Study on the synthesis and performance of hydrogels with ionic monomers and montmorillonite

Two series of the nanocomposite hydrogels were synthesized by in-situ solution polymerization. One pre-gel solution was obtained by directly dispersing the montmorillonite (MMT) powder into aqueous monomer solution and the other pre-gel solution was obtained by mixing monomer aqueous solution and the dispersion of MMT. The structure and performance of two series of hydrogels in dry state were studied by XRD, Raman spectroscopy, TEM and Al-27 MAS NMR. Compressing test results showed that the gel strength of the hydrogels prepared by the latter method was much higher than that by the former method. When acryloyloxyethyl trimethyl ammonium chloride (DAC) was introduced into the system, hydrogels with excellent nanostructure could be synthesized. The result of Al-27 MAS NMR suggested that the chemical environment of aluminum in MMT was changed by the introduction of DAC due to the interaction between the groups of DAC and MMT layers. Thus, the combination of copolymerizing with strong polar monomers and using the dispersion of MMT were the effective ways to obtain tranocomposite hydrogel of MMT and ionic monomers. The nanostructure of the hydrogel improved the gel strength, while the swelling ratio of the hydrogel depended on synergic effects of multifunctional groups.

The critical lowest molecular weight for PEG to crystallize in cross-linked networks

Poly(ethylene glycol) (PEG) networks were synthesized by gamma-irradiation. The crystalline behavior of PEG was investigated by differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD). It was shown that the crystallinity of PEG is dramatically lower in the cross-linked, networks than in pure PEG. When the molecular weight of PEG in the networks decreased to 1000, it could not crystallize at all. Moreover, we also found that the melting temperature of PEG is greatly affected by the presence of a cross-linked network.

Rapid synthesis of Mn0.65Zn0.35Fe2O4/SiO2 homogeneous nanocomposites by modified sol-gel auto-combustion method

MnZn-ferrite/SiO2 nanocomposites with different silica content were successfully fabricated by a novel modified sol-gel auto-combustion method using citric acid as a chelating agent and tetraethyl orthosilicate (TEOS) as the source of silica matrix. The auto-combustion nature of the dried gel was studied by X-ray diffraction (XRD), Infrared spectra (IR), thermogravimetry (TG) and differential thermal analysis (DTA). Transmission electron microscope (TEM) observation shows that the MnZn-ferrite particles are homogeneously dispersed in silica matrix after auto-combustion of the dried gels. The magnetic properties vary with the silica content. The transition from the ferromagnetic to paramagnetic state is observed by Mossbauer spectra measurement with the increasing silica content. Vibrating sample magnetometer (VSM) shows that the magnetic properties of Mn0.65Zn0.35Fe2O4/SiO2 nanocomposites strongly depend on the silica content.

A room-temperature ionic-liquid-templated proton-conducting gelatinous electrolyte

Novel proton-conducting gelatinous electrolytes templated by room-temperature ionic liquid (RTIL) 1-butyl-3-methyl-imidazolium-tetrafluoroborate (BMImBF(4)) have been prepared in methylsisesquioxane backbone containing H3PO4, and the influences of the RTIL on the structure, morphology, thermal stability, and electrochemical properties of the gelatinous electrolytes have been examined. X-ray diffraction and scanning electron microscopy proved that BMImBF(4) acted as structure-directing template during the sol-gel process of methyl-trimethoxysilane. X-ray photoelectron spectra and infrared spectroscopy demonstrated that the hydrogen-bonding was formed between BMImBF(4) and H3PO4. The electrolytes had good thermal stability up to 300 degreesC and showed superior mechanical and electrochemical properties. A room-temperature conductivity of 1.2 x 10(-3) S cm(-1) was obtained for the electrolyte at the molar ratio of RTIL/Si/H3PO4 0.3/1/1, and its electrochemical window was up to 1.5 V.

TiO2-SnO2复合凝胶的水-乙醇蒸汽吸附动力学研究

中国科学院山西煤炭化学研究所

TiO2-SnO2复合凝胶的结构表征及其吸附与催化性能研究

中国科学院山西煤炭化学研究所

Carbon ceramic electrodes bulk-modified with nanoparticles of ferrocenebutyrate-intercalated Mg-Al layered double hydroxide

Ferrocenebutyrate-intercalated layered double hydroxide (FcLDH) was prepared by the coprecipitation method and characterized by PXRD, FTIR, TEM and elemental analysis. FcLDH nanoparticles in deionized water were deposited onto the surface of graphite powder to yield graphite powder-supported FcLDH, which was subsequently dispersed into methyltrimethoxysilane-derived gels to fabricate surface-renewable, stable, rigid carbon ceramic electrodes containing the electroactive ferrocenyl group. Cyclic voltammetric study revealed that peak currents of the FcLDH-modified electrode were diffusion-con trolled in 0.1 mol l(-1) KCl aqueous solution. In addition, the formal potential of the modified electrode is related to the activity of chloride ion with a Nernst slope of 56 mV per decade.

Sol-gel derived carbon ceramic electrode containing methylene blue-intercalted alpha-zirconium phosphate micro particles

Methylene blue-intercalated a-zirconium phosphate (MBZrP) micro particles in deionized water were deposited onto the surface of graphite powder to prepare graphite powder-supported MBZrP, which was subsequently dispersed into methyltrimethoxysilane-derived gels to yield a conductive composite. The composite was used as electrode material to fabricate a surface-renewable, rigid, leak-free carbon ceramic composite electrode, bulk-modified with methylene blue (MB). In the configuration, alpha-zirconium phosphate was employed as a solid host for MB, which acted as a catalyst. Graphite powder ensured conductivity by percolation, the silicate provided a rigid porous backbone and the methyl groups endowed hydrophobicity and thus limited the wetting section of the modified electrode. Peak currents of the MBZrP-modified electrode were surface-confined at low scan rates but diffusion-controlled at high scan rates. Square-wave voltammetric study revealed that MBZrP immobilized in carbon ceramic matrix presented a two-electron, three-proton redox process in acidic aqueous solution with pH ranged from 0.44 to 2.94. In addition, the chemically modified electrode showed an electrocatalytic activity toward nitrite reduction at +0.15 V (vs. Ag/AgCl) in acidic aqueous solution (pH=0.44). The linear range and detection limit are 1 x 10(-6)-4 x 10(-3) mol L-1 and 1.5 x 10(-7) mol L-1, respectively.

Photoluminescence of organic-inorganic hybrid SiO2 xerogels

Organic-inorganic hybrid SiO2 xerogels were prepared by the sol-gel method under various preparation conditions and compositions by using tetraethoxysilane (TEOS), (3-aminopropyl) triethoxysilane (A-PS), (3-glycidoxypropyl) trimethoxysilane (GPS), organic acid (CH3COOH) and inorganic acids (HCl, HNO3, H2SO4) as the main precursors. Luminescence and FT-IR spectra were used to characterize the resulted hybrid SiO2 xerogels. The result of FT-IR spectrum shows that the xerogels are composed of non-crystalline -Si-O-Si- networks containing some organic groups such as -NH, -CH and -OH. Under the excitation of 365 nm, all the hybrid xerogels exhibit strong luminescence in the blue region, but the emission intensity and position depend on the starting precursor compositions to a large extent. Suitable amount of polyethylene glycol (PEG500 and PEG10000) in the hybrid xerogels can enhance the emission intensity. Additionally, the emission intensity of the hybrid xerogels increases with heat treatment temperature in the range of ambient to 200degreesC, and vacuum condition is also able to enhance the emission intensity.

Cupric hexacyanoferrate nanoparticle modified carbon ceramic composite electrodes

Graphite powder-supported cupric hexacyanoferrate (CuHCF) nanoparticles were dispersed into methyltrimethoxysilane based gels to produce a conducting carbon ceramic Composite, which was used as electrode material to fabricate surface- renewable CuHCF-modified electrodes. Electrochemical behavior of the CuHCF-modifled carbon ceramic composite electrodes was characterized using cyclic and square-wave voltammetry. Cyclic voltammograms at various scan rates indicated that peak currents were surface-confined at low scan rates. In the presence of glutathione, a clear electrocatalytic response was observed at the CuHCF-modified composite electrodes. In addition, the electrodes exhibited a distinct advantage of reproducible surface-renewal by simple mechanical polishing on emery paper, as well as ease of preparation, and good chemical and mechanical stability in a flowing stream.

Carbon ceramic electrodes modified with sub-micron particles of new methylene blue (NMB) intercalated alpha-zirconium phosphate

New methylene blue-intercalated a-zirconium phosphate (NMBZrP) was synthesized in the presence of n-butylamine and characterized by powder XRD, FTIR, TEM and elemental analysis. Sub-micron particles of NMBZrP in deionized water were apt to deposit onto the surface of graphite powder to yield graphite powder-supported NMBZrP, which was subsequently dispersed into methyltrimethoxysilane-derived gels to fabricate surface-renewable, stable, rigid carbon ceramic electrodes containing new methylene blue. Cyclic voltammetric studies revealed that peak currents of the NMBZrP-modified electrode were surface-confined at low scan rates but diffusion-controlled. at high scan rates. In addition, NMBZrP immobilized in a carbon ceramic matrix presented a two-electron, three-proton redox process in acidic aqueous solution in the pH range from 0.52 to 3.95.

Sol-gel derived carbon ceramic electrode bulk-modified with tris(1,10-phenanthroline-5,6-dione)iron(II) hexafluorophosphate and its use as an amperometric iodate sensor

A surface-renewable tris (1,10-phenanthroline-5, 6-dione) iron (II) hexafluorophosphate (FePD) modified carbon ceramic electrode was constructed by dispersing FePD and graphite powder in methyltrimethoxysilane (MTMOS) based gels. The FePD-modified electrode presented pH dependent voltammetric behavior, and its peak currents were diffusion-controlled in 0.1 mol/L Na2SO4 + H2SO4 solution (pH = 0. 4). In the, presence of iodate, clear electrocatalytic reduction waves were observed and thus the chemically modified electrode was used as an amperometric sensor for iodate in common salt. The linear range, sensitivity, detection limit and response time of the iodate sensor were 5 x 10(-6)-1 x 10(-2) mol/L, 7.448 muA.L/mmol, 1.2 x 10(-6) mol/L and 5 s, respectively. A distinct advantage of this sensor is its good reproducibility of surface-renewal by simple mechanical polishing.

Renewable three-dimensional Prussian blue modified carbon ceramic electrode

Prussian blue (PB) supported on graphite powder was prepared by the chemical deposition technique and subsequently dispersed into methyltrimethoxysilane-derived gels to yield a conductive graphite organosilicate composite. The composite was used as the electrode material to fabricate a three-dimensional PB-modified electrode. PB acts as a catalyst, graphite powder ensures conductivity by percolation, the silicate provides a rigid porous backbone, and the methyl groups endow hydrophobicity and thus limit the wetting section of the modified electrode. The chemically modified electrode can electrocatalyze the oxidation of hydrazine, and exhibits a distinct advantage of polishing in the event of surface fouling, as well as simple preparation, good chemical and mechanical stability and good repeatability of surface-renewal. Hydrodynamic voltammetric experiments were performed to characterize the electrode as an amperometric sensor for the determination of hydrazine. (C) 2000 Elsevier Science B.V. All rights reserved.

Surface renewable graphite organosilicate composite electrode containing indium(III) hexacyanoferrate(II/III)

Indium(III) hexacyanoferrate(II/III) (InHCF) supported on graphite powder was prepared using the in situ chemical deposition procedure and subsequently dispersed into methyltrimethoxysilane-derived gels to yield a conductive graphite organosilicate composite. The composite was used as the electrode material to fabricate a three-dimensional InHCF-modified electrode. InHCF acts as a catalyst, graphite powder ensures conductivity by percolation, the silicate provides a rigid porous backbone and the methyl groups endow hydrophobicity and thus limit the wetting section of the modified electrode. The chemically modified electrode can electrocatalyze the oxidation of thiosulfate, and exhibits a good repeatability of surface-renewal by simple mechanical polishing, as well as simple preparation, good chemical and mechanical stability.