Preparation of poly (styrene-co-4-vinyl pyridine) /silica nanoscale hybrids supported cyclopentadienyltitanium trichloride (CpTiCl3) catalyst and styrene polymerization

To obtain a novel support with practical value for metallocene catalyst (eta -C5H5)TiCl3 (CpTiCl3), poly (styrene-co-4-vinylpyridine) /SiO2 nanoscale hybrid material (SrP/SiO2) was firstly produced as support. After pretreatment by methylaluminoxane (MAO), the hybrid materials reacted with CpTiCl3. The results from SAXS, SEM and TEM indicated the morphology and structure of organic/inorganic hybrid materials, and the size of inorganic particle in hybrid was nanoscale. The results from IR and XPS showed that there were two possible cationic active species in the hybrid-supported catalyst, the polymerization results of styrene proved this possibility.

Simple preparation method of multilayer polymer films containing Pd nanoparticles

A simple route to the fabrication of multilayer films containing Pd nanoparticles is described. Following layer-by-layer assembly of PdCl42- and polycation, QPVP-Os (a quaternized poly(4-vinylpyridine) complexed with [Os(bpy)(2)Cl](2+/+)), on 4-aminobenzoic acid-modified glassy carbon electrodes, the three-dimensional Pd nanoparticle multilayer films are directly formed on electrode surfaces via electrochemical reduction of PdCl42- sandwiched between polymers. The growth of PdCl42- is easy on electrode surfaces by electrostatic interaction, and the assembly processes are monitored by cyclic voltammetry and UV-vis spectroscopy. The depth profile analyses by X-ray photoelectron spectroscopy verify the constant composition of the Pd nanoparticle multilayer films. Atomic force microscopy proves that the as-prepared Pd nanoparticles are uniformly distributed with an average particle diameter of 3-7 mn. The resulting Pd nanoparticle multilayer-modified electrode possesses high catalytic activity for the reduction of dissolved oxygen and oxidation of hydrazine compounds in aqueous solution.

Preparation and properties of a selenium-containing catalytic antibody as type I deiodinase mimic

Conversion of thyroxine (T-4) to 3,5,3'-triiodothyronine is an essential first step in controlling thyroid hormone action. Type I deiodinase (DI) can catalyze the conversion to produce the bulk of serum 3,5,3'-triiodothyronine. Acting as a mimic of DI, a selenium-containing catalytic antibody (Se-4C5) prepared by converting the serine residues of monoclonal antibody 4C5 raised against T4 into selenocysteines, can catalyze the deiodination of T4 with dithiothreitol (DTT) as cosubstrate. The mimic enzyme Se-4C5 exhibited a much greater deiodinase activity than model compound ebselen and another selenium-containing antibody Se-Hp4 against GSH. The coupling of selenocysteine with the combining pocket of antibody 4C5 endowed Se-4C5 with enzymatic activity. To probe the catalytic mechanism of the catalytic antibody, detailed kinetic studies were carried out in this paper. Investigations into the deiodinative reaction revealed the relationship between the initial velocity and substrate concentration. The characteristic parallel Dalziel plots demonstrated that Se-4C5-catalyzed reaction mechanism was ping-pong one, involving at least one covalent enzyme intermediate. The kinetic properties of the catalytic antibody were similar to those of DI, with K-m values for T-4 and DTT of approximately 0.8 muM and 1.8 muM, respectively, and a V-m value of 270 pmol per mg of protein per min. The activity could be sensitively inhibited by 6-propyl-2-thiouracil (PTU) with a K-i value of similar to 120 muM at 2.0 muM T-4 concentration. The PTU inhibition was progressively alleviated with the increasing concentration of added DTT, revealing that PTU was a competitive inhibitor for DTT.

Preparation and characterization of nanometer-sized CeO2/polystyrene hybrid material

Nanometer-sized CeO2/polystyrene hybrid material was prepared using reversed micelles microemulsion method. XRD analysis revealed that the CeO2 nanoparticles in polystyrene were amorphous. XPS patterns indicated that the hybrid material was not a simply physical mixture, but a certain strength of chemical bond between CeO2 nanoparticles and polystyrene existed. FTIR patterns revealed that the absorption of Ce-O bond in hybrid material was blue-shifted.

Preparation and application of a novel core-shell-particle-supported zirconocene catalyst

The use of functional groups bearing silica/poly(styrene-co-4-vinylpyridine) core-shell particles as a support for a zirconocene catalyst in ethylene polymerization was studied. Several factors affecting the behavior of the supported catalyst and the properties of the resulting polymer, such as time, temperature, Al/N (molar ratio), and Al/Zr (molar ratio), were examined. The conditions of the supported catalyst preparation were more important than those of the ethylene polymerization. The state of the supported catalyst itself played a decisive role in both the catalytic behavior of the supported catalyst and the properties of polyethylene (PE). IR and X-ray photoelectron spectroscopy were used to follow the formation of the supports. The formation of cationic active species is hypothesized, and the performance of the core-shell-particle-supported zirconocene catalyst is discussed as well. The bulk density of the PE formed was higher than that of the polymer obtained from homogeneous and polymer-supported Cp2ZrCl2/methylaluminoxane catalyst systems. (C) 2001 John Wiley & Sons, Inc.

Preparation, characterization and luminescent properties of MCM-41 type materials impregnated with rare earth complex

Hybrid materials incorporating Eu-(TTA)(3). 2H(2)O (7hereafter designated as Eu-TTA, with TTA: thenoyltrifluoroacetone) in unmodified or modified MCM-41 by 3-aminopropyl-triethoxysilane (APTES) were prepared by impregnation method. The obtained materials were characterized using X-ray diffraction (XRD), IR and diffuse reflectance spectroscopy and luminescence spectra. All the hybrid samples exhibited the characteristic emission bands of EU3+ under UV light excitation at room temperature, and the excitation spectra showed significant blue-shifts compared to the pure rare-earth complex. Although the red emission intensity in the modified hybrid was almost the half of the red emission intensity in the pure Eu-TTA complex at room temperature, the hybrid showed a much higher thermal stability due to the shielding character of the MCM-41 host.

Preparation and mass spectrometric study of egg yolk antibody (IgY) against rabies virus

Rabies virus was used as the antigen to immunize laying chickens. Anti-rabies virus immunoglobulin Y(IgY) was isolated from yolks of the eggs laid by these chickens using a two-step salt precipitation and one-step gel filtration protocol. The purified IgY was reduced with dithiothreitol, and heavy chains (HC) and light chains (LC) were obtained. In addition, the purified IgY was digested with pepsin and the fragment with specific antigen binding properties (Fab) was produced. Using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOFMS), the average molecular weights of IgY, HC, LC, and Fab were determined as 167 250, 65 105, 18 660, and 45,359 Da, respectively. IgY has two structural differences compared with mammalian IgGs. First, the molecular weight of the heavy chain of IgY is larger than that of its mammalian counterpart, while the molecular weight of the light chain of IgY is smaller. Second, upon pepsin digestion, anti-rabies virus IgY is degraded into Feb, in contrast to mammalian IgG, which has been reported to be degraded into F(ab')(2) under the same conditions. Copyright (C) 2001 John Wiley & Sons, Ltd.

Preparation and optical characterization of an organoeuropium-doped sol-gel transparent luminescence thin film

Binary and ternary europium complexes with dibenzplymethane (DBM) and 1,10-phenanthroline (phen) were synthesized and doped into a sol-gel luminescence thin film and polyvinylbutyral (PVB) film. The luminescent spectra and lifetime of the films were measured. The final results showed that Eu(III) characteristic emission bands were observed in the spectra of all the doped films. Longer lifetimes and a higher photo-stability were observed in SiO2:Eu(III) complex luminescent thin films than in PVB:Eu(III) complex films that contained a corresponding amount of pure complexes. Heat-stability tests showed that SiO2:Eu(III) complex thin films still showed certain fluorescence after heat-treatment at a temperature of 130 degreesC, while little fluorescence could be observed in PVB:Eu(III) complex films under a UV lamp. (C) 2001 Elsevier Science B.V. All rights reserved.

The preparation and property studies of transparent resins containing rare earth terbium(III) complex

The binary and ternary rare-earth terbium(m) complexes were introduced into the styrene/alpha -methylacrylic acid copolymerization system, and some optical resins that possess a high transparency in visible light region were obtained. The study of the optical property showed that they have good luminescent properties such as a high luminous intensity and a long luminous lifetime, In addition, we investigated the relationship among the transparency, the luminescent property of the copolymer, and the content of the components in the polymeric system. The results indicated that the optical resins can provide a relatively stable environment for composite rare earth complexes, which is good to exhibit the luminescent properties of rare earth complexes. At the same time, the rare earth complexes can offer the transparent resin a novel function.

Preparation of stable mesoporous silica FSM-16 from water glass in the presence of cetylpyridium bromide

The synthesis and characterization of the mesoporous materials FSM-16 (folded sheets mesoporous materials) with highly ordered structure in open-vessel by using cetylpyridium bromide (CPBr) and the single-layered polysilica Kanemite as new template and silicon source, respectively, has been investigated systematically. The hexagonal arrangements of uniformly size pores were characterized by FTIR. XRD. nitrogen adsorption. TG-DTA. SEM and TEM. Especially, the porous products with higher surface areas show remarkable thermal stability up to 1000 C. The potential application as carrier of catalysts or host-guest materials is anticipated. (C) 2001 Elsevier Science B.V. All rights reserved.

Preparation and luminescence properties of lanthanide complexes and their silica-based composites

Binary complexes of europium and terbium with N-propyl-4-carboxyphthalimide (NP) were prepared and characterized. The luminescence behaviors of the lanthanide complexes as well as their doped silica-based composites were investigated by fluorescence spectra. The results indicated that the lanthanide complexes showed fewer emission lines and slightly lower intensities in silica matrix than that of corresponding pure complexes. The lifetimes of the lanthanide complexes became longer when they were incorporated in silica matrix. (C) 2001 Elsevier Science B.V. All rights reserved.

Preparation of poly(4-vinylpyridine)/silica hybrids supported cyclopentadienyltitanium trichloride (CpTiCl3) catalyst and styrene polymerization

Poly(4 - vinylpyridine)/silica( PVP/SiO2) organic - inorganic nanoscale hybrid was prepared using sol - gel method, in which PVP was used as an organic component and TEOS as a SiO2 precusor, This hybrid was used as CpTiCl3 support. The XPS and IR measurements showed that two kinds of catalytic active site were formed through analyzing the interaction mode between support and CpTiCl3. The results of styrene polymerization showed that syndiotactic was the highest at 50 degreesC. The catalytic activity was 1.09 x 10(6) g PS/ (mol Ti . h) at 70 degreesC when n(Al)/n(Ti) = 1500. GPC results showed a bimodal molecular weight distribution.

Preparation and properties of nanocrystalline Yb2O3

Nanocrystalline Yb2O3 of various particle sizes was prepared using sol-gel method. XRD analysis shows that the prepared nanocrystalline Yb2O3 is cubic in structure with space group Ia3. TEM photographs indicate that Yb2O3 nanoparticles are basically spherical in shape. Calculation of crystallite size indicates that the average crystallite size of Yb2O3 increases with increasing calcination temperature, but the average crystal lattice distortion rate decreases with increasing calcination temperature and crystallite size. This result shows that the smaller the crystallite size, the bigger the crystal lattice distortion, and the worse crystal growth. Solubility test of Yb2O3 in nitric acid shows that the surface activity of Yb2O3 increases with decreasing crystallite size. Fourier Transform Infrared Spectrometer (FTIR) spectra reveal that nanocrystalline Yb2O3 has higher surface activity; than that of ordinary Yb2O3. Absorbance intensity of Yb-O bond of nanocrystalline Yb2O3 is weaker than that of ordinary Yb2O3, and the absorbance of Yb-O bond of nanocrystalline Yb2O3 is small blue-shifted.

Preparation of polyimide-BaTiO3 hybrid films by a dispersion process and their microstructure

Barium titanate (BaTiO3) powders with particle sizes of 30 similar to 50 nm were prepared from barium stearate, titanium alkoxides and stearic acid by stearic acid-gel method. Dispersing the agglomerate of BaTiO3 nanoparticles into poly(amic acid) solution followed by curing led to the formation of polyimide hybrid films. The hybrid films were transparent and well distributed with BaTiO3 nanoparticles when the BaTiO3 content was less than 1 wt%. Highly loaded hybrid film containing 30 wit % BaTiO3 was tough, had a smooth surface and possessed much higher dielectric and piezoelectric constants than the parent polyimide.

Preparation and spectra study of TiO2 gel doped with fluorescein

TiO2 gel doped with fluorescein was prepared by a sol-gel method, and the fluorescence of fluorescein and its effect on formation of the: gel were investigated with absorption, fluorescence, IR spectroscopies and TG-DTA analysis. The results indicated that FL incorporated into TiO2 gel had exhibited big changes compared to that in ethanol solution both in the absorption and the emission spectra, and the formation of TiO2 gel was influenced greatly by FL.