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    10 September 2007, Volume 28 Issue 9
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    高等学校化学学报2007年第28卷第9期目次
    2007, 28(9):  0.  doi:
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    研究论文
    Preparation of SnO2/MCM-41 Semiconducter Sensors with MOCVD and Their Properties
    LIU Xiu-Li1, GAO Guo-Hua1*, KAWI Sibudjing2
    2007, 28(9):  1609-1612.  doi:
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    SnO2/MCM-41 semiconductor sensors were prepared by metallorganic chemical vapor deposition(MOCVD). The amount of deposition, specific surface area and pore distribution of SnO2/MCM-41 depend on the deposition time and temperatures. The fact that pore size are closely related with the amount of deposition indicates that SnO2 is coated smoothly in the pore of MCM-41. SnO2/MCM-41 sensor has high sensitivities for CO and H2. The sensitivities show a linear relation with the concentration of CO and H2.
    Effect of Anneal on the Properties of MgxZn1-xO Thin Films Deposited by Metal-organic Chemical Vapor Deposition
    DONG Xin1, ZHU Hui-Chao2, ZHANG Bao-Lin2, LI Xiang-Ping2, DU Guo-Tong1,2*
    2007, 28(9):  1613-1616.  doi:
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    High-quality MgxZn1-xO thin films were grown at 610 ℃ on c-sapphire substrates by metal-orga-nic chemical vapor deposition (MOCVD). To research the effect of anneal on the characteristics of MgxZn1-xO, MgxZn1-xO were annealed in vacuum and oxygen for 1 h, respectively. We can find the (002) peaks of the samples which were annealed in vacuum and oxygen are both enhanced, especially in oxygen measured by XRD. From the PL spectrum, the UV emission peak of the sample annealed in vacuum increase clearly and deep-level emission peak minish. The UV emission of the sample annealed in oxygen weakened and the deep-level emission peak enhanced remarkably due to the concentration of vacancy oxygen. It is shown that anneal can regulate the crystal, optical and electrical qualities of MgxZn1-xO film.
    Hydrothermal Synthesis and Characterization of Two Coordination Polymers of Flexible Acid and Lead: [Pb6(H2O)2(cit)4]·3H2O and Pb(tar)(H2O)2
    SHI Jing1, XU Jia-Ning1, ZHANG Ping1*, FAN Yong1, WANG Li1, BI Ming-Hui2, MA Kui-Rong1, SONG Tian-You2*
    2007, 28(9):  1617-1621.  doi:
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    Two coordination polymers [Pb6(H2O)2(cit)4]·3H2O(1)(H3cit=citric acid) and Pb(tar)(H2O)2(2)(tar=tartaric acid) were synthesized under hydrothermal conditions and characterized via IR, TG-DTA, C, H, N elemental analysis, XRD and single crystal X-ray diffraction analysis. There are three Pb, two cit ligand and two free water molecules in the asymmetry unit in complex 1. The Pb ions in complex 1 coordinate to cit anions with the coordination number of 4, 5, 7 to form a neutral 3D framework. Complex 1 crystallizes in the triclinic system, space group P1 with a=0.97053(19) nm, b=0.9764(2) nm, c=1.0955(2) nm, α=109.016(3)°, β=98.380(3)°, γ=92.136(3)°, V=0.9671(3) nm3, Z=2, R1=0.0420, wR2=0.01049, GOF=1.064. In the asymmetry unit of complex 2, there are a six-coordinated Pb, a tar ligand and a water molecule. Complex 2 has a structure of extended racemic ladder-like chain, these chains are assembled by complicated H-bonds to 3D supramolecular structure. It crystallizes in the orthorhombic system, space group Pbac with a=1.39739(6) nm, b=0.64922(2) nm, c=1.80354(10) nm, V=1.63620(13) nm3, Z=8, R1=0.0283, wR2=0.0649, GOF=1.014. In both complexes 1 and 2, the α hydroxyl and α carboxyl adopt a chelate mode, and the 6s lone pair of electrons of Pb has a stereochemistry activity resulting the distribution of the bonds in a hemisphere.
    Preparation of Vertically Aligned Carbon Nanotubes by Pyrolysis of Phthalocyanine at Lower Pressure
    SONG Hai-Yan1,2, LI Yan-Nan2, ZHAO Kun1, YE Xiao-Yan1, HE Pin-Gang1,2*, SUN Zhuo2*, FANG Yu-Zhi1
    2007, 28(9):  1622-1627.  doi:
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    Large scale vertically aligned carbon nanotubes(ACNTs) with a uniform length and diameter were prepared by the pyrolysis of iron(Ⅱ) phthalocyanine at a low pressure. The pyrolysis was performed in a dual furnace fitted with independent temperature controller. The morphology and microstructure of ACNTs were analyzed by SEM, FESEM and TEM. The ACNTs have a cylindrical and bamboo-like structure and are multi-walled carbon nanotubus. The influences of parameters such as gas pressure, growth temperature, gas flow rate and the volume ratio of Ar to H2 were studied. We found that ACNTs with best quality could been prepared at a pressure of 5×104 Pa and a higher temperature above 950 ℃. Some properties, such as field emission, capacitor, and sensor electrode of ACNTs were studied and discussed. The results showed a very powerful ability of electron emission with a lower turn-on voltage of 0.67 V·μm-1(I=1 μA) , a significant performance of power capacitor and electrical conductivity, which indicated that ACNTs are new highly efficient materials for practical devices application.
    研究快报
    Oxidative DNA Cleavage Catalyzed by Mn(Ⅲ) Corroles
    LIU Hai-Yang1,2*, LIU Lan-Ying1, ZHANG Lei3, YING Xiao4, WANG Xiang-Li1, JIANG Huan-Feng1, CHANG Chi-Kwong2*
    2007, 28(9):  1628-1630.  doi:
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    Several Mn(Ⅲ) 10-(hydroxylphenyl)-5,15-bis(pentafluoro-phenyl)corroles with the hydroxyl at ortho-, meta- and para-position of 10-phenyl group were used as the catalysts in the oxidative cleavage of plasmid DNA in the presence of H2O2. The catalytic system was composed of 10 μL 0.5 mg/mL pC DNA 6 in TE buffer solution(pH=8.0, 4.0×10-2 mol/L Tris, 1.0×10-3 mol/L EDTA), 10 μL 1.0×10-5 mol/L Mn(Ⅲ) corrole in DMSO and 10 μL 0.3% H2O2. After 8 h incubation at room temperature, significant oxidative DNA damage could be observed with the ortho-hydroxyl Mn(Ⅲ) corrole showing a better activity as detected by agarose-gel electrophoresis. Plasmid DNA was completely damaged after 12 h incubation. These observations show Mn(Ⅲ) corrole can be used as an artificial model of nuclease.
    研究简报
    Preparation and Luminescent Properties of BaZnP2O7∶Eu3+ Salmon Pink-emitting Phosphor
    YANG Zhi-Ping1*, YANG Guang-Wei1, WANG Shao-Li1, TIAN Jing2, LI Pan-Lai1, LI Xu1
    2007, 28(9):  1631-1633.  doi:
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    BaZnP2O7∶Eu3+ phosphor was synthesized by a high temperature solid state reaction. The compound shows four major emission peaks locating at 588, 613, 622 and 654 nm that correspond to the 5D0-7F1, 5D0-7F2 and 5D0-7F3 typical transition of Eu3+, respectively. The influence of the concentration of Eu3+ ions on the emission intensity was investigated and the concentration quench did not occured. The role of charge compensation of Li+, Na+ and Cl- ions to the emission intensity was also studied. It was found that Li+ ions gave the best improvement to enhance the intensity of the emissions. The results show that BaZnP2O7∶Eu3+ red-emitting phosphor is very suitable for white light emitting diode(w-LED) based on UV InGaN chip.
    High Temperature Synthesis of NaY Zeolite
    XIONG Xiao-Yun, LI Cai-Jin, DING Hong, HUANG Shi-Ying, LIANG De-Sheng, XIAO Feng-Shou, LI Shou-Gui*
    2007, 28(9):  1634-1636.  doi:
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    This work describes a novel method to synthesize NaY zeolite at high temperature(100—140 ℃) by using NaY seeds solution as a silica source, which is also a method for the activation of silica source in the synthesis of NaY zeolite. Conventionally, the synthesis temperature of NaY zeolite from water glass is about 100 ℃, and higher temperature(>100 ℃) leads to the formation of impurity. However, this work shows that high-temperature synthesis(100—140 ℃) still exhibits a pure phase NaY. It is very interesting that, compared with conventional temperature, high-temperature in the synthesis of NaY zeolite has obvious advantages such as short crystallization time and high n(Si)/n(Al) ratio in the product. More importantly, this method is possible to extend to the synthesis of NaA, NaX, Ω, ECR-1and MOR.
    Hydrothermal Synthesis and Crystal Structure of [In2(HPO3)4]·(NH3CH2CH2NH3)
    LIU Cheng-Zhan1,2, ZHU Guang-Shan1, FANG Qiang-Rong1, XUE Ming1, SUN Fu-Xing1, QIU Shi-Lun1*
    2007, 28(9):  1637-1639.  doi:
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    A new three-dimensional indium phosphite, [In2(HPO3)4]·(NH3CH2CH2NH3), was prepared under hydrothermal conditions via using ethylenediamine as a template. Its structure was solved by singlecrys-tal X-ray diffraction. The compound crystallizes in a monoclinic system, space group P2/n, with cell parameters a=0.91405(5) nm, b=0.91984(5) nm, c=0.96120(5) nm, β=115.9950(10)°, V=0.72640(7) nm3, Z=2, R1=0.0249, wR2=0.0650, GOF=1.044. The inorganic topological structure is built up from the vertex linking of InO6 octahedral and HPO3 pyramidal tetrahedral units, forming eight-membered ring channels along the [506] direction. The diprontonated ethylenediamine molecules are entrapped in eight-membered ring channels.
    研究论文
    Identification of Differentially Expressed Genes Using Disjoint Principal Component Analysis Coupled with Genetic Algorithm
    SU Zhen-Qiang1,3, HONG Hui-Xiao2, TONG Wei-Da3*, PERKINS Roger2, SHAO Xue-Guang4, CAI Wen-Sheng1,4*
    2007, 28(9):  1640-1644.  doi:
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    A new method for the feature selection using disjoint principal component analysis(PCA) coupled with genetic algorithm(GA) was proposed and was used to identify differentially expressed genes based on microarray gene expression profiles. The discriminatory power of combination of genes is assessed with using disjoint PCA, the combinatorial optimization problem of genes is solved by using GA, and the chance correlation of genes is assessed by a statistic method. Due to considering the cooperation between genes which is a way to approximate the synergistic regulation by genes during the biological processes, the genes identified by our method are capable of powerful ability to express the differences. This method has been applied to analyze the gene microarray data of hepatocellular caricinoma(HCC). It is found that the genes identified by the proposed method has more discriminatory power in distinguishing two-class samples than those identified by SAM(significance analysis of microarrays), which is very popular in the analysis of microarray data.
    In vitro and in vivo Activation of Mouse Liver Astral Cell by Confocal Raman Microspectroscopy

    GOAN Il-Ho1,2, SHEN Ai-Guo1,2, LIAO Zhang-Xiu3, WANG Hui3, HU Ji-Ming1,2*

    2007, 28(9):  1645-1650.  doi:
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    The feasibility of a novel and efficient diagnostic method for liver fibrosis via Raman spectroscopy was studied. Confocal Raman Spectroscopy(CRS) was utilized to monitor the molecular changes of rat hepatic stellate cells(HSCs) in vitro as well as in vivo activation. In vitro activation was induced by growth in uncoated plastic plates while the in vivo activation was induced by a single intraperitoneal injection of carbon tetrachloride(CCl4). Raman spectroscopy in combination with biological method perfectly established a correlation between spectral changes and morphologic changes within HSCs. The biochemical changes of HSCs during the activation such as the loss of retinoid, the increase of a-helical protein, and the increased production of extracellular matrix proteins were observed by CRS. Raman spectroscopy combined with fiber optical probe could be potentially accomplished in vivo detection, which can lead to a novel and efficient diagnosis for liver fibrosis.
    研究快报
    Color Surface Plasmon Resonance Imaging
    SHEN Gang-Yi1,2, HAN Zhi-Qiang1,2, LIU Wei1,2, CHEN Yi1*
    2007, 28(9):  1651-1653.  doi:
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    A method of color surface plasmon resonance imaging was developed and true color SPR images of solvents and BSA microdot arrays were recorded by using our laboratory-built device. The color signals, which were observed to be complementary to the resonance absorption of the incident light, depended on the feature of samples and the incident angle as expected. This new method looks to be a potential color analytical tool for high throughput detection of biochips.
    Rapid Preparation of Molecularly Imprinted Capillary Monolithic Columns by Microwave Polymerization
    ZHANG Yu-Ping1*, ZUO Guo-Qiang2, XU Guang-Ri1, LI Quan-Min2, YUAN Zhuo-Bin1,3
    2007, 28(9):  1654-1656.  doi:
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    Microwave irradiation was firstly attempted to prepare molecularly imprinted polymers (MIPs) monoliths, which were in situ prepared rapidly with methacrylic acid (MAA) as a functional monomer, ethylene glycol dimethacrylate (EDMA) as a cross-linking agent, toluene and isooctane as the porogenic solvents and AIBN as an initiator. The baseline separation of isomers of hydroxybenzoic acid was achieved on these monolithic columns with 4-HBA as the template, but not on the blank polymer. Furthermore, some neutral compounds could also be baseline-separated on the imprinted polymer columns in the modes of pressure-driven capillary electrochromatography and low-pressure driven capillary electrochromatography. It was shown that the monoliths were not only used as the molecularly imprinted polymers but also as the reverse phase chromatographic material.
    Cooperative Effects in the Fluorescent Labeling of Proteins Studied by High-performance Liquid Chromatography
    QIAO Xiao-Qiang, ZHANG Lin, LIANG Zhen, ZHANG Wei-Bing, ZHANG Li-Hua*, ZHANG Yu-Kui
    2007, 28(9):  1657-1659.  doi:
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    To improve the detection sensitivity of low abundance proteins in samples, fluorescence labeling might be a good solution method. In this manuscript, with 5-({2-[(iodoacetyl)amino]ethyl} amino) naphthalene-1-sulfonic acid (1,5-I-AEDANS) as the derivatizing reagent, the cooperative effects of insulin and BSA during the derivatization were studied. Through HPLC analysis, it was found that with BSA added, the detection sensitivity of the derivatized insulin could be improved. When the concentration ratio of BSA to insulin reached 200∶1, the peak area of insulin was increased by over 4-fold, which demonstrates that the existence of BSA had a positive effect on the derivatization of insulin. Furthermore, even when the ratio reached 1000∶1, the S/N of insulin was 8, which could not be detected without BSA being added. However, on the contrary, with insulin being added, the peak area of the derivatized BSA was decreased, demonstrating that insulin had a negative effect on that of BSA. All these results might be of great significance to the detection of low abundance proteins in proteome study.
    研究简报
    Electrochemical Behavior of CO2 on Copper Electrode
    ZHANG Li, LUO Yi-Wen, NIU Dong-Fang, XIAO Li-Ping, LU Jia-Xing*
    2007, 28(9):  1660-1662.  doi:
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    The electrochemical reduction of CO2 on copper electrode was investigated in acetonitrile(MeCN), dimethyl formamide(DMF) and dimethyl sulfoxide(DMSO) containing 0.1 mol/L tetraethylammonium bromioe(TEABr) by cyclic voltammetry and chronocoulometry at 298 K and under atmospheric pressure. There were obviously irreversible one-electron reduction peaks after saturated with CO2 on copper electrode in three solvents, which generated anion radical of CO2. The influence of scan rate was also studied by cyclic voltammetry. The diffusion coefficients of CO2 in MeCN, DMF and DMSO were 8.981×10-6, 1.019×10-6 and 1.032×10-6 cm2/s and the transfer coefficients were 0.064, 0.042 and 0.059, respectively. These results show that the electroreduction of CO2 was an irreversible diffusion controlled process.
    Simultaneous Determination of Sudan Ⅱ and Sudan Ⅲ via Synchronous Fluorescence Spectrometry
    CAI Qi-Hong1,2, ZOU Zhe-Xiang1, LI Yao-Qun1*
    2007, 28(9):  1663-1665.  doi:
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    A new method of constant-wavelength synchronous fluorescence spectrometry for simultaneous determination of Sudan Ⅱand Sudan Ⅲ was developed with using their fluorescence phenomenon. Only one single scan is needed for effective identification and quantitative determination of the two compounds simultaneously when Δλ=60 nm is chosen. The linear ranges for Sudan Ⅱ and Sudan Ⅲ were 0—3.3 and 0—2.8 μg/mL, respectively. The detection limits for Sudan Ⅱ and Sudan Ⅲ were 14 and 11 ng/mL, respectively. By using this method, Sudan Ⅱand Ⅲ in sausage samples were determined directly with the recoveries of 83.8%—109.5%.
    研究论文
    Synthesis and Herbicidal Activities of Novel 4,5,6-Trisubstituted Pyrimidine Sulfonylureas
    GUO Wan-Cheng, WANG Mei-Yi, LIU Xing-Hai, LI Yong-Hong, WANG Su-Hua, LI Zheng-Ming*
    2007, 28(9):  1666-1670.  doi:
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    In order to develop new herbicidal active compounds and study the structure-activity relationship, nineteen new sulfonylurea compounds were synthesized. Their structures were confirmed via 1H NMR, MS and elemental analysis. The preliminary herbicidal activity of these new sulfonylurea compounds was determined with rape disc assay and pot bioassay experiments. The results show that most of the sulfonylureas consisting of 4,5,6-trisubstituted pyrimidines displayed a herbicidal activity at 1.5 kg/ha.
    Synthesis and Biological Activities of 1,2,3-Thiadiazol-4-acetamide(Acetmorpholide) Derivatives
    DONG Wei-Li1, YAO Hong-Wei1, WANG Feng-Long2, LI Zheng-Ming1, SHEN Li-Li2, QIAN Yu-Mei2, ZHAO Wei-Guang1*
    2007, 28(9):  1671-1676.  doi:
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    In the investigation of new agrochemicals, we found 1,2,3-thiadiazole derivatives with good biological activities, had received only limited attention, but commercial pesticides containing 1,2,3-thiadiazole often possess a unique active mechanism, such as TDZ, BTH and tiadinil. We became interested in making 1,2,3-thiadiazoleacetamides, analogues of three commercial pesticides. In order to search for novel 1,2,3-thiadiazole derivatives with high activities, we designed and synthesized a series of novel 1,2,3-thiadiazole-4-acetamide(acetmorpholide)derivatives using diketene as the starting materials. Their structures were identified by means of elemental analysis, IR, 1H NMR and MS spectra. The results of the preliminary biological activity tests show that some of the compounds exhibit a better anti-TMV activity, plant growth regulator activity and fungicidal activity.
    Synthesis of Menthols via Selective Hydrogenation of Citronellal Catalyzed by Cu/ZrO2-SiO2 in Ionic Liquid
    NIAN Bao-Yi1*, XU Gang2, WU Jian-Ping2, YANG Li-Rong2
    2007, 28(9):  1677-1680.  doi:
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    The simple and efficient catalyst of Cu/ZrO2-SiO2 was prepared and chemoselective hydrogenation of citronellal was performed over this catalyst in room temperature [bmim][Al2Cl7] ionic liquids as the clean solvent and assisted-catalysts. The isomerization of citronellal under very mild hydrogenation conditions can be favor toward isopulegols that was hydrogenated to further menthols in Lewis acid ionic liquids. Citronellal can be converted, 100% of conversion and 91.3% of selectivity based on menthols were obtained in one-pot process by competitive hydrogenation. The products distribution was found to depend strongly on hydrogen bond formed between carbonyl group of citronellal molecule and cation of ionic liquids. This reaction process was discussed especially and its evolution was also suggested to use in the future. The catalysts and ionic liquids can readily be recovered and reused.
    Synthesis of Novel Spiro-dendrimer
    LIANG Ya, GUO Jin-Jing, WEI Rong-Bao*
    2007, 28(9):  1681-1684.  doi:
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    A novel dendrimer-9H, 9H, 11H, 11H, 12H, 12H-hexahydrobenzo[9,10]-1H, 1H, 3H, 3H, 4H, 4H, 5H, 5H, 7H, 7H, 8H, 8H-dodecahydrophenanthrene-2,6,10-trione ketal-tri-(4-(4-(3-(9-(4-(2,6-disulfo-cyclohexyl)phenyl))-2,4,8,10-tetra-oxa-spiro[5.5]undecyl))phenyl-1,1-(2,6-dioxa)cyclohexanedimethanol was conveniently synthesized by the reaction of hexahydrobenzo[9,10] dodecahydrophenanthrene-2,6,10-trione ketal-tri-2,2-dihydromethyl-1,3-propanediol with 4-(4-(3-(9-(4-(2,6-disulfo-cyclohexyl)phenyl))-2,4,8,10-tetra-oxa-spiro[5.5]undecyl))phenyl-1,1-(2,6-dioxa)cyclohexanedimethanol. Some reaction intermediates were prepared with common chemical reagent . Novel dendrimer and intermediates were identified via IR, 1H NMR and MS spectra and elemental analysis.
    Cloning of Flocculent Gene and Morphology Characterization of Flocculent
    CHANG Yu-Guang, MA Fang*, GUO Jing-Bo, ZHANG Jin-Feng
    2007, 28(9):  1685-1689.  doi:
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    One strain, named as Bacillus sp. F2, with the flocculent ability as high as 84%, was separated. Flocculent genomic library was constructed and a Bacillus coli. Positive clone FC2, which could express flocculent activity, was acquired after selection. The flocculent tests showed that the flocculent efficiency of FC2 was 90%, which was slightly higher than the original flocculent bacterium F2 and greatly higher than the competent cell JM109(6.9%), which demonstrated that FC2's flocculent characteristics inherited from the original flocculent bacterium F2. By adopting the tapping mode AFM, light microscope technique and ζ potential test, the flocculent microtopography of FC2, F2 and pure Kaolin suspending solution was identified. The AFM study revealed that, compared to the Kaolin suspending solution with and without F2's fermented liquid, the kaolin suspending solution to which fermented liquid with cloning bacterium FC2 was added had larger flocculent gel and more compact spherical structure, and the surface was rough with high degree concave and convex, had large specific surface area and strong adsorption ability to the suspending particles in the solution. After delivering the fermented solution of cloning bacterium FC2 into kaolin suspending solution, the amorphous and incompact flocculent particles transformed into spherical structure which was compact and had even horizontal dimension, this indicates that the agglutinin in FC2's fermented liquid could easily take Kaolin suspending particles as its adsorption core and adsorbed on its surface and the flocculent efficiency was about 90%, which gave further confirmation to the favorable pollution removal capability of FC2's fermented liquid. The results of ζ-potential test illustrates that the intensity of electrovalent bond was different, resulting in various flocculent morphology, which provided significant evidences for studying flocculent mechanisms of biofloculant.
    Bioeffects of Silica Nanoparticles and Silica Microparticles as Carriers for Enzyme Immobilization
    SHI Hui1,2,4, HE Xiao-Xiao1,2,3,4, WANG Ke-Min1,2,4*, YUAN Yin1,2,4, TAN Wei-Hong1,2,4
    2007, 28(9):  1690-1695.  doi:
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    In this paper, the differences between silica nanoparticles(SiNPs)and silica microparticles(SiMPs)in the bioeffects of them as carriers for enzyme immobilization were investigated. By choosing bovine liver catalases and horseradish peroxidases as the multimeric enzyme model and monoer enzyme model, respectively, four kinds of immobilized enzymes were obtained through the covalently binding method. After the characterization of above four immobilized enzymes, the following conclusion was stated. Firstly, in the yields of enzyme activity, SiNPs exhibit non-selective excellent biocompatibility to both enzyme models; secondly, SiMPs are superior to SiNPs on thermostability; thirdly, both SiNPs and SiMPs could greatly improve the stability of enzymes in organic solvents; lastly, there is no obvious rule indicated on the optimum temperature of enzyme catalysis, namely, SiNPs are better than SiMPs in the multimeric enzyme model and SiMPs possess much more advantages over SiNPs in the monomer enzyme model. The results would be instructional to the evaluation of nanomaterials' bioeffcts and the application of nanomaterials for enzyme immobilization.
    Spleen Lymphocyte Proteome Analysis in Bronchial Asthma of Wistar Rats
    LI Shan-Yu1,2, FAN Jia1, XI Jing-Hui1,3, ZHANG Hai-Yu2, DU Hong-Wei2, ZHOU Xin1, WANG Xu1, NING Bo1, LIU Lan-Ying4, HAO Dong-Yun1*
    2007, 28(9):  1696-1700.  doi:
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    To study the molecular mechanisms of asthma, the bronchial asthma model was established with OVA-sensitized Wistar rats. The differentially expressed spleen lymphocyte proteomes between asthmatic rats and normal rats were profiled and the proteins were identified via two-dimensional electrophoresis and MALDI-TOF-MS. The results reveal that the expression of some protein genes was up-regulated in asthmatic rats in comparison with the normal rats. These includes hnRNPK, involving the transcriptional regulation of collagen proteins, and cell structural protein Fibrinogen. However, the energetic metabolism-relating protein such as CoQ10 and mitochondrial inner membrane protein were exhibited to be down-regulated. Further analysis using bioinformatic tools suggests that the above-mentioned proteins are likely important components involving the airway chronic inflammation, airway hyper-responsiveness and airway remodeling of asthmatic rats.
    Expression, Purification and Crystal Growing Conditions of Recombinant Oryza sativa PHGPx
    WANG Feng, LIU Jin-Yuan*
    2007, 28(9):  1701-1706.  doi:
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    Phospholipid hydroperoxide glutathione peroxidase(PHGPx) is a unique antioxidant enzyme that directly reduces lipid hydroperoxides in biomembranes. It plays potential important roles in oxidative stress response. Oryza sativa PHGPx gene was cloned into expression vector pGEX-6P-1 and transformed into E.coli strain BL21(DE3). OsPHGPx for crystals was prepared with employing Glutathione SepharoseTM affinity, cation-exchange and gel filtration chromatography. The purity of the purified OsPHGPx was over 95%. OsPHGPx showed an obvious PHGPx activity towards lipid hydroperoxides. MALDI-TOF analysis shows that the exact molecular weight of OsPHGPx was 19275.568, which was in accordance with the theoretical molecular weight. The microcrystals of OsPHGPx were obtained under several conditions. In addition, a tertiary structure model of the OsPHGPx generated from http://swissmodel.expasv.org/ displayed the thioredoxin fold.
    研究简报
    Synthesis and Antifungal Activity of Novel Triazole Derivatives
    SUN Qing-Yan*, CAO Yong-Bing, XU Jian-Ming, ZHANG Wan-Nian, ZHANG Jun, WU Qiu-Ye, ZHANG Da-Zhi, JIANG Yuan-Ying
    2007, 28(9):  1707-1709.  doi:
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    A series of 1-(1H-1,2,4-triazol-1-yl)-2-(2,4-difluorophenyl)-3-[(4-substitutedphenyl)-piperazin-1-yl]-propan-2-ols were designed and synthesized on the basis of the active site of fungal Lanosterol 14α-demethylase(CYP51), the structure-activity relationships and antimycotic mechanism of azole antifungal agents. Their structures were confirmed via elemental analysis, IR, MS and 1H NMR. The results of preliminary antifungal tests against eight human pathogenic fungi(Candida albicans, Candida parapsilosis, Candida tropicalis, Cryptococcus neoformans, Aspergillus fumigatus, Trichophyton rubrum, Fonsecaea compacta, Microsporum gypseum) in vitro show that all compounds exhibited higher activities against fungi than that of fluconazole, voriconazole and amphotericin B; compounds 4a, 4b and 4d showed higher activities against Aspergillus fumigatus than fluconazole and voriconazole(with the MIC values of 0.25, 0.25 and 0.25 μg/mL respectively). For antifungal activity of these novel triazole derivatives, it is very helpful to introduce the 4-(4-substitutedphenyl) piperazine as side chains to interact with the residues of the narrow hydrophobic cleft of CYP51 and adjust the physico-chemical properties of title molecules.
    研究论文
    Preparation and Photocatalytic Properties of Activated Carbon Supported TiO2 Nanoparticles with Cu Ions Doping
    LI You-Ji*, SONG Zhi-Juan, LI Zhi-Ping, OUYANG Yu-Zhu, YAN Wen-Bin
    2007, 28(9):  1710-1715.  doi:
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    Composite photocatalysts(Cu2+-TiO2/AC) were prepared via a sol-gel method by means of activated carbon(AC) supported TiO2 nanoparticles with copper ions doping. The photocatalysts were characterized by XRD, ESR, FS, UV-Vis and BET analysis. The effects of specific surface area of AC and amount of Cu ions doping on the photoactivity of the as-prepared samples were analyzed by photodegradation of Rhodamine B(RB). The results show that Cu ions exist in a form of the Cu2+ ions and there are a few of Ti3+ ions state in titanium dioxide. The TiO2 nanoparticles show the quantum size efficiency, the notablely blue shifting of absorption threshold and the optic response range expanding to visual light. Additionally, the FS intensity of TiO2/AC decreases via proper amount of Cu ions doping. The microcosmic structure of AC is changed by coating and heat treatment at a high temperature. Photocatalysts(3%Cu2+-TiO2/AC3) show the highest photoactivity by using AC3 as the carrier with 3% Cu2+ ions doping, meanwhile, they can be easily recovered from the reaction solution and reused with a high photoactivity.
    Synthesis of Nonasil(HMI) Induced by Crystal Seeds
    XING Hai-Jun, WU Shu-Jie, JIA Ming-Jun, WU Tong-Hao, KAN Qiu-Bin*
    2007, 28(9):  1716-1719.  doi:
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    By using different zeolites(Nonasil, MCM-22 or MCM-49) as the crystal seeds, the synthesis of Nonasil(HMI) porosil was studied under hydrothermal conditions in the presence of hexamethyleneimine(HMI) as the organic template. Various synthesis parameters, including the type of crystal seeds, silica source, temperatures and the concentrations of Na+, are investigated for the synthesis of nonasil(HMI). It was found that the addition of crystal seeds could considerably shorten the time of crystallization in the presence of appropriate amount of Na+ and that different kinds of crystal seeds could accelerate the crystal growth with different degrees. Particularlly, nonasil(HMI) with a high crystallinity level can be obtained with heterogeneous crystal seeds(i.e. MCM-22, MCM-49).
    Rheological Properties of Colloidal Liquid Aphrons
    YAN Yong-Li1*, QU Cheng-Tun1, ZHANG Ning-Sheng2, CHEN Jie-Rong3
    2007, 28(9):  1720-1725.  doi:
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    Colloidal liquid aphrons(CLA) composed of polyoxyethylene 3 dodecyl ether(AEO-3)/n-decane/ sodium dodecyl sulphate(SDS)/water were subjected to a full rheological characterization. Steady-state flow and dynamic viscoelasticity were measured via a Haake RV-30 viscosimeter and a controlled stress rheometer Haake RS 300 with cone-plate geometry, respectively. The effects of the volume ratio of dispersed oil phase to the continuous phase(PVR), temperature and shear rate on the rheological behavior of CLA were also discussed. The results of the steady-state analysis indicate that both CLA and emulsions studied here were typical non-Newtonian liquids and exhibited strong shear thinning behavior. The flow curves of CLA were well described by the Hershel-Bulkley equation. Thixotropy was not observed in any of CLA and emulsions. The findings from the oscillatory viscoelastic analysis suggest that no linear viscoelasticity region existed in the entire range of stresses for low PVR(2—4), and at the PVR of 8, the systems display a viscoelastic behavior. The effect of temperature on the flow behavior and viscoelasticity of CLA and emulsions was not evident. The rheological properties of CLA are analogous to that of high internal phase ratio emulsions(HIPRE) through a comparison of the findings throughout this work and conclusions of HIPRE reported previously. This similarity further suggests that CLA and HIPRE display a similar microstructure.
    Structure and Acid Properties of Phosphate-modified MCM-49 Zeolites and Their Catalysis Performance for the Alkylation of Benzene with Propylene in Liquid
    ZHANG Yu1, WANG Li-Xia2, WU Shu-Jie2, YANG Xu-Wei2, JIA Ming-Jun2*, WU Tong-Hao2, SUN Chia-Chung3
    2007, 28(9):  1726-1730.  doi:
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    MCM-49 zeolite was synthesized hydrothermally in a 10 L autoclave by dynamic method. The phosphate-modified MCM-49 zeolites were prepared by impregnation. The resulting solids were characterized by different techniques, such as XRD, N2 adsorption-desorption, NH3-TPD, FTIR and 27Al NMR. Benzene alkylation with propylene was carried out by using MCM-49 and phosphate-loaded MCM-49 zeolite as the catalysts. Both the amounts of Bronsted and Lewis acid on phosphate-modified MCM-49 were decreased. 27Al NMR spectrum reveals that the loading of phosphate onto MCM-49 results in a increase of the amounts of extraframework aluminum, and two new signals corresponding to Al(OP)6 and Al(PO)4 can be found, respectively. Loading of phosphate onto MCM-49 greatly enhances the selectivity to IPB in benzene alkylation with propylene. The phosphate-modified MCM-49 catalyst containing 2.0%(mass fraction) phosphorus, at a reaction temperature of 140 ℃, exhibits 81.1% selectivity to IPB and 97.2% selectivity to all alkyaltion products(including IPB, DIPBs and TIPB) with a similar conversion of propylene in comparision with MCM-49.
    Theoretical Studies on Electronic Structures and Third-order Nonlinear Optical Properties of Di-metallocene Complexes Zn2(η5-E5)2(E=N, P, As, Sb)
    ZHAO Shu-Kui1, SUN Xiu-Yun1*, FANG Liang2, ZHU Yu-Lan3*
    2007, 28(9):  1731-1734.  doi:
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    Electronic structures of di-metallocene complexes Zn2(η5-E5)2(E=N, P, As, Sb) were investigated with DFT PBE0 method. Charge distribution and bonding characters are analyzed with Natural Bond Orbital(NBO) Theory. The results show that a single σ-bond of Zn—Zn exists in these complexes with a nearly pure s character. The nonlinear third-order polarizabilities(γ) were calculated for the four di-metallocene complexes by time-dependent density functional theory(TD-DFT ) combined with sum-over-states(SOS) method. The calculated results show that γ value is in direct proportion to the maximum absorption wavelength(λmax). Analysis of the main contributions to the third-order polarizability suggests that electron transfer(Zn—Zn σ-bond →Zn—Zn σ*-bond ) along z-axis direction plays a key role in the nonlinear optical response.
    Adsorbent Structure Design and Adsorption Mechanism by Computer Simulation
    WEI Zhong, HUANG Wei, LI Ji-Hong, YUAN Zhi*
    2007, 28(9):  1735-1738.  doi:
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    Endotoxins are lipopolysaccharides(LPSs) of the outer cell wall of Gram-negative bacteria and show strong biological effects on human beings when entering the blood stream. Serious endotoxin intoxication can cause endotoxermia, so the removal of endotoxin duly and effectually is very important. In this paper, three adsorbents with dimethylamine ligands β-OH, γ-OH and β-SH were synthesized based on the agarose matrix to remove endotoxin from aqueous solution. The static and dynamic adsorption results show that the structure of ligand influenced greatly on the endotoxin adsorption and the β-OH adsorbent had the highest endotoxin removal percentage(ERP), 90.7%. Computer simulation method was employed to investigate the interaction between endotoxin and ligand. It was found that electrostatic force and cooperative hydrogen bond contributed much to the adsorption of endotoxin. A β-OH adsorbent interaction model was developed.
    Preparation and Properties of Conducting Polymer Poly(3,4-ethylenedioxythiophene) Nanoparticles
    YANG Ya-Jie, JIANG Ya-Dong*, XU Jian-Hua, YING Zhi-Hua
    2007, 28(9):  1739-1742.  doi:
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    Poly(3,4-ethylene dioxythiophene)(PEDOT) nanoparticles was prepared by reverse micelles technique. The nanoparticles were characterized by UV-Vis-near IR(UV-Vis-NIR) adsorption spectrum, IR spectrum, X-ray photoelectron(XPS), scanning electron microscopy(SEM) and transmission electron microscopy(TEM). The results confirmed that size distribution of this particle was 30—40 nm and the nanoparticles has been doped by Cl- during synthesis process. The conductivity of nanoparticles was investigated by four-probe and it has been found that this nanopartices showed higher conductivity(10.2 S/cm)than conventional one. Furthermore, the gas sensitivity of nanoparticles deposited on quartz crystal microbalance(QCM) was studied and the nanopartices deposited device exhibited excellent sensitivity to NH3 gas at low concentration. The mechanism of conductivity and gas sensitivity of the nanoparticles are also included in this paper.
    Quantum Study on Abstracting Hydrogen Mechanism in Hydroxyl Radical Scavenging of Trans-resveratrol
    SHEN Yong-Li1, HAO Jin-Ku1,2*, CAO Ying-Yu2, YANG En-Cui2
    2007, 28(9):  1743-1746.  doi:
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    All possible conformations of trans-resveratrol were optimized by using DFT B3LYP/6-31g, and natural bond analysis on the most stable conformation was carried out, the result shows that the most active position in the hydroxyl radical scavenging of trans-resveratrol was the phenolic hydroxyl in the single hydroxyl circle. The mechanism of this reaction has been theoretically studied at DFT B3LYP/6-31g. The IRC also has been carried out at the same theoretical level. The results show that the hydroxyl of trans-resveratrol reacted with hydroxyl radical to produce H2O. The energy of stationary points in the reaction path shows that the energy of reactant was E1=173.5193 kJ/mol, higher than that of the reactant complex, the activation energy was Ea=16.5143 kJ/mol, and the energy of product was E2=51.8799 kJ/mol, higher than that of the reactant complex. So when the reaction complex formed it would be trasformed into transition state and product immediately.
    In-Cell Indirect Electrooxidation of 2-Picoline
    LI Ke-Chang, CAO Xue-Jing, ZHANG Heng-Bin*, ZHANG Yu-Min
    2007, 28(9):  1747-1750.  doi:
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    In the electrolytic cell with proton exchange membrane as a diaphragm, the reaction conditions for preparing 2-pyridinecarboxylic acid from 2-picoline via indirect electrooxidation with Cr2O72-/Cr3+ as a mediator were studied, the results show that concentrations of H2SO4, Cr2(SO4)3 and 2-picoline, reaction temperature and anode potential have an important influence on yield, conversion, selectivity and current efficiency. The optimal conditions ara as follows: H2SO4 concentration 6.0 mol/L, reaction temperature 60 ℃, Cr2(SO4)3 concentration 0.15 mol/L, 2-Picoline concentration 0.1 mol/L, anode potential 1.50 V.
    Improved Tight-binding Monte Carlo Method and Its Application in Carbon Nanopeapod
    LIN Yi1, CAI Wen-Sheng1,2*, SHAO Xue-Guang2
    2007, 28(9):  1751-1755.  doi:
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    An improved tight-binding Monte Carlo method is proposed, by which the CPU time can be greatly decreased through reducing the number of atoms in calculating the tight-binding energy. The simulation of the parallel nanotube junction indicates that the improved method is much more efficient than the previous one. This method is successfully applied in study of the large carbon nanopeapod. The calculation results show that, the fullerene coalescence occurs inside the single-walled carbon nanotube at about 2000 K with the formation of vacancies on the close sides of fullerenes, or the fullerene coalescence is only observed at a high temperature of about 4500 K. The orientation of fullerenes does not influence the coalescence.
    研究简报
    Preparation of Ag Nanoparticles by Ultrasound-assisted Membrane Reaction
    WANG Zhen-Yang, GUAN Xiao, HE Hong*, DAI Hong-Xing, ZI Xue-Hong
    2007, 28(9):  1756-1758.  doi:
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    Ag nanoparitcles were prepared via Ultrasound-assisted Membrane Reaction(UAMR) method. The key issue of the method is to control precisely the injection speed of the reactants by pulseless pump to make the nanoparticles of Ag with small size and narrow size distribution. The size and morphology of silver nanoparticles were characterized with Transmission Electron Microscope(TEM) and UV-Vis spectrum. The experiment results show that the size of Ag nanoparticles prepared via UAMR method was smaller than that via Ultrasound-assisted Dropping Reaction(UADR) method. The size of 80% Ag nanoparticles prepared via UAMR was ranged from 3 nm to 5 nm with the mean particle size 4.7 nm and considerable narrow size distribution. The Ag hydrosol fabricated via UAMR method was very stable at room temperature, even within three months.
    Preparation of SiO2 Ordered Macroporous Material by Floating Assembly Method
    WANG Xiao-Dong*, YI Gui-Yun
    2007, 28(9):  1759-1761.  doi:
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    Floating assembly method is a new way for preparing ordered macroporous materials. In this process, the co-mixture of binary colloidal particles was fabricated through the rapid assembly of polystyrene(PS) as a template and SiO2 nanoparticles at the air-water interface of the suspension, the ordered macroporous materials were obtained by removing the template. Scanning Electron Micrographs(SEM) show that macroporous material had regular close-packed face-centered cubic(fcc) structure and spaces left by templates were connected through some windows. The results indicate that the formation of ordered porous structure was influenced by the diameter of PS microspheres remarkably. When the diameter was in the range of 200—500 nm the ordered structure could be obtained easily. And the volume ratio of PS microspheres to SiO2 nanoparticles in the maxed suspension wasn't primary factor of the the formation of the ordered structure.
    Mechanism of Chromium Poisoning of LSM Cathode in Solid Oxide Fuel Cell
    FU Chang-Jing1, SUN Ke-Ning2*, ZHANG Nai-Qing1, ZHOU De-Rui1
    2007, 28(9):  1762-1764.  doi:
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    Although metallic interconnects have many advantages, the formation of Cr2O3 scale and the evaporation of Cr(Ⅵ) species from alloys will greatly degrade the solid oxide fuel cell(SOFC) performance. In this paper, the electrochemical impedance spectroscopy(EIS) and the cathode polarization method of galvanostatic current interruption were employed to investigate the deposition mechanism of chromium with the electrochemical behavior of LSM cathode in the presence of chromia-forming alloys. The results show that the dissociative adsorption and the diffusion of oxygen on the LSM surface were inhibited by the gaseous chromium species and the migration processes of oxygen ions into YSZ electrolyte were inhibited by the solid chromium species deposited on the YSZ surface.
    Electrochemical Behavior of Aqueous Electrochemical Reactions in Super Gravity Field
    XING Hai-Qing1,2, GUO Zhan-Cheng1,3*, WANG Zhi1, WANG Ming-Yong1
    2007, 28(9):  1765-1767.  doi:
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    The electrochemical behavior of Fe3+/Fe2+system and ferricyanide ion were investigated by cyclic voltammetry, linear sweep voltammetry, and chronoamperometry in the super gravity field. The results show that diffusion coefficient of ferricyanide ion increased in the super gravity field, and diffusion coefficient under gravity coefficient 125 is almost two times of that in the natural gravity field. The peaks of oxidation and the reduction of Fe3+/Fe2+ disappeared gradually with the increase of the gravity coefficients, and the limiting current densities appeared at 0.10 and 0.80 V(vs. SCE), with increasing super gravity coefficients. When G=30, the limiting current density is 0.100 A/cm2 at 0.10 V, while it is up to 0.196 A/cm2 under G=280.
    Electrocatalytic Activity of a Novel Nanoporous Platinum Electrode Towards Methanol Oxidation
    YI Qing-Feng1*, CHEN Ai-Cheng2, ZHANG Jing-Jing1, HUANG Wu1
    2007, 28(9):  1768-1770.  doi:
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    A novel titanium-supported nanoporous platinum (nanoPt/Ti) with a network structure was fabricated by using the hydrothermal process. Electrochemical oxidation of methanol on nanoPt/Ti was investigated in alkaline solutions for the first time. It was shown from the voltammograms that the peak current density of methanol oxidation on the nanoPt/Ti electrode increases significantly compared to the polycrystalline Pt. As shown in anodic polarization curves at 1 mV/s, the peak current density on the nanoPt/Ti is over 45 times higher than that on the polycrystalline Pt. Moreover, chronoamperometric measurements at different potentials locating round the peak potential of methanol oxidation exhibit highly stable current densities under the applied experimental conditions.
    研究论文
    Evolutions of Structure and Tropism of Fibers During Preparation of Polymer-derived High-temperature Resistant Continuous SiC Fibers
    ZHENG Chun-Man, LI Xiao-Dong*, WANG Hao, ZHAO Da-Fang, HU Tian-Jiao
    2007, 28(9):  1771-1775.  doi:
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    High-temperature resistant continuous SiC fibers were prepared by polymer-derived method using precursor polyaluminocarbosilane(PACS). The evolutions of the fibers structure and tropism during the preparation and its effect on the properties of the fibers were investigated. The results show that the evolutions of structure of continuous cured PACS fibers included four stages: crosslinking among the molecules of the fibers(≤600 ℃), basically inorganic transformation(600—800 ℃), completely inorganic transformation(800—1300 ℃), crystallization and redistribution of the structure(1300—1800 ℃). The tropism of the fibers changed with the evolutions of the structure. Continuous PACS fibers had the weak tropism along the fiber axis and it was evolved to the products prepared at 1300 ℃. The fibers transformed from anisotropic to isotropic state at 1500 ℃. The properties of continuous SiC fibers were affected greatly by the evolutions of the structure and tropism.
    Preparation of Sustained-release Gelatin Microspheres as the Cell Microcarrier
    WANG Yi-Juan1, LIU Shou-Xin1*, FANG Yu1, HUANG Sha2, JIN Yan2, JIANG Yu1
    2007, 28(9):  1776-1780.  doi:
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    The BSA-impregnated large diameter gelatin microspheres were prepared with the improved and emulsified cold-condensation method. The results indicate that the gelatin solution 25%(mass fraction), volume ratio(3∶20) of water phase to oil phase, stirring rate 300 r/min, glutaraldehyde 0.1 mL(25%, mass fraction), and surfactant span-80 0.1 g were an optimal condition to prepare the gelatin microsphere. The average diameter of microspheres was 250 μm. By using three different ways to process the microspheres the gelatin microspheres with the different surface structures and cell adsorption ratio could be obtained. The blank microspheres can biodegrade absolutely in vitro. The BSA release from the BSA-impregnated gelatin microsphere can be sustained for 30 d. Fibroblasts grew well on the surface of gelatin microcarrier.
    Synthesis of Polymer Electrolyte Based on P(VAc-MA)/PMMA and Its Application in Electrochromic Devices
    YANG Dao-Jun1,2, FU Xiang-Kai1,2,3*, JIANG Qing-Long1,2, GONG Yong-Feng1,2
    2007, 28(9):  1781-1786.  doi:
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    A random copolymer P(VAc-MA) was synthesized via seeded emulsion copolymerization with vinyl acetate(VAc) and methyl acrylate(MA) as the monomers, and the polymer electrolytes comprising blend of the corresponding copolymer P(VAc-MA) and PMMA as a host polymer and LiClO4 as a dopant were prepared with solution casting technique. The performances of the synthesized copolymer and prepared polymer membrane and electrolyte were studied with FTIR, XRD, TG, UV, mechanical testing and AC impedance. It was found that copolymer P(VAc-MA) was formed with breaking the double bonds of monomers. After blending P(VAc-MA) and PMMA, the energy barrier of the segmental motion in the polymer electrolyte was reduced because of the amorphous nature increased; the thermal stability and mechanical performance increased. The polymer electrolytes based on blends P(VAc-MA)/PMMA possess an excellent transparence and the maximum ionic conductivity value was found to reach 1.17×10-3 S/cm at 25 ℃; the ionic conductivity increases as temperature rising, the conductivity temperature plots are found to follow basically the Arrhenius equation. The polymer electrolytes were further evaluated in electrochromic devices(ECD) fabricated by transparent PET-ITO and electrochromic active viologen derivative films, and its excellent performance promised the usage of the polymer electrolytes as the ionic conductor material in ECD.
    Preparation and Properties of Superabsorbent by Graft Co-polymrization of Acrylic Acid onto Different Celluloses of Crops Stems
    WANG Cun-Guo1*, HE Li-Xia1, DONG Xian-Guo1, GAO Xiao-Ping1, LIU Wei1, DONG Xiao-Chen1,2, YUAN Tao1, ZHANG Jun1
    2007, 28(9):  1787-1790.  doi:
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    The different celluloses of crops stalks such as corn, cotton and wheat stem were studied by graft copolymerization with acrylic acid. Many factors, such as ratios of starch to cellulose, de-ionized water, running water and rain water, which affected the absorbency of copolymers, were researched. The copolymer prepared from cotton stem cellulose and acrylic acid can absorb de-ionized water 930 g/g, running water 670 g/g, and rain water 380 g/g. The copolymer of corn crop cellulose and sweet potato starch(3∶2, mass ratio) with acrylic acid can absorb rain water 540 g/g.
    Synthesis of Thiol-Terminated Poly(ε-caprolactone)
    XU Ning, WANG Rui, DU Fu-Sheng, LI Zi-Chen*
    2007, 28(9):  1791-1795.  doi:
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    Thiol-terminated poly(ε-caprolactone)(PCL) was synthesized with 2-mercapto ethanol and through two mild, simple and efficient methods: one is the ring-opening polymerization of ε-caprolactone with 2-mercaptoethanol as initiator and stannous (Ⅱ) trifluoromethane sulfonate as catalyst; the other is the ring-opening polymerization of ε-caprolactone with 2-hydroxyethyl disulfide as initiator, followed by reduction reaction. In the first method, when the polymerization temperature was increased, the molecular weight distribution of the final product was broad, while the structure remained unchanged; this thio-end capped PCL can be coupled to form a new polymer with a disulfide group in the center. The structures of these polyesters were confirmed by 1H NMR spectra and gel permeation chromatography. The polymers show controlled molecular weights and narrow molecular weight distributions. These methods may also be used to prepare other polyesters with thiol-end groups.
    Novel Hyperbranched PEU Polymer Electrolytes for Lithium-ion Batteries
    BAI Ying1,2, PAN Chun-Hua1, WU Feng1,2, WU Chuan1,2*, YE Lin3, FENG Zeng-Guo3
    2007, 28(9):  1796-1800.  doi:
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    A novel type of hyperbranched PEU(PHEU) was prepared from the reaction of the hyperbranched polyether(PHEMO) with hexaethylene diisocyanate(HDI) in electrolytes containing lithium salts. The thermal stabilities and ionic conductivities of the as-prepared electrolytes were investigated by Fourier transform infrared spectroscopy(FTIR), differential scanning calorimetry(DSC), thermogravimetric analysis(TGA) and alternating current(AC) impedance. When the concentration of the electrolyte is 3 mol/L, and the mass of the electrolyte is three folds as high as that of the polymer matrix, the polymer electrolyte can achieve an ionic conductivity of 6.12×10-4 S/cm at room temperature. Cyclic voltammogram indicates that the electrochemical stability window is from 2.2 to 4.0 V. In addition, the small molecules of electrolyte were perfectly enclosed by the polymer chains, which can avoid liquid leaking. Therefore, it is benefit for the safety of lithium-ion batteries.
    研究快报
    UV Cure for Multi Thiol-Vinyl Silizane and Pyrolysis
    SONG Jia-Le, CHEN Li-Xin*, WANG Ya-Zhou, WANG Ru-Min
    2007, 28(9):  1801-1803.  doi:
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    Si3N4 ceramic was prepared with pyrolyzing ceramic precursor of UV cured multi thiol-vinyl silizane. The results of in-suit FTIR show that thiol-vinyl silizane curing system was polymerized rapidly with a little photoinitiator. The photopolymerization rate was promoted, but the final vinyl bond conversion was depressed with enhancing the functionality of thiol group. The results of DMA and TGA show that Tg of the copolymer films of thiol-vinyl silizan cured by UV was elevated, however, the maxiumu rate of mass loss was decreased with increasing the functionality of thiol group. The ceramic yield was determined by the composition of copolymer and was independent of the thiol functionality. A majority of Si3N4 microcrystalline was obtained after pyrolyzing at 1400 ℃ for 15 h in N2 atmosphere.
    研究简报
    Synthesis of Branched PEG-b-PCL Block Copolymer
    REN Ya-Ran, SHI Yan*, FU Zhi-Feng
    2007, 28(9):  1804-1806.  doi:
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    A novel branched block copolymer was synthesized with self-condensing vinyl polymerization(SCVP) of macroinimer, PEGMA-b-PCL-Br, via atom transfer radical polymerization(ATRP). The macro-inimer was prepared with enzyme-catalyzed ring-opening polymerization(ROP) of ε-caprolactone(ε-CL) with poly(ethylene glycol)methacrylate(PEGMA) as the initiator and esterification of the ω-hydroxyl group of the obtained PEGMA-PCL with α-bromoisobutyryl bromide.
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