A solid spin-labeled material was obtained starting from 2-chloro-3,5-dinitro-N-(4-(2,2,6,6-tetramethyl-piperidine-1-oxyl)-benzamide) and aminopropyl-silica gel. Stability tests showed that even after several months the spin-labeled material had the same properties as immediately after synthesis. EPR properties of the TEMPO-derivatized silica were studied as a function of solvent polarity and temperature. Rotational correlation times were calculated from EPR spectra and correlated with solvent characteristics and temperature. Polar solvents induce a fast motion of the spin-label, clearly seen in the EPR spectra by the apparition of the well-known TEMPO radical triplet. The solid spin-labeled (dry) sample showed a high interspin interaction, which can be disrupted not only by different (liquid) solvents, but also by absorption of different solids, like cyclodextrins, dendrimers or polyethyleneglycols. Also, changes induced by the temperature were studied in the case of toluene wet sample. From 150 to 370 K, the spectrum is changing from a slow motion spectrum type to a fast motion regime. The preparative procedures to obtain the spin-labeled silica as well as some of its parameters are described. 相似文献
After oxidation of tannins (Tannins 1–3) extracted from grape seeds, Tanoxil compounds with increased solubility and enhanced antioxidant activities were synthesized. In this research, ABTS+· assay and a chemiluminescence method were used for antioxidant measurement of hydrophilic compounds (Tanoxils 1–3).
It was observed that the antioxidant activity (AA, %) is very similar for the three samples, while at the same time AA is quite high (93.16%–96.48%). The percentage of inhibition by ABTS+· is higher for Tanoxil 2 (96.4%) as compared to Tannin 2 compound (14.34%). Moreover, the total content (TCF) of carboxyl and phenolic groups was investigated. TCF values, determined for Tanoxil products, revealed a double (Tanoxil 1) or triple (Tanoxil 2) increase as compared to the value of the TCF of Tannin 1. Tanoxil products represent an interest for future research as they have a high AA (96.4%) and the content of acidic groups is significant (TCF, 0.191 meq g?1).
Journal of Thermal Analysis and Calorimetry - Two new zinc(II) coordination compounds have been synthesized by the reaction of diazine-ring containing Schiff bases di(2-pyridyl) ketone... 相似文献
In this study, the preparation by grafting of amino-functionalized SBA-15 molecular sieves was carried out. Amino-functionalized molecular sieves were synthesized using a silane coupling agent and different types of amination reagents which react with modified SBA-15. These composites were characterized by FT-IR spectroscopy, X-ray diffraction at low angles, nitrogen physisorption at 77 K, and evaluated by the adsorption of CO2 and its temperature-programmed desorption—TPD. Thermal stability was investigated by TGA and DTA methods. In the view of a possible use of these amino-functionalized molecular sieves as sorbents for CO2 removal, their adsorption–desorption properties towards CO2 were also investigated by the TPD method. The mass loss of amino-functionalized molecular sieves above 215 °C was due to the oxidation and decomposition of amino propyl functional groups. This means that these composites could be used for adsorption of CO2 at temperatures below 215 °C. The adsorption of CO2 and its temperature programmed desorption using thermogravimetry were studied for amino-functionalized molecular sieves at 60 °C. The evolved gases during the adsorption–desorption of CO2 on amino-functionalized molecular sieves were identified by online mass spectrometry coupled with thermogravimetry. CO2 adsorption isotherms of functionalized samples at 60 °C showed that both the adsorption capacity (mg CO2/g adsorbent) and the efficiency of amino groups (mol CO2/mol NH2) depend on the type of amination reagents and the amount of organic compound used.
Suitably functionalized dihydroazulenes (DHAs), dithienylethenes (DTEs), and spiropyrans (SPs) are photo-active molecules that upon irradiation undergo isomerization by ring-opening/closure reactions, which involve carbon-carbon or carbon-heteroatom bond formation/breakage. These photo-isomers may return to the original ones under light or thermal activation. Introducing molecular photoswitches into macrocyclic structures can have strong implications for the forward and backward switching properties. In this report we summarize synthetic protocols for making macrocycles based on one or more units of DHA, DTE, and SP and the resulting properties of these macrocycles. 相似文献
Whereas the internal fragment topological index (IFTI) is calculated in the normal manner as for any molecule, the external fragment topological index (EFTI) is calculated so as to reflect the interaction between the excised fragment F and the remainder of the molecule (G-F). For selected topological indices (TIs), a survey of EFTI values, formulas and examples is presented. Some requirements as to the fragment indices are formulated and examined. In the discussion of the results, it is shown that for some TIs regularities exist in the dependence of EFTI values upon the branching of fragment F, or upon the marginal versus central position of the fragment F in the graph G. New vortex invariants can be computed as EFTI values for one-atom fragments over all graph vertices; by iteration, it is in principle possible to devise an infinite number of now vertex invariants. 相似文献
Hybrid nanocomposite films of ITO-coated, self-assembled porous nanostructures of tungsten trioxide (WO(3)) were fabricated using electrochemical anodization and sputtering. The morphology and chemical nature of the porous nanostructures were studied by Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS), respectively. The photoelectrochemical (PEC) properties of WO(3) porous nanostructures were studied in various alkaline electrolytes and compared with those of titania nanotubes. A new type of alkaline electrolyte containing a mixture of NaOH and KOH was proposed for the first time to the best of our knowledge and shown to improve the photocurrent response of the photoanodes. Here, we show that both the WO(3) nanostructures and titania nanotubes (used for comparison) exhibit superior photocurrent response in the mixture of NaOH and KOH than in other alkaline electrolytes. The WO(3) porous nanostructures suffered from surface corrosion resulting in a huge reduction in the photocurrent density as a function of time in the alkaline electrolytes. However, with a protective coating of ITO (100 nm), the surface corrosion of WO(3) porous nanostructures reduced drastically. A tremendous increase in the photocurrent density of as much as 340% was observed after the ITO was applied to the WO(3) porous nanostructures. The results suggest that the hybrid ITO/WO(3) nanocomposites could be potentially coupled with titania nanotubes in a multi-junction PEC cell to expand the light absorption capability in the solar spectrum for water splitting to generate hydrogen. 相似文献
A transition‐metal‐free reductive hydroxymethylation reaction has been developed, enabling the preparation of tetrahydroisoquinolines bearing C4‐quaternary centers from the corresponding isoquinolines. Deuterium labelling studies and control experiments enable a potential mechanism to be elucidated which features a key Cannizzaro‐type reduction followed by an Evans–Tishchenko reaction. When isoquinolines featuring a proton at the 4‐position are used, a tandem methylation‐hydroxymethylation occurs, leading to the formation of 2 new C?C bonds in one pot. 相似文献
Abstract A novel, fast, and easy method for synthesizing a carbon-supported Ni2P nanocomposite (C/Ni2P) is described. The process involves a reaction between a nickel salt, phosphoric acid, and a carbon source by utilizing microwave irradiation. The carbon source for the nanocomposite is from renewable supplies, namely, tannin and lignin. The method has successfully synthesized Ni2P nanoparticles dispersed in a carbon matrix with a particle size ranging from 20 to 50 nm in diameter. During the microwave process, tannin and lignin provided a reducing environment in the microwave irradiation process. The synthesized products are characterized by several characterization methods. The method showed that phosphoric acid, which is a nontoxic compound, could be used as an alternative P source for synthesizing Ni2P. The method is fast, easy, and an economical process to synthesize the carbon-coated Ni2P nanocomposite. 相似文献