Preparation and characterization of bis-phosphonated polycarbohydrates.

A simple, cost-effective, one-pot method was proposed to introduce bis-phosphonic groups onto alginic acid and carboxymethyl cellulose (CMC). New derivatives were characterized by means of nuclear magnetic resonance, X-ray photoelectron, and attenuated total reflectance Fourier transform infrared spectroscopy. These analyses confirmed the successful transformation of carboxylic groups present in alginic acid and CMC into bis-phosphonic groups. Additionally, thermogravimetric analysis coupled with differential scanning calorimetry was employed to investigate the thermal properties of the bis-phosphonic derivatives of alginate and CMC. The results clearly demonstrate the char-forming ability of both studied bis-phosphonated polycarbohydrates, suggesting their potential as intumescent materials.

Insight into Potassium Vanadates as Visible-Light-Driven Photocatalysts: Synthesis of V(IV)-Rich Nano/Microstructures for the Photodegradation of Methylene Blue.

Photocatalysis is regarded as a promising tool for wastewater remediation. In recent years, many studies have focused on investigating novel photocatalysts driven by visible light. In this study, K2V6O16·nH2O nanobelts and KV3O8 microplatelets were synthesized and investigated as photocatalysts. Samples were obtained via the facile method based on liquid-phase exfoliation with ion exchange. By changing the synthesis temperature (20-80 °C), different compositions, morphologies, and V4+/V5+ ratios were obtained and investigated as photocatalysts for organic dye degradation. Potassium vanadates' structural, morphological, and optical properties were characterized using X-ray diffraction(XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Physical Property Measurement System (PPMS), thermogravimetric analysis (TGA) with mass spectrometry (MS), N2 adsorption, scanning electron microscopy (SEM), photoluminescence (PL), and UV-vis diffuse reflectance spectroscopy (DRS). Synthesized K2V6O16·nH2O and KV3O8 showed an efficient absorption in the visible wavelength region with a narrow band gap energy of 1.80 and 1.91 eV, respectively. Their photocatalytic activity was evaluated by the degradation of methylene blue (MB) under simulated solar light illumination. The KV3O8 microplatelets exhibited the greatest photocatalytic activity, resulting in more than 90% degradation of the dye within the first 30 min. It is suggested that the observed excellent photocatalytic performance is attributed to the high content of V4+ species. Furthermore, the influence of active species was investigated, and the mechanism responsible for the photodegradation of the MB dye was discussed for the first time for potassium vanadates.

From phosphanylphosphaalkenes to coordination copper and silver polymers containing P-P bonds.

This study was focused on the activation of the CP bond via reactions of Ph2CP-PtBu2 (1) with 1,6-hexanediol and selected dithiols (1,4-butanedithiol, 1,4-benzenedithiol and 1,4-benzenedimethanethiol). These reactions proceed according to a 1,2-addition mechanism, providing new compounds with formulas {(Ph)2(H)C-P-PtBu2}{µ2-(O-(CH2)6-O)}{tBu2P-P-C(H)(Ph)2} (2), {(Ph)2(H)C-P-PtBu2}{µ2-(S-(CH2)4-S)}{tBu2P-P-C(H)(Ph)2} (3a), {(Ph)2(H)C-P-PtBu2}{µ2-(S-C6H4-S)}{tBu2P-P-C(H)(Ph)2} (3b), and {(Ph)2(H)C-P-PtBu2}{µ2-(S-CH2-C6H4-CH2-S)}{tBu2P-P-C(H)(Ph)2} (3c). Next, the reactions of 3a and 3c with metal chlorides led to the growth of desired coordination polymers of copper(I) and silver(I). All the obtained compounds remained stable under atmospheric conditions.

Tailoring Physicochemical Properties of V2O5 Nanostructures: Influence of Solvent Type in Sol-Gel Synthesis.

The influence of different solvents, including aqueous and nonaqueous types, on the physicochemical properties of V2O5 nanostructures was thoroughly investigated. Various characterization techniques, such as XRD, XPS, FTIR, Raman spectroscopy, UV-vis DRS, SEM, TEM, and BET, were employed to analyze the obtained materials. Additionally, the adsorption properties of the synthesized V2O5 nanostructures for methylene blue were examined, and kinetic parameters of adsorption were calculated. The results demonstrate that the morphology of the obtained crystals can be finely controlled by manipulating water concentration in the solution, showcasing its profound impact on both the structural characteristics and adsorption properties of the nanostructures. Furthermore, the structural changes of the resulting V2O5 material induced by solvents show strong impacts on its photocatalytic properties, making it a promising photocatalyst.

Enhancing colloidal stability of nanodiamond via surface modification with dendritic molecules for optical sensing in physiological environments.

Pre-treatment of diamond surface in low-temperature plasma for oxygenation and in acids for carboxylation was hypothesized to promote the branching density of the hyperbranched glycidol polymer. This was expected to increase the homogeneity of the branching level and suppress interactions with proteins. As a result, composite nanodiamonds with reduced hydrodynamic diameters that are maintained in physiological environments were anticipated. Surfaces of 140-nm-sized nanodiamonds were functionalized with oxygen and carboxyl groups for grafting of hyperbranched dendritic polyglycerol via anionic ring-opening polymerization of glycidol. The modification was verified with Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy. Dynamic light scattering investigated colloidal stability in pH-diverse (2-12) solutions, concentrated phosphate-buffered saline, and cell culture media. Thermogravimetric analysis of nanodiamonds-protein incubations examined non-specific binding. Fluorescence emission was tested across pH conditions. Molecular dynamics simulations modeled interparticle interactions in ionic solutions. The hyperbranched polyglycerol grafting increased colloidal stability of nanodiamonds across diverse pH, high ionic media like 10 × concentrated phosphate-buffered saline, and physiological media like serum and cell culture medium. The hyperbranched polyglycerol suppressed non-specific protein adsorption while maintaining intensive fluorescence of nanodiamonds regardless of pH. Molecular modelling indicated reduced interparticle interactions in ionic solutions correlating with the improved colloidal stability.

Bovine Serum Albumin - Hydroxyapatite Nanoflowers as Potential Local Drug Delivery System of Ciprofloxacin.

Introduction: Hybrid nanoflowers are structures consisting of organic (enzymes, proteins, nucleic acids) and inorganic components (mostly metal phosphates) with a flower-like hierarchical structure. Novel hybrid nanoflowers based on bovine serum albumin (BSA) and hydroxyapatite (HA) were obtained and characterized. Study on BSA-HA nanoflowers as potential drug delivery system is reported for the first time. Methods: Embedding ciprofloxacin in the structure of hybrid nanoflowers was confirmed by ATR-FTIR and thermogravimetric analysis. The inorganic phase of the nanoflowers was determined by X-ray diffraction. UV‒Vis spectroscopy was used to evaluate the release profiles of ciprofloxacin from nanoflowers in buffer solutions at pH 7.4 and 5. The agar disk diffusion method was used to study the antibacterial activity of the synthesized nanoflowers against Staphylococcus aureus and Pseudomonas aeruginosa. Results: Bovine serum albumin - hydroxyapatite nanoflowers were obtained with diameters of ca. 1-2 µm. The kinetics of ciprofloxacin release from nanoflowers were described by the Korsmeyer-Peppas model. The antibacterial activity of the synthesized nanoflowers was demonstrated against S. aureus and P. aeruginosa, two main pathogens found in osteomyelitis. Conclusion: The formulated nanoflowers may act as an efficient local antibiotic delivery system. Due to the use of nonhazardous, biodegradable components and benign synthesis, hybrid nanoflowers are very promising drug delivery systems that could be applied in the treatment of skeletal system infections.

Synthesis of Phosphonated Carbon Nanotubes: New Insight into Carbon Nanotubes Functionalization.

Carbon nanotubes were successfully functionalized for the first time in a free radical phosphonylation reaction. Three synthetic protocols were proposed. Carbon nanotubes and diethylphosphite reacted in the presence of known radical initiator, such as azobisisobutyronitrile, single electron oxidant-Mn(OAc)3, or under UV radiation. The functionalized material was fully characterized by means of spectroscopic methods, together with microscopic, surface area and thermogravimetric analyses. UV-illumination was found to be the most effective approach for introducing phosphonates onto carbon nanotubes. X-ray photoelectron spectroscopy analysis showed 6% phosphorus in this sample. Moreover, the method was performed at room temperature for only one hour, using diethylphosphite as a reactant and as a solvent. The functionalized carbon nanotubes showed an improved thermal stability, with a decomposition onset temperature increase of more than 130 °C. This makes it very promising material for flame retarding applications.

Tailoring the Size and Shape-New Path for Ammonium Metavanadate Synthesis.

Ammonium metavanadate, NH4VO3, plays an important role in the preparation of vanadium oxides and other ammonium compounds, such as NH4V3O8, (NH4)2V3O8, and NH4V4O10, which were found to possess interesting electrochemical properties. In this work, a new route for the synthesis of NH4VO3 is proposed by mixing an organic ammonium salt and V2O5 in a suitable solvent. The one-step procedure is carried out at room temperature. Additionally, the need for pH control and use of oxidants necessary in known methods is eliminated. The mechanism of the NH4VO3 formation is explained. It is presented that it is possible to tailor the morphology and size of the obtained NH4VO3 crystals, depending on the combination of reagents. Nano- and microcrystals of NH4VO3 are obtained and used as precursors in the hydrothermal synthesis of higher ammonium vanadates. It is proven that the size of the precursor particles can significantly affect the physical and chemical properties of the resulting products.

Solvent-Free Synthesis of Phosphonic Graphene Derivative and Its Application in Mercury Ions Adsorption.

Functionalized graphene was efficiently prepared through ball-milling of graphite in the presence of dry ice. In this way, oxygen functional groups were introduced into material. The material was further chemically functionalized to produce graphene derivative with phosphonic groups. The obtained materials were characterized by spectroscopic and microscopic methods, along with thermogravimetric analysis. The newly developed material was used as an efficient mercury adsorbent, showing high adsorption efficiency. The adsorption isotherms were fitted using Freundlich and Langmuir models. The adsorption kinetics were fitted with pseudo-first order and pseudo-second order models. Adsorption selectivity was determined in the presence of cadmium ions and nickel ions. The presence of mentioned bivalent ions in the solution did not affect mercury adsorption efficiency.

Mechanism of Reduced Sintering Temperature of Al2O3⁻ZrO2 Nanocomposites Obtained by Microwave Hydrothermal Synthesis.

A novel method to obtain Al2O3⁻ZrO2 nanocomposites is presented. It consists of the co-precipitation step of boehmite (AlO(OH)) and ZrO2, followed by microwave hydrothermal treatment at 270 °C and 60 MPa, and by calcination at 600 °C. Using this method, we obtained two nanocomposites: Al2O3⁻20 wt % ZrO2 and Al2O3⁻40 wt % ZrO2. Nanocomposites were characterized by Fourier transformed infrared spectroscopy, Raman spectroscopy, X-ray diffraction, and transmission electron microscopy. Sintering behavior and thermal expansion coefficients were investigated during dilatometric tests. The sintering temperatures of the nanocomposites were 1209 °C and 1231 °C, respectively-approximately 100 °C lower than reported for such composites. We attribute the decrease of the sintering temperature to the specific nanostructure obtained using microwave hydrothermal treatment instead of conventional calcination. Microwave hydrothermal treatment resulted in a fine distribution of intermixed highly crystalline nanoparticles of boehmite and zirconia. Such intermixing prevented particle growth, which is a factor reducing sintering temperature. Further, due to reduced grain growth, stability of the θ-Al2O3 phase was extended up to 1200 °C, which enhances the sintering process as well. For the Al2O3⁻20 wt % ZrO2 composition, we observed stability of the zirconia tetragonal phase up to 1400 °C. We associate this stability with the mutual separation of zirconia nanoparticles in the alumina matrix.

Fully scalable one-pot method for the production of phosphonic graphene derivatives.

Graphene oxide was functionalized with simultaneous reduction to produce phosphonated reduced graphene oxide in a novel, fully scalable, one-pot method. The phosphonic derivative of graphene was obtained through the reaction of graphene oxide with phosphorus trichloride in water. The newly synthesized reduced graphene oxide derivative was fully characterized by using spectroscopic methods along with thermal analysis. The morphology of the samples was examined by electron microscopy. The electrical studies revealed that the functionalized graphene derivative behaves in a way similar to chemically or thermally reduced graphene oxide, with an activation energy of 0.014 eV.