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Microwave-Assisted Sol-Gel Preparation of the Nanostructured Magnetic System for Solid-Phase Synthesis.

ABSTRACT: This work describes a new synthesis method for core-shell magnetite nanoparticles with a secondary silica shell, functionalized with a linker system (Fe₃O₄-PABA-SiO₂-linker) using a microwave-assisted heating technique. The functionalized solid nanomaterial was used for the nanophase synthesis of peptides (Fmoc route) as a solid support. The co-precipitation method was selected to obtain magnetite nanoparticles and sol-gel technique for silica coating using a microwave-assisted (MW) procedure. The magnetic properties of the nanoparticle core offer the advantage of a quick and easy alternative for the magnetic separation of the product from the reaction mixture, facilitating all the intermediary washing and separation operations. The intermediate and final materials were analyzed by advanced characterization methods. The effectiveness of the nanophase peptide synthesis using this nanostructured material as solid support was demonstrated for a short peptide sequence.

SUBMITTER: Istrati D

PROVIDER: S-EPMC8709383 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Sol-Gel Synthesis of the Double Perovskite Sr2FeMoO6 by Microwave Technique.

Project description:The effect of microwave radiation on the hydrothermal synthesis of the double perovskite Sr2FeMoO6 has been studied based on a comparison of the particle size and structural characteristics of products from both methods. A temperature, pressure, and pH condition screening was performed, and the most representative results of these are herein presented and discussed. Radiation of microwaves in the hydrothermal synthesis method led to a decrease in crystallite size, which is an effect from the reaction temperature. The particle size ranged from 378 to 318 nm when pH was 4.5 and pressure was kept under 40 bars. According to X-ray diffraction (XRD) results coupled with the size-strain plot method, the product obtained by both synthesis methods (with and without microwave radiation) have similar crystal purity. The Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) techniques showed that the morphology and the distribution of metal ions are uniform. The Curie temperature obtained by thermogravimetric analysis indicates that, in the presence of microwaves, the value was higher with respect to traditional synthesis from 335 K to 342.5 K. Consequently, microwave radiation enhances the diffusion and nucleation process of ionic precursors during the synthesis, which promotes a uniform heating in the reaction mixture leading to a reduction in the particle size, but keeping good crystallinity of the double perovskite. Precursor phases and the final purity of the Sr2FeMoO6 powder can be controlled via hydrothermal microwave heating on the first stages of the Sol-Gel method.

| S-EPMC8305548 | biostudies-literature

Mono-amine functionalized phthalocyanines: microwave-assisted solid-phase synthesis and bioconjugation strategies.

Project description:Phthalocyanines (Pcs) are excellent candidates for use as fluors for near-infrared (near-IR) fluorescent tagging of biomolecules for a wide variety of bioanalytical applications. Monofunctionalized Pcs, having two different types of peripheral substitutents, one for covalent conjugation of the Pc to biomolecules and others to improve the solubility of the macrocycle, are ideally suited for the desired applications. To date, difficulties faced during the purification of monofunctionalized Pcs limited their usage in various types of applications. Herein are reported a new synthetic method for rapid synthesis of the target Pcs and bioconjugation techniques for labeling of the oligonucleotides with the near-IR fluors. A novel synthetic route was developed utilizing a hydrophilic, poly(ethylene glycol) (PEG)-based support with an acid-labile Rink Amide linker. The Pcs were functionalized with an amine group for covalent conjugation purposes and were decorated with short PEG chains, serving as solubilizing groups. Microwave-assisted solid-phase synthetic method was successfully applied to obtain pure asymmetrically substituted monoamine functionalized Pcs in a short period of time. Three different bioconjugation techniques, reductive amination, amidation, and Huisgen cycloaddition, were employed for covalent conjugation of Pcs to oligonucleotides. The described microwave-assisted bioconjugation methods give an opportunity to synthesize and isolate the Pc-oligonucleotide conjugate in a few hours.

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Copper-/Zinc-Doped TiO<sub>2</sub> Nanopowders Synthesized by Microwave-Assisted Sol-Gel Method.

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Optical, Structural, and Magnetic Hyperthermia Properties of Yttrium Iron Garnet Synthesized by Hybrid Microwave-Assisted Hydrothermal and Sol–Gel Auto Combustion Routes

Project description:Magnetic hyperthermia

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Biphasic Sol-Gel Synthesis of Microstructured/Nanostructured YVO4:Eu3+ Materials and Their H2O2 Sensing Ability.

Project description:Microstructured/nanostructured YVO4:Eu3+ powders and films were synthesized through a biphasic sol-gel method, aiming at their application as H2O2 sensing materials based on the turn-off luminescence of Eu3+ ions. The synthesis was typically carried out at temperatures of 80 °C or lower by using organic solutions to dissolve vanadium alkoxide and aqueous solutions to dissolve yttrium and europium salts together with sodium carboxylates. The resultant crystalline YVO4:Eu3+ powders and films were characterized as containing micrometer-sized particles comprising primary nanoparticles with high specific surface areas. A comparative study was performed on the H2O2-responsive turn-off luminescence properties for the above samples and those synthesized by a single-phase sol-gel or a conventional solid-state reaction method. The results indicated that the microstructural feature of the samples from the biphasic sol-gel method was effective for detecting H2O2 through its adsorption on the particle surface and quenching of the Eu3+ luminescence. The film samples showed repeatable and quantitative turn-off luminescence, thereby demonstrating their suitability as solid-state H2O2 sensors.

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Sol-Gel Combustion-Assisted Electrostatic Spray Deposition for Durable Solid Oxide Fuel Cell Cathodes.

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| S-EPMC9035593 | biostudies-literature

Microwave-assisted solid-phase synthesis of side-chain to side-chain lactam-bridge cyclic peptides.

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| S-EPMC4654418 | biostudies-literature

The Preparation of Porous Sol-Gel Silica with Metal Organic Framework MIL-101(Cr) by Microwave-Assisted Hydrothermal Method for Adsorption Chillers.

Project description:Abstract: Metal organic framework (MOF) of MIL-101(Cr)-Silica (SiO₂) composites with highly mesoporous and uniform dispersions were synthesized by a microwave-assisted hydrothermal method followed by the sol-gel technique. Water vapor adsorption experiments were conducted on the MIL-101(Cr)-SiO₂ composites for industrial adsorption chiller applications. The effects of MIL-101(Cr)-SiO₂ mixing ratios (ranging from 0% to 52%), the surface area and amount of Lewis and Brønsted sites were comprehensively determined through water vapor adsorption experiments and the adsorption mechanism is also explained. The BET and Langmuir results indicate that the adsorption isotherms associated with the various MIL-101(Cr)-SiO₂ ratios demonstrated Type I and IV adsorption behavior, due to the mesoporous structure of the MIL-101(Cr)-SiO₂. It was observed that the increase in the amount of Lewis and Brønsted sites on the MIL-101(Cr)-SiO₂ composites significantly improves the water vapor adsorption efficiency, for greater stability during the water vapor adsorption experiments.

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Preparation of macroporous transition metal hydroxide monoliths via a sol-gel process accompanied by phase separation.

Project description:Three-dimensional transition metal hydroxide monoliths were facilely fabricated by a sol-gel process accompanied by phase separation in the presence of polyacrylic acid (PAA) and propylene oxide (PO). In the typical ZnCl2-PAA-PO system, PAA is used as a phase separation inducer as well as a framework former to control the phase separation and the formation of macrostructures, whereas PO works as a proton scavenger to initiate the gelation of the system and freeze the macrostructures. Appropriate amount of PAA, PO and solvents allow the formation of zinc (Zn) hydroxide monolith with cocontinuous skeletons and interconnected macropores, and the construction mechanism and characteristics of macrostructure are also investigated. The resultant dried gels are amorphous Zn hydroxide monolith with a narrow macropore size distribution (~1 μm). This approach is further used to successfully prepare macroporous single or binary composite transition metal hydroxide monoliths.

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