Preparation of water and alkali durable porous glass membrane coated on porous alumina tubing by sol-gel method

Composite porous glass membranes were prepared by the sol-gel method. A thin porous glass layer, about 2 μm thick, was coated on the surface of the porous ceramic tubing (Al₂O₃:99.9 wt.%, pore diameter: 200 nm). The composition of the porous glass layer of the composite membrane was SiO₂-ZrO₂. Considering from the fact that the desalination ratio of the feed aqueous NaCl solution (NaCl 0.5 wt.%) was about 90% by use of these membranes, they were defect-free. The best composition of the porous glass layer was 70 SiO₂-30 ZrO₂ from the standpoint of preparing membranes. These membranes had a large water and alkali durability. These membranes can be expected to apply to recovering dyes and paints from organic solvents and to be used as a gas separation membrane.     

Ordered SBA-15 nanorod arrays inside a porous alumina membrane

The growth of ordered nanorods of mesoporous SBA-15 inside a porous alumina membrane has been achieved for the first time by a simple sol-gel method. The obtained SBA-15 nanorods themselves have ordered hexagonal mesochannels with a size of about 6 nm and have been arranged to form hexagonal arrays by the limitation of pores of the alumina membrane. The synthesized alumina membrane with mesoporous SBA-15 inside combines the advantages of porous alumina membranes and mesoporous SBA-15 and provides fine and vertical mesochannels, which may serve as a new and efficient mold and lead to extensive applications in nanodevice fabrication, biomacromolecule separations, etc.     

Investigation of confined ionic liquid in nanostructured materials by a combination of SANS, contrast-matching SANS, and nitrogen adsorption

Small-angle neutron scattering (SANS), contrast-matching SANS, and nitrogen adsorption have been utilized to investigate the confined ionic liquid (IL) [bmim][PF(6)] phase in ordered mesoporous silica MCM-41 and SBA-15. The results suggest that the pores of SBA-15 are completely filled with IL whereas a small fraction of the pore volume, the pore "core", of MCM-41 is empty. The contrast-matching SANS measurements confirm the enhanced solubility of water in IL. In addition, they provide strong evidence that water does not enter the empty pore core of MCM-41, possibly because of the preferred orientation of the IL molecules in the adsorbed layer.     

Evaluation of the dehydration performance of zeolite NaA membrane on porous alumina tube by the alumina X-ray diffraction intensity.

A zeolite NaA (A-type zeolite of ca. 0.4 nm pore size; Linde Type A, LTA) membrane for the dehydration of alcohol was characterized by X-ray diffraction analysis (XRD). Also, the relationship between the X-ray absorption and the EtOH/H2O pervaporation (PV) dehydration performance (water selectivity and permeation flux) of the LTA membrane was first investigated. The LTA membranes used here were gel-synthesized hydrothermally on an alumina porous support tube. Since diffraction lines from the alumina generate from a deeper layer than those of the LTA crystal, and are absorbed by both the surface LTA crystal and materials embedded in the alumina porous support, the alumina (113) diffraction line was intensively monitored to estimate the overall X-ray absorption by the LTA membrane. The intensity of the alumina (113) diffraction line showed a good correlation with the PV dehydration performance of the LTA membrane, that is, lower values with the water selectivity and higher values with the permeation flux. The lower diffraction intensity means stronger X-ray absorption by the LTA membrane. The major factor causing the difference in the X-ray absorption is the thickness or quantity of materials embedded in an alumina porous support, rather than those of the surface LTA crystal. These phenomena can be used conveniently (without real PV experiments) to determine the EtOH/H2O PV dehydration performance of the LTA membrane.     

Preparation of monodisperse SiO2 nanoparticles by membrane emulsification using ideally ordered anodic porous alumina

Monodisperse SiO2 particles of nanometer dimensions were fabricated by membrane emulsification using ideally ordered anodic porous alumina. For the preparation of monodisperse emulsion droplets, the dispersed phase was pressed through a porous alumina membrane into the continuous phase. After solidification treatment of the emulsion droplets, prepared spherical SiO2 nanoparticles with uniform sizes were obtained. From scanning electron microscope observation of the obtained particles, it was confirmed that the size distribution of SiO2 nanoparticles is relatively narrow.     

Permeation flux of organic molecules through silica-surfactant nanochannels in a porous alumina membrane.

The permeation fluxes of phenol, benzene sulfonate (BS) and benzene disulfonate (BDS) through a porous anodic alumina membrane with the perpendicularly oriented silica-surfactant nanochannel assembly membrane (NAM) were measured in water-ethanol mixture media. The permeation flux depended on solute charges and on solvent composition. As the ethanol ratio increased, the fluxes of BS and BDS increased and the flux of phenol decreased. The results of extraction/elution experiments also depended on the solute charges and the solvent composition. Chromatographic experiments in n-hexane showed that dipole and hydrophobic interactions affect the retention of solutes. Permeation of the solute across the NAM in water-ethanol mixture is likely to be determined by various factors such as dipole interaction, hydrophobic interaction, solvation, and anion-exchange efficiencies.     

Diffusion of metal complexes inside of silica-surfactant nanochannels within a porous alumina membrane

The present paper describes diffusivities of a series of metal complexes inside of silica-surfactant nanochannels (channel diameter = 3.4 nm), which were formed within a porous alumina membrane by a surfactant-templated method using cetyltrimethylammonium bromide (CTAB) as a template surfactant. The metal complexes used in this study were Fe(CN)6(3-), Ru(NH3)6(3-), ferrocenecarboxylic acid (Fc-COO-), (ferrocenylmethyl)-trimethylammonium (Fc-NMe3+), N,N-(dimethylamminomethyl)ferrocene (Fc-NMe2), and ferrocene methanol (Fc-OH). Apparent diffusion coefficients of these metal complexes were estimated by measuring their mass transports through the silica-surfactant nanochannels. The estimated apparent diffusion coefficients were on the order of 10(-11) cm2 s(-1) for Fe(CN)6(3-) and Ru(NH3)6(3-), and these values were five orders of magnitude smaller than those in a bulk aqueous solution. For the ferrocene derivatives, the apparent diffusion coefficients of charged ferrocene derivatives are almost the same (5.3 x 10(-11) cm2 s(-1) for Fc-COO- and 5.4 x 10(-11) cm2 s(-1) for Fc-NMe3+), whereas neutral ferrocene derivatives (Fc-NMe2 and Fc-OH) show faster diffusion than the charged species. In addition, the apparent diffusion coefficient of Fc-NMe2 (27 x 10(-11) cm2 s(-1)) was about three times larger than that of Fc-OH (10 x 10-11 cm2 s(-1)). The difference in these diffusion coefficients is discussed by considering the mesostructure of the silica-surfactant nanochannels, that is, an ionic interface with cationic head groups of CTA and their counteranions, a hydrophobic interior of the micellar phase, and a silica framework. As a result, it is inferred that the slow diffusivities of the charged metal complexes are due to the electrostatic interaction between the charged species and the ionic interface, whereas less interaction between neutral ferrocenes and the ionic interface causes distribution of metal complexes into the hydrophobic micellar phase, which is a less viscous medium compared to the ionic interface, resulting in the faster diffusivities of the neutral species.     

吸附柱分离-离子色谱法测定锑中微量硫

建立了吸附柱分离-离子色谱法测定锑样中微量硫的方法.方法采用王水,氢溴酸,浓HCl等试剂将锑样溶解,并使锑样中的硫转化为SO42-,低温加热蒸干,使锑完全挥发.然后在氧化铝柱上过柱,用氨水洗脱,最后将处理好的样品溶液注入离子色谱系统进行分析测定.优化了离子色谱操作条件,以流速为1.2 mL/min的3.5 mmol/L的Na2CO3与1.0 mmol/L的NaHCO3作为淋洗液,对标准液和样品溶液的测定,线性范围为0.2～100 μg/mL,检出限为0.2 μg/mL,回收率为92.9%～103.1%,该法适合锑样中微量硫的测定.     

Extraction mechanisms of charged organic dye molecules into silica-surfactant nanochannels in a porous alumina membrane

Extraction mechanisms of charged organic dye molecules are examined for an assembly of silica-surfactant nanochannels with a channel diameter of 3.4 nm, which is formed inside the pores of an anodic alumina membrane by a surfactant-template method. Experimental results confirm that the extraction mechanism depends on the sign of a charge of the dye molecules. The extraction of the cationic rhodamine 6G is predominantly caused by an ion-pair extraction process, whereas an anion-exchange process is mainly responsible for the extraction of the anionic sulforhodamine B. These extraction mechanisms are discussed by considering the microstructures of the silica-surfactant nanochannels.     

Fluoride wastewater treatment by adsorption onto metallurgical grade alumina

The adsorption of fluoride onto metallurgical grade alumina (to produce Al) was investigated under different conditions: pH, contact time and adsorbent concentration. Data were evaluated with the aim of developing an alternative treatment technology for washing wastewater arising from an Aluminum can production plant. Kinetics and adsorption isotherms data have been also produced Sorption is greatly affected by pH and the best condition for fluoride removal are obtained at pH 5-6 and alkalinity competes successfully with fluoride ions for the exchange sites. Experiments with fixed beds indicate that fluoride is removed from wastewater by metallurgical-grade alumina with a capacity of 12.21 mg of F per gram and adsorption increases of about 25% at appropriate pH. The Mass Transfer Zone at 5% of the breakthrough occupies 70.6% of the total column length. The optimization of aluminum precipitation by pH adjustment and with different precipitant agents has been done.     

Characterisation of zeolitic catalysts by the adsorption of molecular probes

Few examples of the characterisation by FTIR spectroscopy supplemented by the use of CO₂, CO and NO molecular probes of acid, base and redox centres in zeolites (NaX and NaY) and zeolitetype (HSAPO-34, a silicon-aluminophosphate, and CoAPO-18, a cobalt-aluminophosphate) catalysts, are illustrated.     

Preparation of unsupported alumina membrane by sol-gel techniques

Unsupported alumina membranes were prepared by sol-gel technique using aluminum isoproxide. The influence of the hydrolysis conditions, the type and concentration of peptizant acid on the boehmite sols has been studied. The suitable hydrolysis temperature for the aluminum isoproxide was above 50°C. Crack-free unsupported alumina membranes were obtained by rapid gelation processing of sols. The boehmite gel membrane and γ-Al₂O₃ membrane formed exhibited (020) and (440) preferred orientation.     

SANS and SAXS analysis of charged nanoparticle adsorption at oil-water interfaces

A systematic study of the adsorption of charged nanoparticles at dispersed oil-in-water emulsion interfaces is presented. The interaction potentials for negatively charged hexadecane droplets with anionic polystyrene latex particles or cationic gold particles are calculated using DLVO theory. Calculations demonstrate that increased ionic strength decreases the decay length of the electrostatic repulsion leading to enhanced particle adsorption. For the case of anionic PS latex particles, the energy barrier for particle adsorption is also reduced when the surface charge is neutralized through changes in pH. Complementary small-angle scattering experiments show that the highest particle adsorption for PS latex occurs at moderate ionic strength and low pH. For cationic gold particles, simple DLVO calculations also explain scattering results showing that the highest particle adsorption occurs at neutral pH due to the electrostatic attraction between oppositely charged surfaces. This work demonstrates that surface charges of particles and oil droplets are critical parameters to consider when engineering particle-stabilized emulsions.     

Perforated organometallic nanotubes prepared from a Rh N-heterocyclic carbene using a porous alumina membrane

Fabrication of perforated organometallic nanotubes using a di-rhodium bis(N-heterocyclic carbene) complex by a simple nanoporous template wetting technique is described along with characterization data from scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), proton NMR and Mass spectroscopy.     

Characterisation of porous materials for bioseparation

A set of chromatographic materials for bioseparation were characterised by various methods. Both commercial materials and new supports presenting various levels of rigidity were analysed. The methods included size-exclusion and capillary phenomena based techniques. Both batch exclusion and inverse size-exclusion chromatography were used. Gas adsorption, mercury porosimetry and thermoporometry were applied as well as a new method based on water desorption starting from the saturated state. When the rigidity of adsorbents is high enough, the agreement is reasonable between the values of the structural parameters that were determined (surface area, porosity, and pore size) by various methods. Nevertheless, a part of macroporosity may not be evidenced by inverse size-exclusion chromatography whereas it is visible by batch exclusion and the other methods. When the rigidity decreases, for example with soft swelling gels, where standard nitrogen adsorption or mercury porosimetry are no more reliable, two main situations are encountered: either the methods based on capillary phenomena (thermoporometry or water desorption) overestimate the pore size with an amplitude that depends on the method, or in some cases it is possible to distinguish water involved in the swelling of pore walls from that involved in pore filling by capillary condensation.     

Methanol adsorption by amorphous silica alumina in the critical temperature range

The methanol adsorption capacity of an amorphous silica-alumina was measured using an equilibrium technique. The experimental temperature range was of 140 to 260°C and the pure methanol pressure range was 0.1 to 1.2 MPa. A multilayer adsorption was found, also for temperatures above the critical temperature of the adsorbate. Based on the Jovanovic adsorption model, the mean residence times of the adsorbed molecules were calculated. Surprisingly, the heat of adsorption was found to be independent of the temperature in the multilayer adsorption range.Symbols Units a parameter defined by Equation (7) - a parameter defined by Equation (10) Pa - a(T) parameter in the Peng-Robinson equation Pa/(mol/m³)² - b parameter defined by Equation (8) - b parameter defined by Equation (11) Pa^–1 - b(T) parameter in the Peng-Robinson equation m³ mol^–1 - c constant in the BET equation - k Boltzmann constant, being 1.3806 · 10^–23 JK^–1 - K characteristic constant in the Peng-Robinson equation - m mass of one adsorbate molecule kg - p pressure Pa - q adsorption capacity g/g - Q heat of adsorption J mol^–1 - R gas constant, being 8.314 J mol^–1 K^–1 - T absolute temperature K - V molar volume m³ mol^–1 - x relative pressure (=p/p ₀) - active molecule area m² - residence time s - acentric factor     

Low-temperature ionic liquids immobilized in porous alumina

The pores in an aluminum oxide matrix can be completely filled with 1-alkyl-3-methylimidazolium tetrafluoroborates, hexafluorophosphates, triflates, and bis(trifluoromethylsulfonyl)imides. This possibility can be utilized to produce solid electrolytes for batteries and fuel cells.     

Impurity-driven defect generation in porous anodic alumina

We report that the morphologies of porous anodic alumina films are affected significantly by the presence of small amounts of copper impurity in the aluminium substrate, resulting in generation of defects during anodizing in phosphoric acid over a wide range of conditions. The copper is accumulated at the metal/film interface and transported preferentially to triple points of the alumina cells, where oxygen gas is generated leading to development of gas-filled voids.     

Nanoscale membrane electrode assemblies based on porous anodic alumina for hydrogen–oxygen fuel cell

In this paper, we demonstrate that nanoscale membrane electrode assemblies, functioning in a H₂/O₂ fuel cell, can be fabricated by impregnation of anodic alumina porous membranes with Nafion® and phosphotungstic acid. Porous anodic alumina is potentially a promising material for thin-film micro power sources because of its ability to be manipulated in micro-machining operations. Alumina membranes (Whatman, 50 μm thick, and pore diameters of 200 nm) impregnated with the proton conductor were characterized by means of scanning electron microscopy, X-ray diffraction, and thermal analysis. The electrochemical characterization of the membrane electrode assemblies was carried out by recording the polarization curves of a hydrogen–oxygen 5 cm² fuel cell working at low temperatures (25?÷?80 °C) in humid atmosphere. Our assemblies realized with alumina membranes filled with phosphotungstic acid and Nafion® reach respectively the peak powers of 20 and 4 mW/cm² at room temperature using hydrogen and oxygen as fuel and oxidizer.