Thermal treatment on composite γ-zirconium phosphate-silica

The prepared amorphous γ-ZrP\SiO₂ composite had a complicated composition, since a part of γ-ZrP is converted to α-form during the exfoliation of it. The γ-ZrP\SiO₂ composite have specific surface area of 421 m²g^–1. The acidic P–OH groups of the lamellae species placed on the surface (it is ≈1.0 meq g^–1), do not destroy until the temperature of 1030 K. During the thermal treatment the total mass loss of 7.79% was found. This value corresponds to 0.42 mole of H₂O per molecule unit. The water loss process was found very slow, because of the placing of bilamellar species in the composite.     

Liquid phase oxidation of p-chlorotoluene to p-chlorobenzaldehyde over cobalt-doped mesoporous titania with a crystalline framework

Cobalt-doped mesoporous titania with a crystalline framework synthesized by surfactant templating method presented highly selective (99%) and reasonable conversion rate (49%) of catalytic oxidation of para-chlorotoluene to para-chlorobenzaldehyde in acetic acid using aqueous hydrogen peroxide as oxidant for the first time. Recycling of the catalyst indicates that the catalyst can be used a number of times without losing its activity to a greater extent. By contrast, cobalt-doped mesoporous titania without a crystalline structure and cobalt doped the commercial titania, Degussa P25 prepared by impregnation method with the similar concentration of cobalt were found inactive. The effects of catalyst concentration, reaction time, reaction temperature, and solvents on the performance of the catalyst were also investigated.     

Effects of Polymer Bridging and Electrostatics on the Rheological Behavior of Aqueous Colloidal Dispersions†

Effects of a low molecular weight physically adsorbed polyethylene oxide (PEO) and the range of the electrostatic repulsion on the rheological behavior of silica dispersions (as a model system) has been investigated. Particular attention is given to the evolution of the rheological behavior with increasing the polymer concentration in the system and also effectiveness of the polymer as a dispersant under extreme conditions (high ionic strength). Results indicate that at small separation distances and low polymer coverage, the polymer chains are long enough to adsorb on the surface of two particles simultaneously causing bridging flocculation in the system and hence increasing the viscosity and linear viscoelastic functions of the dispersion. A significant increase was observed in the viscosity of the dispersion at salt concentrations high enough to eliminate electrostatics between the particles. Under these conditions,the viscosity of the system increased significantly when PEO was added to the dispersion showing that at high electrolyte concentrations, a neutral polymer such as PEO is not able to stabilize the system.     

An optical fibre pH sensor based on dye doped mesostructured silica

This paper describes the synthesis and optical pH sensing properties of a pH indicator dye activated mesostructured silica coated optical fibre. The pH-sensitive dye bromothymol blue was incorporated into the mesostructure sol precursor and thin films/coatings were used for pH-sensing applications without prior removal of the surfactant. The pH sensitivity range and operating wavelength were analysed by absorption measurements on layer dip-coated on glass slides. The pH sensing properties of coated optical fibre were tested by evanescent wave method. Experiments were carried out by using a series of solutions of known pH. No leaching was observed (except at very high pH) and an excellent reversibility was obtained between pH=2 and 5.     

Evaluation of Polycation-Stabilized Lactate Oxidase in a Silica Sol–Gel as a Biosensor Platform

 Whereas glucose oxidase and related proteins are encapsulated readily in silica sol–gels, α-hydroxy enzymes such as lactate oxidase (LOx), are reported to be damaged by electrostatic interaction with these matrices. Based on a previous report, poly(ethyleneimine), PEI, was evaluated as a protecting compound under conditions suited to analytical measurements. With LOx and PEI co-encapsulated in a silica sol–gel, the enzyme retained 62% of its initial activity after 20 days. In the absence of PEI, activity was lost during the processing. Batch analytical measurements with enzyme-doped sol–gel yielded a linear response over the range 0.5–2.0 mM lactate and a detection limit of 0.03 mM lactate. Both simple incorporation of LOx in a silica sol–gel and an alternative protection method, blocking the ion-exchange sites on silica with La(III), failed. These negative results supported the hypothesis that the efficacy of PEI was related to its formation of a protective sheath around the enzyme. Author for correspondence. E-mail: coxja@muohio.edu Received July 29, 2002; accepted December 15, 2002 Published online May 19, 2003     

Synthesis and adsorption properties of gold nanoparticles within pores of surface‐functional porous polymer microspheres

Mesoporous polymer microspheres with gold (Au) nanoparticles inside their pores were prepared considering their surface functionality and porosity. The Au/polymer composite microspheres prepared were characterized by transmission electron microscope (TEM), X‐ray diffraction (XRD), and Brunauer–Emmett–Teller (BET) techniques. The results showed that the adsorption of Au nanoparticles could be increased by imparting the pore structure and surface‐functional groups into the supporting polymer microspheres (in this study, poly (ethylene glycol dimethacrylate‐co‐acrylonitrile) and poly (EGDMA‐co‐AN) system). Above all, from this study, it was established that the porosity of the polymer microspheres is the most important factor that determines the distribution and adsorption amount of face‐centered cubic (fcc) Au nanoparticles in the final products. Our study showed that the continuous adsorption of Au nanoparticles with the aid of the large surface area and surface interaction sites formed more favorably the Au/polymer composite microspheres. The BET measurements of Au/poly(EGDMA‐co‐AN) composite microspheres reveals that the adsorption of Au nanoparticles into the pores kept the pore structure intact and made it more porous. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5627–5635, 2004     

掺Eu3+硅基材料的发光性质

通过溶胶－凝胶技术制备了掺Eu^3 的硅基材料并测试了其三维荧光光谱、激光谱和发射光谱，结果显示，最佳激发波波长为350nm,最强荧光波长为620nm；在350nm光激发下的发射光谱显示Eu^3 的特征发射光谱，产生4条谱带，分别是577nm(^5D0-^7F0)，588nm(^5D0-^7F1),596nm(^5D0-^7F1)和610nm(^5D0-^7F2)。     

Modeling of environmentally significant interfaces: Two case studies

When some parameters cannot be easily measured experimentally, mathematical models can often be used to deconvolute or interpret data collected on complex systems, such as those characteristic of many environmental problems. These models can help quantify the contributions of various physical or chemical phenomena that contribute to the overall behavior, thereby enabling the scientist to control and manipulate these phenomena, and thus to optimize the performance of the material or device. In the first case study presented here, a model is used to test the hypothesis that oxygen interactions with hydrogen on the catalyst particles of solid oxide fuel cell anodes can sometimes occur a finite distance away from the triple phase boundary (TPB), so that such reactions are not restricted to the TPB as normally assumed. The model may help explain a discrepancy between the observed structure of SOFCs and their performance. The second case study develops a simple physical model that allows engineers to design and control the sizes and shapes of mesopores in silica thin films. Such pore design can be useful for enhancing the selectivity and reactivity of environmental sensors and catalysts. This paper demonstrates the mutually beneficial interactions between experiment and modeling in the solution of a wide range of problems.     

Influence of Particle Morphology and Flow Conditions on the Dispersion Behavior of Fumed Silica in Silicone Polymers

The dispersion behavior of agglomerates of several grades of fumed silica in poly(dimethyl siloxane) liquids has been studied as a function of particle morphology and applied flow conditions. The effects of primary particle size and aggregate density and structure on cohesivity were probed through tensile and shear strength tests on particle compacts. These cohesivity tests indicated that the shear strength of particle compacts was two orders of magnitude higher than the tensile strength at the same overall packing density. Experiments carried out in both steady and time‐varying simple‐shear flows indicate that dispersion occurs through tensile failure. In the steady‐shear experiments,enhanced dispersion was obtained at higher levels of applied stress and, at comparable levels of applied stress, dispersion was found to proceed faster at higher shear rates. Experiments conducted in time‐varying flows further corroborated the results obtained in tensile cohesivity tests. Experiments in which the mean and maximum stresses in the time‐varying flows were matched to the stresses produced in steady shear flows highlight the influence of flow dynamics on dispersion behavior.     

Separation of Monovinyl and Divinyl Protochlorophyllides Using C30 Reverse Phase High Performance Liquid Chromatography Column: Analytical and Preparative Applications

A new, high performance liquid chromatography method has been developed for the separation of monovinyl- and divinyl-protochlorophyllides, using commercially available, C₃₀ reverse phase column and isocratic elution. This method can be used both for analytical applications and preparative scale purification of monovinyl- and divinyl-protochlorophyllides using the same column where submilimolar concentrations of the crude protochlorophyllide extract can be separated in one run. The purity of the obtained protochlorophyllides was demonstrated by spectroscopic methods, as well by the formation of aggregates in toluene.