Complex-Emulsion synthesis of organo-inorganic amphiphilic sorbents with specific affinity for glucose

Granular organo-inorganic amphiphilic sorbents with specific affinity for glucose were synthesized with the aim of developing selective hemosorbents for efferent therapy of hyperglycemia. The sorbents were prepared in oil/water/oil complex emulsions by copolymerization of 2-hydroxyethyl methacrylate and ethylene glycol dimethacrylate on the surface of selenium nanoparticles stabilized with polyvinylpyrrolidone. The phases were stabilized with excess selenium/polyvinylpyrrolidone nanocomplexes. Optimum synthesis conditions ensuring formation of hybrid sorbents with the physicochemical properties required for performing efficient preparative hemosorption and plasma adsorption processes were found. The specific affinity for glucose was reached by modification of these sorbents via imprinting with template glucose molecules in the surface polymer layer and via introduction of boric acid as an affine ligand into the hybrid matrices.     

New hybrid chelating sorbents with grafted 3-aminopropionate groups based on mixed silicon,aluminum, titanium,or zirconium oxides

A series of new hybrid organo-inorganic sorbents with the 3-aminopropionate chelating group was synthesized. The synthesis includes the copolycondensation (sol—gel method) of tetraethoxysilane, 3-aminopropyltriethoxysilane, and several modifiers (MeSi(OEt)₃, EtSi(OEt)₃, Ti(OEt)₄, AlONO₃, ZrOCl₂) followed by carboxyethylation with acrylic acid. The obtained chelating sorbents were characterized by elemental analysis, FT-IR and ¹H NMR spectroscopy, and thermogravimetry. The N-carboxylated sorbents have a higher sorption capacity with respect to metal ions (0.5–0.9 mmol g⁻¹, pH 6.3, NH₄OAc, 20 °C) than the starting sorbents with the primary amino group (0.05–0.2 mmol g⁻¹) and manifest high selectivity for copper(II) ion extraction. __________ Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1783–1788, August, 2005.     

Organometallic functional materials based on siloxane block copolymers

Efficient synthetic approaches to designing nanoscale hybrid organo-inorganic composites containing metal (Zn, Cd, Cu, Zr) sulfides or oxides have been developed. These approaches were used to design the materials with specific electrophysical properties and controllable phase structure. The composites can be used as electroinsulating functional materials (adhesives, varnishes, coatings, and sealants) in microelectronics.     

Structure, hydrophobicity, and hydrothermostability of MCM-41 organo-inorganic mesoporous silicates silylated with dimethoxydimethylsilane and dichloromethylphenylsilane

Changes in the structure, hydrophobicity, and hydrothermal stability of organo-inorganic composite materials based on MCM-41 as a result of silylation with dimethoxydimethylsilane (DMODMS) and dichloromethylphenylsilane (DCMPS) were considered. Based on the data on the competitive adsorption of water and toluene it was shown, using the Weitkamp procedure, that the grafting of organosilyl groups affects the sorption properties of mesoporous materials. Hydrothermal treatment led to considerable changes in the structure and properties of the materials. The thermal stability of MCM-41 composites and changes in their hydrophilicity due to the grafting of DMODMS and DCMPS and hydrothermal treatment were studied by thermogravimetry.     

Structure and characteristics of chitosan cobalt-containing hybrid systems,the catalysts of olefine oxidation

Cobalt-containing hybrid organo-inorganic materials based on the chitosan-SiO₂, chitosan-Al₂O₃, and chitosan-cellulose systems were obtained. The surface structure and processes that occur during the formation of metal-containing materials, the catalytic properties of which were studied in the oxidation reactions of alkene, were investigated by EPR spectroscopy using a stable pH-sensitive nitroxyl radical, 4-dimethylamino-2-ethyl-5,5-dimethyl-2-(pyridin-4-yl)-2,5-dihydro-1H-imidazole-1-oxyl, as the adsorbed probe molecules.     

铝基氧化铜干法烟气脱硫及再生研究

采用浸渍法制备了XP型和DS型两种铝基氧化铜脱硫剂，并利用制得的脱硫剂进行了烟气循环脱硫-再生实验，同时利用BET、XRD和EPMA等方法研究了载体性质对脱硫剂性能的影响以及脱硫剂的表面微观结构在脱硫和再生过程的变化。实验和分析表明，用于制备脱硫剂的载体应同时具备较大的比表面积和合适的孔结构，实验条件下制得的铝基氧化铜脱硫剂的脱硫效率可达90％，该脱硫剂在多次循环脱硫-再生过程中性能保持稳定。     

Preparation and Ion-Exchange Properties of Mixed Zirconium(IV) Phosphate-Phosphonate Sorbents

Composite sorbents based on Zr(IV) phosphate-hydroxyethylidenediphosphonate with different phosphate-phosphonate ratio were prepared. These sorbents were characterized by elemental analysis, X-ray diffraction, and IR spectroscopy, and their ion-exchange sorption capacity for several transition metals and strontium was studied. The sorption capacity of these sorbents increases with increasing pH.     

Synthesis and Properties of Organo-Inorganic Composites Based on Daunomycin,Polyvinylpyrrolidone, and Selenium Nanoparticles

Two procedures for preparing organo-inorganic composites based on daunomycin, polyvinylpyrrolidone, and selenium nanoparticles were developed with the aim of preparing water-soluble nontoxic derivatives of daunomycin antitumor antibiotic. The first procedure consists in preliminary stabilization of selenium nanoparticles with polyvinylpyrrolidone, followed by addition of daunomycin, and the second procedure, in preliminary formation of a complex of daunomycin with polyvinylpyrrolidone, followed by selenium reduction. As shown by optical spectroscopy and by dynamic and static light scattering, the synthesis procedure does not influence the weight-average molecular mass of the synthesized composites, but influences the structural organization and size of particles and, correspondingly, their mobility. The composite prepared by the second procedure shows promise for antitumor therapy.     

Chelating Sorbents Prepared by the Modification of Silica Gel, Lichroprep RP-8 and Lichroprep RP-18 with Calcon and Their Application in the Analysis of Some Metal Ions

 Two new chelating sorbents for metal ions were prepared by the impregnation of chemically modified silicas LiChroprep RP-8 and RP-18 with ion pairs composed of the cation of Aliquat 336 and the anion of Calcon. The sorbents were compared with an analogous sorbent with a plain silica carrier containing the same ion pairs. A hypothesis for binding this ion pair by the surfaces of the applied carriers was presented. A higher stability of the two sorbents in comparison with that of the plain silica chelating sorbent was demonstrated. The sorbents obtained were applied for chromatographic separations of some chosen mixtures of some metal ions and for additional purification of aqueous solutions of alkali metals from trace amounts of heavy metals. The multiple use of the sorbents based on RP-8 and RP-18 in sorption–desorption processes of metal ions without deterioration of their sorption capacities was demonstrated. Received March 8, 2000. Revision March 5, 2001.     

One teflon-like channelled nanoporous polymer with a chiral and new uninodal 4-connected net: sorption and catalytic properties

Zn(C17H8F6O4) is the first example of a fluoro-lined nanotube organo-inorganic 3D polymeric chiral structure, which possesses two different types of isolated channels, one of them being laid out with a double spiral of CF3-groups from the ligand molecule; the structure is a new uninodal 4-connected net that only exists when bent ligands connect the centres, and the compound exhibits selective sorption and catalytic chiral recognition properties.     

Mechanism of a microwave-assisted polyol synthesis of nanosize CuInSe2 particles and their optical and photoelectric properties

Mechanism of the reaction in which CuInSe₂ nanoparticles are formed in synthesis by the microwaveassisted polyol method was studied. The morphology and optical properties of thin layers (films) produced from the synthesized CuInSe₂ nanoparticles and the morphology and photoelectric properties of composite films based on CuInSe₂ and [6,6]phenyl C61 butyric acid methyl ester were examined. It is shown that CuInSe₂ nanoparticles can be used to form a photo-absorbing layer in composite organo-inorganic solar cells.     

Kaolinite-based Hybrid Material from Interlayer Grafting of 1-(2-Hydroxyethyl)piperazine and Application to the Sensitive Voltammetric Detection of Lead

This work describes the synthesis of an organo-inorganic hybrid material and its application as low-cost electrode material for the electrochemical detection of trace levels of lead in contaminated water. The organo-inorganic hybrid material was obtained by the grafting of 1-(2-hydroxyethylpiperazine) (HEP) in the interlayer space of a natural kaolinite (K). The obtained organokaolinite (K-HEP) was characterized by XRD, FTIR and TGA-DTG techniques. XRD results in particular showed that the structure of the pristine kaolinite was not affected during the synthesis of K-HEP. It was also noticed from ¹³C NMR data that the structure of HEP was preserved during the synthesis process. Taking into account the affinity of the amine group on HEP molecule for lead ions, K-HEP was used to modify the surface of glassy carbon electrode (GCE) (GCE/K-HEP) in order to build a sensor for lead detection. The peak current of Pb(II) recorded on GCE/K-HEP was more intense compared to the signal recorded on bare GCE, and on natural kaolinite film modified GCE. Several parameters that can affect the stripping response were systematically investigated to optimize the sensitivity of the organokaolinite film modified electrode. Under optimized conditions, a calibration curve was obtained in the concentration range from 8.29 to 116.03 ppb; with a detection limit of 0.25 ppb (S/N=3). After the study of some interfering species on the electrochemical response of Pb(II), the developed sensor was successfully applied to the quantification of the same pollutant in tap water and spring water samples.     

Preparation of phenothiazine bonded silica gel as sorbents of solid phase extraction and their application for determination of nitrobenzene compounds in environmental water by gas chromatography-mass spectrometry

In this paper, two phenothiazine bonded silica (PTZ-Si) sorbents were prepared and used as sorbents of solid-phase extraction (SPE) for the determination of nitrobenzene compounds in environmental water samples by gas chromatography-mass spectrometry (GC-MS). Different synthesis routes were proposed to obtain high bonded amount of PTZ on the surface of silica gel. PTZ molecule was derived to its amino or acyl chloride derivatives for reacting with isocyanate or amino silane coupling agent, which was further reacted with the surface silanol groups of silica gel to obtain the PTZ-Si sorbents. The resultant PTZ-Si sorbents were characterized by nitrogen sorption porosimetry (NSP), Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to assure the successful bonding of PTZ on the surface of silica gel. Then the PTZ-Si sorbents were served as SPE sorbents for the enrichment of nitrobenzene compounds. Several parameters affecting the extraction performance were investigated. Under the optimized conditions, the proposed method was applied to the analysis of six nitrobenzene compounds in environmental water samples. Good linearities were obtained for all nitrobenzene compounds with R(2) larger than 0.9958. The limits of detection were found to be in the range of 0.06-0.3 ng/mL. The method recoveries of nitrobenzene compounds spiked in water samples were from 71.4% to 124.3%, with relative standard deviations (RSDs) less than 10.1%.     

Effect of technique of applying layers of metal acetylacetonates on acid-base and chromatographic properties of sorbents

A series of chromatographic sorbents, which differ by way of applying modifying chelates of acetylacetone was obtained. The acid-base and chromatographic properties of sorbents with thermally and chemically grafted layers of metal acetylacetonates were investigated. It was shown that the modifi cation of the mineral sorbents with metal acetylacetonates leads to a change in the surface acidity, as well as to an increase in the polarity and selectivity with respect to different classes of compounds.     

葡萄糖还原法制备CuCl/NaY吸附剂及其CO吸附和CO/H2分离性能

以NaY分子筛为载体,CuCl2为铜源,加入还原剂葡萄糖,在温和条件下制备CuCl/NaY吸附剂,通过变压吸附考察了该吸附剂对CO的吸附性能及CO/H2的分离性能。运用X射线衍射（XRD）、X射线光电子能谱（XPS）及程序升温还原（TPR）对吸附剂进行表征,结果表明采用葡萄糖还原法制备CuCl/NaY吸附剂,其制备条件温和,吸附剂表面的亚铜含量高,对CO的吸附及CO/H2的分离性能优越且稳定性好。     

New chelating sorbents based on pyrazolone containing amines immobilized on styrene-divinylbenzene copolymer-I Synthesis and analytical characterization

A series of new cheating sorbents has been prepared by modification of styrene-divinylbenzene copolymer with different pyrazolone-containing amines. The substances were characterized by elemental analysis and infared spectroscopy. The complexation ability of the sorbents towards alkali, alkaline-earth, transition and precious metals has been studied. The new sorbents may successfully be applied to the simultaneous preconcentration of alkaline-earth and transition elements in neutral medium and to the selective separation of precious metals in acidic medium.     

Effect of binder on the properties of iron oxide sorbent for hot gas desulfurization

The most difficult problem in hot gas desulfurization in Integrated Coal Gasification Combined Cycle (IGCC) is the pulverization of sulfur removal sorbents. Appropriate binders for hot gas sulfur removal sorbents can solve the pulverization problem. In this paper, six sorbents with binders of different argillaceous minerals were prepared by mechanical mixing method. Desulfurization behavior for hot gas desulfurization sorbents was investigated in a fixed-bed reactor. Result showed that sorbent NTKW2 with binder of clay had a better sulfidation performance. NTKW2 had a more stable performance than other sorbents in the continuous sulfidation-regeneration cycles. Sulfur capacity of sorbent remained the same in each cycle. The desulfurization efficiency and mechanical strength of NTKW2 were the best among the tested sorbents. The behavior of NTKW2 at different temperatures showed different performances, and the best reaction temperature was 550 ℃. Higher heat stability, sulfur capacity and desulfurization efficiency were found on NTKW2 in six continuous sulfidation-regeneration cycles.     

Conducting properties of a gel ionite modified with zirconium hydrophosphate nanoparticles

The organo-inorganic composites based on a strongly acid gel resin including zirconium hydro-phosphate nanoparticles and their aggregates were studied by impedance spectroscopy, electron microscopy, and standard contact porosimetry. The porous structure of the polymer was transformed under the action of the inorganic filler. The nanoparticles in the transport pores provided a three- to fivefold increase in the electric conductivity of the nanocomposites compared with the conductivity of the nonmodified ionite and a decrease in the percolation threshold. The nanocomposite ionites demonstrated stability against the accumulation of organic substances during electrodeionization to extract Na⁺ from low-concentrated solutions.     

Adsorption of Methylene Blue and Metanil Yellow Dyes by Modified Carbon Sorbents

Adsorption properties of carbon sorbents modified with glycolic and lactic acid oligomers and copolymers of these toward organic dyes of varied nature: Methylene Blue and Metanil Yellow were studied. Differences in the adsorption of the dyes by the modified sorbents, due to the nature of their surface, were found.     

黏结剂对铁酸锌脱硫剂在高温煤气中脱硫性能的影响

以硝酸铁、硝酸锌、氨水及黏结剂为主要原料,用共沉淀法制成六种铁酸锌脱硫剂。研究了各种黏结剂的加入对脱硫剂的尖晶石结构、硫容量和脱硫效果的影响,在固定床上对其进行脱硫试验。并用X射线衍射（XRD）、扫描电子显微镜(SEM)和气体吸附等测试手段,对脱硫剂的物相组成、结构、比表面积和孔容进行了表征。结果表明,用共沉淀法制备的铁酸锌,具有不受黏结剂影响的尖晶石结构,其颗粒属于微米级;添加高岭土黏结剂的脱硫剂的脱硫效果最好,添加硅藻土的脱硫剂的脱硫效果最差;不同黏结剂对脱硫剂的织构的影响不同;脱硫剂的反应活性和硫容量与其孔容的大小有关。