereolithography, digital light processing as it yields chain-end functional materials that can be further processed.

A Facile Synthesis of RGO-Ag2MoO4 Nanocomposites for Efficient Lead Removal from Aqueous Solution.

Efficiently treating wastewater, particularly the elimination of heavy metal ions from water systems, continues to be one of the most pressing and complex challenges in modern environmental management. In this work, reduced graphene oxide coupled silver molybdate binary nanocomposites (RGO-Ag2MoO4 NCs) have been prepared via hydrothermal method. The crystalline nature and surface properties of the developed RGO-Ag2MoO4 NCs were proved by XRD, FTIR, SEM, and EDS techniques. Adsorption experiments demonstrated that the nanocomposites (NCs) effectively removed Pb(II) ions within 120 min, achieving a maximum removal efficiency ranging from 94.96% to 86.37% for Pb(II) concentrations between 20 and 100 mg/L at pH 6. Kinetic studies showed that the adsorption process followed a pseudo-second order model. Isotherm analysis presented that the Langmuir model provided the greatest fit for the equilibrium data, with a monolayer adsorption capacity of 128.94 mg/g. Thermodynamic analysis revealed that the adsorption process was spontaneous and endothermic. The results of this study highlight RGO-Ag2MoO4 NCs as a highly promising and eco-friendly material for the effective elimination of Pb(II) ions from wastewater. Their strong adsorption capacity, coupled with sustainable properties, makes them an efficient solution for addressing lead contamination, offering significant potential for practical applications in water treatment systems.

Facile one-pot synthesis of photoresponsive Cu1.8S and CuInS2 nanostructures aided by Cu-pyrimidylthiolate molecular precursor

Copper-based binary and ternary sulfides have attracted significant attention due to their excellent photo-physical properties, making them highly promising for high-performance energy harvesting and storage devices. This study focuses on the synthesis and structural characterization of an air-stable hexanuclear Cu-pyrimidylthiolate cluster complex which serves as an efficient single-source precursor for the preparation of Cu1.8S nanocrystals. Furthermore, coupling the molecular precursor with suitable indium source resulted in a facile one-pot pathway for the preparation of technologically important, copper-based ternary CuInS₂, nanocrystals. The crystal structure, phase purity, and compositions of the nanostructures were confirmed using PXRD, XPS, EDS, and area elemental mapping. Electron microscopic studies revealed the formation of polygonal and hexagonal morphology with varied size in Cu1.8S and CuInS₂ nanocrystals respectively. UV-Vis diffuse reflectance spectroscopy showed a slight blue shift in the band gap of the nanostructures compared to their bulk counterparts which can be attributed to quantum confinement or surface lattice distortion effects. The band gap of the pristine nanocrystals along with high photocurrent and stable photo-switching characteristics suggest that they can serve as suitable electrode material for optoelectronic and photodetector devices.

Facile and Efficient Synthesis of Fluorosilicone Polymers by Using an Optimized Gradient Ring-Opening Reaction.

Fluorosilicone rubber is essential for sealing in extreme temperatures and non-polar environments due to its exceptional adaptability. However, achieving a high yield of fluorosilicone polymers with medium and high fluorine content remains a challenge. Herein, a facile gradient strategy is developed that involves modifying the method of cyclic monomer addition based on the rate of ring-opening polymerization (ROP), to improve yield and adjust fluorine content precisely. The polymerization process is designed and tailored based on the reaction rates of anionic ring-opening polymerization (AROP) and cationic ring-opening polymerization (CROP) via an efficient gradient strategy. The effects of the polymerization process on the viscosity and yield of vinyl fluorosilicone polymers and hydrofluorosilicone polymers are investigated and optimized. Notably, the as-prepared vinyl-terminated fluoromethylsilane with 60% fluorine content (FMS-Vi-60F) has a high yield (86.6%) and high viscosity (150000 mPa·s) in a short reaction time, which is superior to previous methods. Clearly, the gradient ring-opening method developed in this work provides a facile and efficient synthesis for fabricating fluorosilicone polymers with a high yield and tunable fluorine content.