1,3-二羟基呫吨酮类化合物的简洁合成及清除亚硝酸根作用研究

以间苯三酚为起始原料,在伊顿试剂的催化作用下,与不同取代水杨酸反应合成1,3-二羟基呫吨酮类化合物3a~3l 12个,收率63%~87%,并探讨了反应机理及结构-反应活性关系.利用紫外分光光度法测定了所合成化合物对亚硝酸盐的清除作用,结果表明,在37℃、pH 3及反应时间为30 min条件下,1,3-呫吨酮类化合物对亚硝酸根均有较好的清除作用,其中化合物3f和3b的清除作用最强,清除率达34%.同时对1,3-二羟基呫吨酮类化合物清除亚硝酸盐的作用机制及构效关系进行了探讨.     

One-step synthesis of silica-coated magnetite nanoparticles by electrooxidation of iron in sodium silicate solution

In the present study, solid-solution gold?Cplatinum (Au?CPt) nanoparticles with controllable compositions were fabricated by high-intensity femtosecond laser irradiation of an aqueous solution of gold and platinum ions without any chemicals and complicated processes. Transmittance electron microscopy revealed that the single nanometer-sized particles were fabricated by femtosecond laser irradiation of mixed aqueous solutions of gold and platinum ions. The crystalline structure of nanoparticles was characterized by electron and X-ray diffractions. Contrary to the bulk Au?CPt binary systems, which commonly contain a pair of diffraction peaks between pure gold and platinum peaks because of its large miscibility gap in phase diagram, or mixture of Au and Pt, the diffraction peaks of Au?CPt nanoparticles fabricated in the experiment showed a characteristic of the fcc-type lattice. Moreover, the diffraction patterns shifted monotonically from the peak position of pure gold to that of pure platinum as the fractions of platinum ions in the solution were increased. These observations strongly imply that the Au?CPt nanoparticles were solid solution with intended compositions. This technique is not only simple and environmentally friendly, but also applicable to other binary and ternary systems.     

Temperature, H2 loading and ultra violet irradiation effects in germanosilicate optical fibers: laser spectroscopy measurements

The effects of heat-treatment and ultraviolet (UV) light at 325 nm on virgin and hydrogen loaded germanosilicate optical fibers have been investigated by using laser spectroscopy technique. The luminescence band around 650 nm is sensitive to heat treatment. The hydrogen reloading of the hydrogen loaded fibers subsequent to heat treatment showed a new emission band around 570 nm. The irradiated fibers have an emission band around 383 nm which was not detected in hydrogen loaded fibers.     

Suppression of particle generation in a plasma process using a sine-wave modulated rf plasma

Sine-wave modulated rf plasma has been used to control particle generation and growth in a plasma-enhanced chemical vapor deposition of silicon dioxide thin films using TEOS/O₂. The density and the size of particles generated in the plasma are greatly reduced when the plasma is modulated with sine-wave modulation at low modulation frequency (<1000 Hz). In addition, particle contamination on the films is significantly reduced also for nanoparticles, and the film growth rates at the range of modulation frequencies where particle generation are greatly reduced do not decrease appreciably. Compared to its counterpart pulse-wave modulation plasma, the sine-wave modulation plasma has demonstrated a better performance in terms of reduction of particle generation and film contamination, and of film growth rate. Thus, the sine-wave modulation plasma has shown as a promising method to be applied in the production of thin film with a high deposition rate and a low particle contamination.     

Photografted thin polymer hydrogel layers on PES ultrafiltration membranes: characterization, stability, and influence on separation performance

Highly fouling-resistant ultrafiltration (UF) membranes were synthesized by heterogeneous photograft copolymerization of two water-soluble monomers, poly(ethylene glycol) methacrylate (PEGMA) and N,N-dimethyl-N-(2-methacryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPE), with and without cross-linker monomer N,N'-methylene bisacrylamide (MBAA), onto a polyethersulfone (PES) UF membrane. The characteristics, the stability, and the UF separation performance of the resulting composite membranes were evaluated in detail. The membranes were characterized with respect to membrane chemistry (by ATR-IR spectroscopy and elemental analysis), surface wettability (by contact angle), surface charge (by zeta potential), surface morphology (by scanning electron microscopy), and pure water permeability and rejection of macromolecular test substances (including the "cutoff" value). The surface chemistry and wettability of the composite membranes did not change after incubating in sodium hypochlorite solution (typically used for cleaning UF membranes) for a period of 8 days. Changes in water permeability after static contact with solutions of a model protein (myoglobin) were used as a measure of fouling resistance, and the results suggest that PEGMA- and SPE-based composite membranes at a sufficient degree of graft modification showed much higher adsorptive fouling resistance than unmodified PES membranes of similar or larger nominal cutoff. This was confirmed in UF experiments with myoglobin solutions. Similar results, namely, a very much improved fouling resistance due to the grafted thin polymer hydrogel layer, were also obtained in the UF evaluation using humic acid as another strong foulant. In some cases, the addition of the cross-linker during modification could improve both permeate flux and solute rejection during UF. Overall, composite membranes prepared with an "old generation" nonfouling material, PEGMA, showed better performance than composite membranes prepared with a "new generation" one, the zwitterionic SPE.     

One-step Construction of Xanthone Scaffold Assisted by Microwave Irradiation to Optimize the Synthesis of DMXAA

An efficient and concise synthesis of 5,6-dimethylxanthenone-4-acetic acid(DMXAA) was developed. The overall yield of this 3-step procedure was 82%. The key reaction is the one-step construction of xanthone scaffold between 2,5-dibromo-3,4-dimethylbenzoic acid and 2-hydroxyphenyl-acetic acid assisted by microwave irradiation.     

Phase transformation behaviour in continuously cooled Zr65Al7.5Ni10Cu17.5− x Pd x (x = 0 − 17.5) glass-forming alloys and consequences for structure and property control

Continuous cooling transformation (CCT) diagrams were successfully constructed for Zr₆₅Al_7.5Ni₁₀Cu_{17.5? x} Pd _x (x?=?0???17.5) glass-forming alloys, comparing phase-transformation features in the alloy system to composition. While a low-Pd alloy (x?=?5) showed a single transformation curve, corresponding to the formation of a crystalline phase on the high-temperature side of the undercooled-liquid region, for a given time-scale, a high-Pd alloy (x?=?17.5) revealed an additional curve, corresponding to quasicrystalline phase formation on the lower temperature side. The result provides a clue to the structural and property control on the alloy system. Glassy specimens of the same size but with different intrinsic structure, evaluated by structural relaxation during continuous heating, could be fabricated for the low-Pd alloy (x?=?5). Plasticity was found to increase proportionally with the relaxation enthalpy. On the other hand, the critical size for glass formation could be improved considerably from 5 to 7 mm in diameter for the high-Pd alloy (x?=?17.5).     

Thermal conductivity of an alloy in relation to the observed cooling rate and glass-forming ability

The glass-forming ability (GFA) of an alloy in this case is the largest diameter of a rod which can be cast fully glassy. The present work shows that the thermal conductivity of a liquid alloy has a strong effect on GFA by influencing the cooling rate upon mould casting. The initial cooling rates (for the first 70–100?K of temperature decrease), obtained for Cu-, Zr- and Au-based bulk glass-forming alloys in the liquid state, are found to scale linearly with the thermal conductivities of the liquid base elements. However the low cooling rate found for Ni-based alloy suggests that the heat transfer at the melt–mould interface may also influence the cooling rate. The low thermal conductivity of Ni-based alloys and the correspondingly low cooling rate obtained compared to Cu-based counterparts explains their lower GFA. In the literature, many factors influencing the GFA of alloys have been discussed. To these factors, the present study adds the thermal conductivity of the molten alloy and the melt–mould heat-transfer coefficient. Moreover, the cooling rate depends on temperature and, thus, the critical cooling rate itself is not a suitable parameter for indicating GFA. The cooling can be better described by an appropriate fitting of the cooling curve to an exponential temperature decay function.     

由1,5-二羟基多羟基烃合成哌啶衍生物

以1,5-二羟基多羟基烃为原料,通过磺酰化转化为活泼的1,5-二磺酸酯,再与不同类型的伯胺化合物反应生成多羟基哌啶衍生物。 探讨了反应温度、反应时间和伯胺类型等条件对成环反应的影响,当反应温度为90~100 ℃、反应时间为18 h时,成环反应的收率达到了74%~94%。     

测定心血管紧张素转化酶抑制剂体外抑制动力学的反相HPLC法

报道一种用反相ＨＰＬＣ技术简便、有效地研究心血管紧张素转化酶抑制剂体外抑制动力学的新方法。该法利用马尿酰－甘氨酰－甘氨酸作酶底物，反相ＨＰＬＣ跟踪监测酶解产物马尿酸的浓度随时间变化来研究酶解反应的历程