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Search results for: c-h methylene compounds
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Paweł Możejko dr hab.
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(R,R)-1-Acetyl-1'-(2,4,6-trinitrophenyl)-2,2'-bipyrrolidine
Publication(R,R)-1-Acetyl-1'-(2,4,6-trinitrophenyl)-2,2'-bipyrrolidine has been synthesized and its rentgenostructure has been determined. The structure of the title molecule, C16H19N5O7, is mainly determined by the steric effect of a bulky 2,4,6-trinitrophenyl group attached to the N atom of a pyrrolidine ring. Both pyrrolidine rings adopt an envelope conformation, with one of the methylene C atoms as the flap in each case, and the N-C-C-N...
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Modification of cellulosic filler with diisocyanates – volatile organic compounds emission assessment and stability of chemical structure over time
PublicationThis paper investigated the impact of type and content of diisocyanate on the structure of modified cellulose fillers. Four the most popular isocyanates were applied – isophorone, hexamethylene, toluene and methylene diphenyl diisocyanate – at loadings of 1–15 wt%. Chemical structure, and its short-term storage stability, were investigated for eight weeks. Moreover, the main volatile organic compounds detected during modification,...
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Boron Difluoride Complexes of Carbamoyl Meldrum's Acids
Publication5-[Hydroxy(aryl/alkylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-diones react with BF3•Et2O in mild conditions leading to the formation of boron difluoride complexes of carbamoyl Meldrum's acids. The X-ray structure has been obtained for one representative complex. The obtained new compounds are fairly stable at standard ambient conditions and easily isolable.
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The effect of morphology and crystalline structure of Mo/MoO3 layers on photocatalytic degradation of water organic pollutants
PublicationMolybdenum oxide layers were formed by anodization of the Mo metallic foil in a water/ethylene glycol-based electrolyte containing fluoride ions. The as-prepared, amorphous samples were annealed in air at different temperatures in a range from 100 �C to 700 �C. The crystal phase and morphology of anodized and annealed MoO3 layers were investigated using X-ray diffraction, Raman spectroscopy, and scanning electron microscopy. The...
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Phosphinophosphoranes: Mixed-Valent Phosphorus Compounds with Ambiphilic Properties
PublicationHerein, we present a simple synthesis of mixed-valent phosphinophosphoranes bearing three- and five-coordinate phosphorus centers. Compounds with phosphorus–phosphorus bonds were synthesized via a reaction of lithium phosphides RR′PLi with cat2PCl (cat = catecholate), whereas derivatives with methylene-linked phosphorus centers were obtained via a reaction of phosphanylmethanides RR′CH2Li with cat2PCl. The presence of accessible...
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Screen-printed Sn-doped TiO2 nanoparticles for photocatalytic dye removal from wastewater: A technological perspective
PublicationTiO2 is widely used as a photocatalyst with a wide band gap, which limited its application. Ion doping and formulating a high-quality screen-printing paste enhance its features. However, the printability of objects for advanced application seems essential nowadays. In this research, the Sn-doped TiO2 nanoparticles were prepared through a sol-gel method followed by calcination at various temperatures of 450 °C, 550 °C, 650 °C, 750...
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Sustainable Chemically Modified Mater-Bi/Poly(ε-caprolactone)/Cellulose Biocomposites: Looking at the Bulk through the Surface
PublicationSustainable polymer composites are progressively under development in a technological paradigm shift from "just use more and more" to "convert into value-added products". The bio-based blends based on Mater-Bi bio-plastic (A) and poly(ε-caprolactone) (B), at a weight ratio of 70:30 (A:B) were developed, followed by the addition of UFC100 cellulose (C) filler to yield 70/30 (w/w) (A:B)/C sustainable biocomposites. The effects of...
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Characterization of Highly Filled Glass Fiber/Carbon Fiber Polyurethane Composites with the Addition of Bio-Polyol Obtained through Biomass Liquefaction
PublicationThis work aims to investigate the process of obtaining highly filled glass and carbon fiber composites. Composites were manufactured using previously obtained cellulose derived polyol, polymeric methylene diphenyl diisocyanate (pMDI). As a catalyst, dibutyltin dilaurate 95% and Dabco® 33-LV were used. It was found that the addition of carbon and glass fibers into the polymer matrix causes an increase in the mechanical properties...
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The influence of photointercalaction and photochromism effects on the photocatalytic properties of electrochemically obtained maze-like MoO3 microstructures
PublicationMolybdenum oxide (α-MoO3) thin films with oriented crystalline facets were synthesised by anodization of Mo foils. The obtained samples were exposed to UV–Vis illumination in aqueous electrolytes providing different cations. The morphology and structure of modified samples were investigated. The effect of photointercalated alkali metal cations (Li+, Na+, K+) on optical and structural properties was studied using UV–vis and Raman...
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Atom-economic thiophosphoroselenenylations of C–H acid esters and amides
PublicationThree improved thiophosphoroselenenylation procedures of CHacids, including derivatives of malonic and acetyl-, phosphono-, 4-nitrophenyl- and 3-pyridylacetic acids, have been described and compared to previously reported thiophosphoroselenylation of diethyl malonate using bis(disopropoxyphosphinothioyl)diselenide alone or with the aid of methyl iodide. The use of iodine makes it possible to utilize both equivalents of the selenenylating...
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The structure of novel polyurethanes containing synthetic poly[(R,S)-3-hydroxybutyrate]
PublicationThe aim of this study was to estimate the structure of new polyurethanes with the potential to be used in medicine. Atactic poly[(R,S)-3-hydroxybutyrate], obtained via a ring-opening polymerization, and polycaprolactonediol or polyoxytetramethylenediol were used to built the soft segments. 4,4'-methylene dicyclohexyl diisocyanate and 1,4-butanediol were the components to form hard segments. Polyurethanes with low-molecular weight...
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Hydrothermal modification of TiO2 nanotubes in water and alkali metal electrolytes (LiNO3, NaNO3, KNO3) – Direct evidence for photocatalytic activity enhancement
PublicationThe influence of hydrothermal annealing (HA) of TiO2 nanotubes (TiO2-NTs) in various baths (H2O, LiNO3, NaNO3, KNO3 performed for 4 h, 24 h, 64 h), on their photocatalytic and photoelectrocatalytic properties, was studied. The use of electrolytes was to enable the monitoring of photoactivity changes as a result of the expected impact on the population of hydroxyl groups on the surface. The assumption turned out to be correct and...
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Fully Isohexide-Based Polyesters: Synthesis, Characterization, and Structure-Properties Relations
PublicationHere we present a novel series of biobasedpolyesters solely based on renewable isohexide building blocks,synthesized via melt polymerization. The recently developedisoidide dicarboxylic acid (IIDCA) was polymerized with rigidrenewable diols such as isosorbide (IS), isomannide (IM),isoidide (II), and the novel 2,5-methylene-extended isoididedimethanol (IIDML). Both IIDCA and IIDML weredeveloped to increase the reactivity of the...
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An Investigation of Polyamides Based on Isoidide-2,5-dimethyleneamine as a Green Rigid Building Block with Enhanced Reactivity
PublicationNovel, semicrystalline polyamides and copolyamides were synthesized from a new carbohydrate-based diamine, namely isoidide-2,5-dimethyleneamine (IIDMA). In combination with 1,6-hexamethylene diamine (1,6-HDA) as well as the biobased sebacic acid (SA) or brassylic acid (BrA), the desired copolyamides were obtained via melt polymerization of the nylon salts followed by a solid-state polycondensation (SSPC) process. Depending on the...
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DETERMINATION OF SURFACTANTS IN ENVIRONMENTAL SAMPLES. PART II. ANIONIC COMPOUNDS
PublicationSurfactants (SAA) with negative charge of polar group are named as anionic compounds. They are main constituent of most products containing synthetic surfactants. The linear alkylbenzene sulfonates (LAS), alkyl ethoxysulfates (AES) and alkyl sulfates (AS) are typically applied from this class of compounds. Those surfactants are ingredients of household detergents and cleaners, laundry detergents, cosmetic. Moreover they can be...
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Photocatalytical properties of maze-like MoO3 microstructures prepared by anodization of Mo plate
PublicationIn this work, we present a simple method of the formation of MoO3 microstructures via an electrochemical anodization of Mo plate carried out under varied conditions. The morphology, composition and structure of samples were investigated by SEM, EDX, XRD and Raman spectroscopy. The band gap energy was estimated using the Kubelka–Munk function and was found to be 2.87 eV. Finally, the photocatalytic activities of MoO3 samples were...
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FTIR spectroscopic and thermogravimetric characterization of ground tyre rubber devulcanized by microwave treatment
PublicationIn this work, the phenomena involved in the microwave devulcanization of ground tyre rubber (GTR) were investigated. Three types of GTR with different content of organic compounds (elastomers, plasticizers, etc.), carbon black and ash have been studied. The chemical structure of GTR before and after a microwave devulcanization process was analyzed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA)...
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Fragmentation of Tetrahydrofuran Molecules by H+, C+, and O+ Collisions at the Incident Energy Range of 25–1000 eV
PublicationWe have studied fragmentation processes of the gas-phase tetrahydrofuran (THF) molecules in collisions with the H+, C+, and O+ cations. The collision energies have been varied between 25 and 1000 eV and thus covered a velocity range from 10 to 440 km/s. The following excited neutral fragments of THF have been observed: the atomic hydrogen H(n), n = 4–9, carbon atoms in the 2p3s 1P1, 2p4p 1D2, and 2p4p 3P states and vibrationally...
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Tmscl as a rate accelerating additive in acylations of amines with 5-(α-amino- α'-hydroxy)methylene meldrum's acids
PublicationAspects are presented of the acylation of amines, alcohols and thiols with 5-(α-amino- α'-hydroxy)methylene Meldrum's acids. We placed special emphasis on the acylation reaction of secondary amines with 5-(α-amino- α'-hydroxy)methylene Meldrum's acids, which, due to their basicity, caused problems concerning salt formation with a Meldrum acid derivative. We found that secondary amines, which react at the slowest rate and with a...
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TMSCL as a rate accelerating additive in acylations of amines with 5-(α- amino-α'-hydroxy)methylene meldrum's acids
PublicationAspects are presented of the acylation of amines, alcohols and thiols with 5-(α-amino- α'-hydroxy)methylene Meldrum's acids. We placed special emphasis on the acylation reaction of secondary amines with 5-(α-amino- α'-hydroxy)methylene Meldrum's acids, which, due to their basicity, caused problems concerning salt formation with a Meldrum acid derivative. We found that secondary amines, which react at the slowest rate and with a...
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Synthesis of malonylenamides and thiomalonylenamides
Publication5-[Hydroksyl(aryl(amino))methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione is convenient source of ketenes which can be trapped with various nucleophiles like alcohols, thiols and amines. In reaction between in situ generated ketene and enolizable imines we can easily obtain corresponding malonylenamides. This facile method can be used to obtain thiomalonylenamides using 5-[sulfhydrylo(alkyl(amino))methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione...
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Optimization of electrochemical doping approach resulting in highly photoactive iodine-doped titania nanotubes
PublicationThe paper focuses on the optimization procedure concerning the synthesis method resulting in highly ordered titania nanotubes doped with iodine atoms. The doping process was based on the electrochemical treatment of a titania nanotube layer immersed in a potassium iodide (KI) solution acting as an iodine precursor. A number of endeavors were undertaken in order to optimize the doping conditions. Electrolyte concentration, reaction...
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Influence of CeO2 and TiO2 Particles on Physicochemical Properties of Composite Nickel Coatings Electrodeposited at Ambient Temperature
PublicationThe Ni-TiO2 and Ni-CeO2 composite coatings with varying hydrophilic/hydrophobic characteristics were fabricated by the electrodeposition method from a tartrate electrolyte at ambient temperature. To meet the requirements of tight regulation by the European Chemicals Agency classifying H3BO3 as a substance of very high concern, Rochelle salt was utilized as a buffer solution instead. The novelty of this study was to implement a...
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The effect of UV-C irradiation on lipids and selected biologically active compounds in human milk
PublicationThe effect of UV-C irradiation of human milk on lipid oxidation, content of antioxidants (vitamin C and catalase, CAT) and bactericidal compounds (lysozyme), as well as the total antioxidant capacity (TAC), of the breast milk was investigated. In parallel, the extent of inactivation of some bacteria was also determined. UV-C at doses from 85 to 740 J L−1 caused total inactivation of Escherichia coli and Staphylococcus aureus, but...
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Mn-Co spinel coatings on Crofer 22 APU by electrophoretic deposition: Up scaling, performance in SOFC stack at 850 °C and compositional modifications
PublicationCeramic coatings for metallic interconnects play a key role in limiting corrosion and chromium evaporation in solid oxide cells. This study presents the upscaling of the electrophoretic deposition (EPD) technique to process Mn-Co spinels on real-dimension Crofer 22 APU interconnects and the test in a SOFC stack. Area specific resistance of long-term test conducted for 5000 h at 850 °C demonstrated that two-steps sintering has a...
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Insight into Potassium Vanadates as Visible-Light-Driven Photocatalysts: Synthesis of V(IV)-Rich Nano/Microstructures for the Photodegradation of Methylene Blue
PublicationPhotocatalysis 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...
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Expermental investigation on adsorption of methylene blue dye from waste water using corncob cellulose-based hydrogel
PublicationHydrogel from corncob cellulose was synthesized in this investigation. The synthesized Hydrogel was characterized by SEM, XRD, and FTIR instruments. As the results indicate the synthesized hydrogel has required and important features, these suggest the suitability of hydrogel for the adsorption of methylene blue dye (MBD). Three important process variables (dosage, contact time, and initial concentration) with three levels were...
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Non-metaldoped TiO2 nanotube arrays for high efficiency photocatalytic decomposition of organic species in water
PublicationTitanium dioxide is a well-known photoactive semiconductor with a variety of possible applications. The procedure of pollutant degradation is mainly performed using TiO2 powder suspension. It can also be exploited an immobilized catalyst on a solid support. Morphology and chemical doping have a great influence on TiO2 activity under illumination. Here we compare photoactivity of titania nanotube arrays doped with non-metal atoms:...
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One-Step Synthesis of b-Lactams with Retro-Amide Side Chain
PublicationAbstract: A one pot synthesis for preparation of 1,4-disubstituted-2-oxo-azetidine-3-carboxylic acid amides was developed. 5-(α-N-substituted-amino-α'-hydroxy)methylene Meldrum's acids act as a source of ketenes that react with aldimines in boiling toluene to give b-lactams with retro-amid side chain.
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The effects of calcium–silicate–hydrate (C–S–H) seeds on reference microorganisms
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Decolorisation of Methylene Blue with Sodium Persulfate Activated with Visible Light in the Presence of Glucose and Sucrose
PublicationThe paper presents the results of research on the methylene blue (MB) degradation with sodium persulfate (PDS) activated with visible light (Vis) in the presence of glucose and sucrose. The following test were examined: absence and presence of sugars in concentrations of 50–300 mM, presence and absence of Vis radiation, pH of the model solution (6.0–12.0), identification of free radicals, kinetics of the pseudo-first-order reaction....
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One-step formation of n-alkenyl-malonamides and n-alkenyl-thiomalonamides from carbamoyl meldrum's acids.
PublicationA one-pot synthesis for the preparation of N-alkenyl-malonamides and N-alkenyl-thiomalonamides was developed. 5-[Hydroxy/mercapto(aryl/alkylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione act as a source of ketenes that react with the tautomeric form of alkyl-(2-phenyl-propylidene)-amines. A possible [2+2] or [4+2] cycloaddition product of ketene to imines was not observed.
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Peptide modification with thiomalonoamide moiety
PublicationAbstract: Meldrum acid derivatives under the thermal decomposition are well known source of ketenes. Recently we investigated chemical properties of thiocarbamolyl meldrum acids. We found that 5-(α-alkylamino- α'-sulfhydryl)methylene Meldrum's acids hated in the presence of amines produce thiomalonamides. We used this reaction to the one pot synthesis of series of short peptides containing thiomalonoamide motif.
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SnO2 nanoparticles embedded onto MoS2 nanoflakes - An efficient catalyst for photodegradation of methylene blue and photoreduction of hexavalent chromium
PublicationIn this work, a molybdenum disulfide/tin oxide (MoS2/SnO2) composite was successfully prepared via a hydrothermal method. The MoS2/SnO2 composite was used as a photocatalyst for photoreduction of hexavalent chromium and photodecomposition of methylene blue. It exhibited higher photocatalytic performance under simulated solar light irradiation than MoS2 itself. The obtained material was characterized by several spectroscopic and...
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Synthesis of compounds with C-P-P and C=P-P bond systems based on the phospha-Wittig reaction
PublicationA reactivity study of a β-diketiminate titanium(III) phosphanylphosphido complex [MeNacNacTi(Cl){η2-P(SiMe3)-PtBu2}] (1) towards ketones such as benzophenone, 9-fluorenone, acetophenone, cyclopentanone, cyclohexanone and cycloheptanone is reported. The reactions of 1 with aromatic ketones (without α-protons) directly lead to the Ti(III) complex [MeNacNacTi(μ2-Cl)(OSiMe3)] (5) as well as Ti(IV) complexes with the pinacol condensation...
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Easy formation of acyl-Meldrum's acid anhydride
PublicationAcyl Meldrum's acid are usually a good source of ketenes upon definite thermal composition. However we treated acyl-Meldrum's acid with the Lewis acid and we observed formation of 5[[(2,2-dimethyl-4,6-dioxo-1,3-dioxan 5 ylidene)(acyl/arylamino)mathoxy](acyl/arylamino)methylene]-2,2dimethyl-1,3-dioxane-4,6 dione which means acyl-Meldrum's acid anhydride. The chemical properities of acyl-Meldrum's acid anhydride were explored.
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A new approach to the stereoselective synthesis of trans-3-carbamoyl-b-lactam moieties†
PublicationOne-pot synthesis of optically active 1,4-disubstituted-3-carbamoyl-azetidinones from 5-[(N-arylamino)- (hydroxyl)methylene]-2,2-dimethyl-1,3-dioxa-4,6-diones and chiral aldimines is achieved via thermal generation of carbamoyl ketenes and subsequent [2+2] cycloaddition. Three possible chiral induction approaches were tested and (R)-(+)-1-phenylethylamine was confirmed as the best chiral auxiliary. Among the four possible diastereoisomers,...
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A multi‑criteria approach to investigate spatial distribution,sources, and the potential toxicological effect of polycyclic aromatic hydrocarbons (PAHs) in sediments of urban retention tanks
PublicationBottom sediments deposited in retention tanks (RTs) located on two urban streams (Oliwski and Strzyza) in the central part of Gdansk (Poland) were analysed for polycyclic aromatic hydrocarbons’ (PAHs) content. PAHs were extracted from samples with methylene chloride, then the extracts were subjected to clean-up applying the solid phase extraction (SPE) method. Quantitative and qualitative determination of 16 PAHs was performed...
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Proton transfer reaction from some C–H acids to N-bases in polar aprotic solvents
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TMSCl Promoted Acylation of Amines with 5-(α-amino- α'-hydroxy)methylene Meldrum's Acids - Elucidation of Mechanism.
PublicationRecently we have observed accelerating influence of trimethyl silyl chloride addition on the rate of the reactions of 5-(α-amino- α'-hydroxy)methylene Meldrum's Acids with amines, particularly in the case of highly basic amines. However the nature of the aforementioned process remain unexplained. In proposed communication we wish to report insightful elucidation of this mechanism. The reaction under investigation involves simply...
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Facile preparation of extremely photoactive boron-doped TiO2 nanotubes arrays
PublicationDoping of TiO2 nanotube arrays with boron was realized via electrochemical treatment of as-anodized titania immersed in electrolyte containing boric acid. The photoactivity of doped and pure titania was examined by means of photoelectrochemical and photocatalytic response under UV-vis irradiation. The results showed that photocurrent density of B-TNTs is remarkably higher (7.5 times) than density of pure TiO2 nanotube arrays. Furthermore,...
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Weak hydrogen bonding interaction S-H···O=C studied by FT-IR spectroscopy and DFT calculations
PublicationInteractions between the thiolate group of tri-tert-butoxysilanethiol (TBST) and carbonyl group of acetone are studied with the use of FT-IR spectroscopy and DFT calculations.
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Graphene hydrogels with embedded metal nanopatricles as efficient catalysts in 4-nitrophenol reduction and methylene blue decolorization
PublicationSynthesis and characterization of the graphene hydrogels with three different metallic nanoparticles, that is Au, Ag and Cu, respectively is presented. Synthesized in a one-pot approach graphene hydrogels with embedded metallic nanoparticles were tested as heterogeneous catalysts in a model reaction of 4-nitrophenol reduction. The highest activity was obtained for graphene hydrogel with Cu NPs and additional reaction of methylene...
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Persulfates to degrade a mixture of dyes (rhodamine B, methylene blue) in the presence of glucose and visible light
PublicationA treatment process utilizing visible-light-activated (Vis) persulfates (PS) in the presence of an organic promoter (glucose) was developed for the simultaneous decolorization of a rhodamine B (RhB) and methylene blue (MB) mixture. Various doses of glucose, PS concentrations, pH values, initial dye concentrations and process time were tested to find out the most appropriate parameters for degrading the RhB/MB mixture in the...
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Glutathione conjugation of the antitumor-active 1-nitroacridine derivatives compounds C-857 and C-1748 – the major role of glutathione S-transferase M1-1
Open Research DataObjectives: C-857 and C-1748 are antitumor-active agents, monomers of unsymmetrical bisacridine derivatives. The aim of this study was to analyze their glutathione (GSH) conjugation in vitro in the presence of glutathione S-transferase (GST) M1-1.
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Experimental and quantum chemical evidences for C–H⋯N hydrogen bonds involving quaternary pyridinium salts and pyridinium ylides
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An Aqueous Exfoliation of WO3 as a Route for Counterions Fabrication—Improved Photocatalytic and Capacitive Properties of Polyaniline/WO3Composite
PublicationIn this paper, we demonstrate a novel, electrochemical route of polyaniline/tungsten oxide (PANI)/WO3) film preparation. Polyaniline composite film was electrodeposited on the FTO (fluorine-doped tin oxide) substrate from the aqueous electrolyte that contained aniline (monomer) and exfoliated WO3 as a source of counter ions. The chemical nature of WO3 incorporated in the polyaniline matrix was investigated using X-ray photoelectron...
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Ferrocene-Labeled Carbon-Encapsulated Iron Nanoparticles: The First Magnetic Nanocatalysts for C–H Arylation toward 1,1′-Biphenyl Formation
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Cross-sections for electron-scattering from 2-methyl-1-buten-3-yne, C 5 H 6 , molecules
PublicationtCross-sections for electron collisions with the 2-methyl-1-buten-3-yne [H2C C(CH3)C CH] moleculewere measured and calculated. Absolute grand-total electron-scattering cross-section (TCS) was takenat impact energies from 0.6 to 300 eV in the linear electron-transmission experiment. The TCS energydependence for the electron–C5H6collision has two prominent enhancements separated with a deepminimum located near 1.8 eV. In addition,...