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    10 July 2009, Volume 30 Issue 7
    Review
    Stability of Direct Methanol Fuel Cells
    CHEN Wei-Min, XIN Qin*
    2009, 30(7):  1259-1267. 
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    Direct methanol fuel cells are promising power sources because of their advantages such as high power densities and good portabilities. With the development in technologies and the progress towards commercializations, the operating stability becomes more and more important. Among many factors resulting in cell performance losses, the deterioration of electrocatalysts, the variation in membrane electrode assembly structures, and the contamination caused by impurities play important roles. In this paper, recent studies concer-ning the performance degradation of direct methanol fuel cells are reviewed, and several factors influencing the operating stability of fuel cells are discussed.

    Articles
    Biomimetic Synthesis of Calcium Carbonate on Cellulose-polyester Fibrous Film
    JIAO Peng-Wei, WANG Jian-Ming, ZHOU Jie, WANG Dan, FENG Lin1*, JIANG Lei
    2009, 30(7):  1268-1271. 
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    With oleic acid as soft template, the biomimetic synthesis of CaCO3 on Jetspun ClothTM film was performed by slow gas diffusion method. The preadsorption of oleic acid and Ca2+ was characterized by the ATR-FTIR spectroscopy. The characterization of the deposition of CaCO3 on Jetspun ClothTM film was carried out using scanning electron microscope, showing a CaCO3-polymer film hybrid structure.

    Synthesis, Spectral Properties and Catalytic Oxidative Dechlorination of 2,4,6-Trichlorophenol of Water-soluble Tetra-(p-Sulfophenyl)porphyrin and Its Metalloporphyrin Complex
    LIU Shuang-Yan, REN Qi-Zhi*, DING Xiao-Jian, WANG Ai-Qin, HOU Zong-Sheng, ......
    2009, 30(7):  1272-1278. 
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    Water-soluble porphyrin, tetra-(p-sulfophenyl)porphyrin(H2TPPS), and its metalloporphyrin complex(FeTPPS and ZnTPPS) were synthesized and characterized. The pH control for the reaction system and the use of dialytic bag can efficiently increase the yield and purity of the product. The structural traits and spectral properties were discussed by means of UV-Vis, fluorescence, 1H NMR and FTIR spectroscopic methods. The results show that the existence of the sulfonic groups enhances the intermolecular π-π interaction and the aggregation of the porphyrins. FeTPPS was used as catalyst in 2,4,6-trichlorophenol oxidative dechlorination in the presence of H2O2 as oxidant, FeTPPS/H2O2 system was proved to be an efficient catalysis system and 766 turnover numbers was obtained.

    Growth of Silicalite-2 Zeolite Film in Microchannels of Biomorphic Porous SiC Ceramics
    LUO Min*, LIANG Jun, FANG Jun-Zhuo, WANG Zheng
    2009, 30(7):  1279-1283. 
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    Aligned Silicate-2 zeolite membrane was synthesized by in situ seeding and secondary crystal growth in microchannels of biomorphic porous SiC ceramics support. The Silicate-2/SiC composite materials were characterized by XRD, SEM and BET. The effects of synthesis temperature and seed surface pre-treatment of the beech-derived SiC monolith were studied. The results show that a homogeneous coverage of 5 μm thick zeolite membrane within the pores channel of SiC monolith by Silicate-2 crystals was reached after in situ seeding at 120 ℃ for 36 h with a following hydrothermal treatment at 170 ℃ for 36 h. The film oriented with [101] axis perpendicular to the substrate surface. The structure composites exhibit a hierarchical pore structure with a BET specific surface area of 43.2 m2/g and microporous volume of 0.013 cm3/g. The weight percent of Silicate-2 in the final Silicate-2/SiC composites is about 9.5% after a coating procedure.

    Letters
    Synthesis of High Yield of Higher Endohedral Metallofullerenes
    LI Nan, LIU Jia, SHI Zu-Jin, XU Shu-Kun, GU Zhen-Nan
    2009, 30(7):  1284-1286. 
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    By the DC arc-discharge of graphite rods doped with other substances in He and NH3 mixing gas, higher endohedral metallofullerenes(EMFs) were synthesized in a high yield. This lays the foundation for the separation, purification and further study of higher EMFs. The doped materials act as heat carriers and at the same time catalyze the growth of higher EMFs, whereas NH3 suppresses the formation of fullerenes such as C60 and C70, etc.

    Preparation and Characterization of PbO@C Nanocomposites
    WANG Hui-Qi1, DING Guo-Rong2, ZHAO Yong-Nan1*, YU Jian-Guo1
    2009, 30(7):  1287-1289. 
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    Lead oxide nanoparticles embedded carbon composites have been fabricated via the pyrolysis of Pb(NO3)2 impregnated starch gel under a N2 gas flow. The products were characterized by XRD, TGA, and TEM. The mass ratio between starch and Pb(NO3)2 greatly affected the final produts. The particle sizes of PbO decreased with the content of starch increased in the starting gel. Gel with mass ratio of 85∶15 between starch and Pb(NO3)2 gave rise to well-dispered lead oxide nanoparticles with tubable size and narrow size distribution that embedded in the carbon matrix. The particle sizes were in the range of 9—15 nm. Varying the reaction temperature would change the form of lead oxide. Lead oxide in the products calcined at 1000 ℃ was mainly β-PbO.

    In Situ Synthesis of 4-[(2-Pyridin-2-yl)-1-(pyridin-2-yl)vinylthio]benzoic Acid and Its Copper Complex
    LIU Ming-Li, YIN Yan-Yan, SHI Wei*
    2009, 30(7):  1290-1292. 
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    In situ metal/ligand reactions have been investigated for decades and turn out to be efficient for discovery of new organic reactions and coordination compounds with novel topology and functionalities. 4-[(2-Pyridin-2-yl)-1-(pyridin-2-yl)vinylthio]benzoic acid(L) was in situ generated in solvethermal condition with CuO and CuBr2. A copper coordination polymer[Cu2(L)Br2]n(1) was obtained synchronously and characterized by X-ray single crystal diffraction, elemental analysis and FTIR spectrum. The Cu+ ions were bridged into a tetranuclear cluster by μ3-Br and μ2-Br ions, and the clusters were further linked into 1D ribbon-like chain. The intermolecular in situ elimination is rare but meaningful in the synthesis of organic compounds.

    Articles
    Research of Core-shell Emulsion Polymerization Using in-situ Near Infrared Spectroscopy
    GAO Wen-Ji, YUAN Hong-Fu*, QIU Teng, LI Xiao-Yu
    2009, 30(7):  1293-1299. 
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    Near-infrared spectroscopy was employed in monitoring the core-shell emulsion polymerization and emulsion copolymerization of styrene(St) and butyl acrylate(BA). The three different polymerizations are differentiated by the band assignment and principal component analysis(PCA). The reversal process of inverted core-shell structure can be visually revealed by this method. The soft independent modeling of class analogy(SIMCA) classification model was established, which provides scientific basis for using near-infrared spectrometry to discriminate the core-shell polymerization types.

    Analysis of Essential Oil from Cinnamomum cassia Presl by Microwave-assisted Extraction Coupled with Gas Chromatography-Mass Spectrometry
    ZHU Xiao-Nan, WEI Shi-Gang, WANG Hao-Nan, SUN Ying, JIANG Chun-Zhu, ......
    2009, 30(7):  1300-1304. 
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    The essential oil from Cinnamomum cassia Presl was studied by non-polar solvent microwave-assisted extraction(NPSMAE) coupled with gas chromatagraphy-mass spectrometry(GC-MS). The cinnamaldehyde as a main component in the essential oil was determined. The effects of type of solvent, temperature, extraction time and ratio of solid to solvent(m/V) were examined and optimized. Compared with UAE and HD, NPSMAE has several advantages such as shorter extraction time and higher extraction yield. The proposed method is suitable for the extraction of essential oil.

    Resonance Light Scattering Correlation Spectroscopy A New Single Nanoparticles Method
    WANG Kang-Lin, REN Ji-Cun*
    2009, 30(7):  1305-1308. 
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    Recently, we developed a new single nanoparticles detection method, called as resonance light scattering correlation spectroscopy(RLSCS). In this article, we first described the principle of RLSCS, and then optimized certain parameters of RLSCS system. Finally, we studied the effects of certain factors such as viscosity of solution, nanoparticle size and laser power on the translational diffusion of gold nanoparticles, and the reproducibility of the setup of RLSCS.

    Prediction of HLA-A*0201 Binding Peptides Using Binding-environment-based Peptide Representation
    ZHAO Pu, LI Tong-Hua*
    2009, 30(7):  1309-1313. 
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    In all vertebrates, there is a large genomic region or gene family that has a major influence on graft survival referred to as the Major Histocompatibility Complex(MHC). T cells only recognize antigens as a complex with MHC molecules. Therefore MHC binding peptides prediction is an important step in T cells epitopes discovery. To facilitate vaccine design, computational methods have been developed for predicting MHC-binding peptides. A large variety of machine-learning techniques are commonly used in this field. This work explored Support Vector Machine(SVM) as such a method for developing prediction systems of HLA-A*0201 by using experiment dataset. Data representations play a key role in SVM models, so we examined different types of inputs variables for predicting HLA-binding peptides. The AUCs of these SVM models were 0.932—0.936. Then this work proposed a new way to encode peptides, which uses the information of peptides′ binding environment, and achieved an impressive AUC of 0.953. The results of independent dataset prediction showed that the overall performance of our novel environmental encoding based SVM models is improved in comparison to other traditional encodings.

    Interaction of Keyhole Limpet Hemocyanin with Niclosamide and Its Derivative
    GUO Wei, WU Yong-Quan, ZHENG Lü-Yin, XU Li-Rong, FAN Xiao-Lin*
    2009, 30(7):  1314-1321. 
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    PEG200-niclosamide was obtained from niclosamide. The interaction between keyhole limpet hemocyanin(KLH) and niclosamide/PEG200-niclosamide was investigated by fluorescence spectra, synchronous fluorescence spectra, ultraviolet absorption spectra and circular dichroism(CD) spectra. It was shown that KLH fluorescence at 340 nm was quenched regularly with the addition of niclosamide/PEG200-niclosamide; the quenching constant decreased as temperature increased; and the quenching mechanism with KLH was suggested as a static fluorescence quenching process. The binding constants(K) were obtained respectively according to Lineweaver-Burk equation at different temperatures, while there was a weaker interaction of the PEG200-niclosamide with KLH than that with niclosamide. The calculated thermodynamic parameters(ΔH, ΔS) by Van′t Hoff equation indicated that the electrostatic interaction played major roles in the binding processes. The binding processes of KLH with niclosamide/PEG200-niclosamide were spontaneous inter-molecular interaction in which entropy increased and Gibbs free energy decreased. The distances between KLH and niclosamide/PEG200-niclosamide were less than 7 nm according to the theory of the Frster energy transference. The effects of niclosamide and PEG200-niclosamide on the conformation of KLH were further analyzed by synchronous fluorescence spectra and circular dichroism spectra. Both niclosamide and PEG200-niclosamide could be deposited and transported by KLH and they affected the conformation of KLH. The CD spectra proved that the α-helix contents of KLH decreased, and the relative contents of secondary structure units of KLH changed in these binding processes. The relationship between the molecule structures and their binding ability was discussed preliminarily by comparison of the interactions between KLH and niclosamide/PEG200-niclosamide..

    Molecular Interactions Between Imidazole-based Ionic Liquids and Gases Using Quartz Crystal Microbalance
    XU Xiu-Ming, LI Chang-Zhi, ZHAO Zong-Bao, WANG Jun-De, LI Hai-Yang*
    2009, 30(7):  1322-1325. 
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    A convenient method to measure the solubility and thermodynamic properties for ionic liquids(ILs) towards gases under atmospheric pressure was developed based on the quartz crystal microbalance(QCM) technique. By using ILs as sensitive coating of QCM, Henry′s constants of typical volatile organic compounds(VOCs) on five imidazole-based ILs were measured. The molecular interactions between ILs and VOCs were discussed based on the values of Henry′s constants. Results indicated that the QCM technique could be an efficient approach for studing the solubility property and interaction properties of ILs.

    Letters
    Synthesis and Performance of Polymeric Ionic Liquid as Stationary Phase for Gas Chromatography
    SUN Xiao-Jie, ZHANG Shao-Wen, WANG Fang, ZHENG Jing-Jing, WU Cai-Ying, ......
    2009, 30(7):  1326-1328. 
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    An ionic liquid bonded polysiloxane(PSOIL) was prepared through the reaction between 1-methylimidazole and γ-chloropropyl-polysiloxane and used as gas chromatography stationary phase for the first time. The column efficiency was 3200 plates/m after being conditioned at 210 ℃. Grob reagent, aromatic isomers and homologous series were employed to evaluate the selectivity of the column. The results demonstrate that the PIL stationary phase exerted good selectivity and high separation efficiency.

    Articles
    First Asymmetric Synthesis of (7R,10S)-Boivinianin B
    XU Bo-Yan, SONG Na, LI Wen-Ze, XIN Zhi-Jun, LI Ying*
    2009, 30(7):  1329-1331. 
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    (7R,10S)-Boivinianin B(1), a naturally occurring sesquiterpene which has a synthetically challenging 2,2,5-tri-substituted tetrahydrofuran skeleton, was isolated from Laurencia tristicha and Cipadessa boiviniana. First asymmetric synthesis of the title compound was developed by sharpless asymmetric dihydroxyation to generate a stereocenter which as a chiral pool in the next procedure and an intramolecular iodoetherification to construct the tetrahydrofuran skeleton. The method developed here will be a useful tool for the stereoselective synthesis of 2,2,5-tri-substituted tetrahydrofurans bearing sterically congested benzylic quaternary center.

    Synthesis of a Novel Bisimidazolium Branched Zinc Metalloporphyrin and Its Recognition for Halide Anion
    XIE Zhao-Yang, OUYANG Qin, ZHU Yi-Zhou, HUANG Wei-Wei, ZHENG Jian-Yu*
    2009, 30(7):  1332-1336. 
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    Artificial receptors that are capable of selectively binding anionic species show promise in the diagnosis and treatment of diseases, and in environmental remediation. Several anion receptors have been constructed from five-membered heterocycles, such as imidazole. In this article, an imidazolium branched zinc porphyrin was designed and synthesized as chemosensor because the electronic spectra of porphyrin were very sensitive to the change of the environment. The UV-Vis, fluorescence and 1H NMR studies revealed that this receptor could selectively bind F- and Cl- over other halide anions. After comparing with the imidazolium branched freebase porphyrin, the model of the anionic binding was considered as three-point cooperation with haloid anions through porphyrin core and two imidazole moieties.

    Self-assembling Structure and Mechanism of a Wedge-shaped Peptide Detergent A3V3D
    CHEN Yong-Zhu, QIU Feng, ZHAO Xiao-Jun*
    2009, 30(7):  1337-1341. 
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    A wedge-shaped peptide detergent A3V3D was designed by changing the amino acid sequence of traditional peptide detergents. Although the secondary structure of this peptide is random coil as revealed by circular dichroism(CD) assessment, it can still undergo well-ordered self-assemble in water solution into stable, smooth and straight nanofibers, which are observed by transmission electron microscopy(TEM) and atomic force microscopy(AFM). Pyrene probe fluorescence analysis indicated that it could form hydrophobic domains in which pyrene molecules were imbedded. It was believed that driven by its wedge-like geometrical shape, A3V3D undergoes self-assemble in the form of cylindrical micelles, making it a novel self-assembling peptide material, and indicating the critical role of geometrical shape effect in controlling the self-assembling behavior.

    Investigation of Chiral Recognition of β-Cyclodextrin Toward 1,1′-Bi-2-Naphthol Enantiomers in the Presence of Different Alcohols by Fluorescence and HPLC
    LI Wei, ZAI Yan-Qiang, GUO Lei, XIE Jian-Wei
    2009, 30(7):  1342-1347. 
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    The chiral recognition of β-cyclodextrin(β-CD) to R,S-1,1′-bi-2-naphthol(BiNOL) has been investigated by fluorescence probe spectroscopy and high performance liquid chromatography(HPLC) in the presence of various alcohols or mobile phases. The effects of alcohols on the chiral recognition of CD/R or S-BiNOL have been discussed based on the binding constants and quenching constants. Chiral discrimination in the quenching of R,S-BiNOL complexed to β-CD was observed with adding alcohols, belonging to static quenching. The inclusion interaction between R,S-BiNOL and β-CD was significantly affected with the addition of alcohols and phosphate salt, and leading to the chiral selection or chiral resolution enhanced. The results of two methods are consistent for the chiral recognition of β-CD/R,S-BiNOL inclusion. The chiral recognition mechanism of R,S-BiNOL by CD was well explained by these experiments.

    Design, Synthesis and Bioactivity of New N-Methoxycarbamate Containing Pyrazole
    LI Miao, ZHANG Jin-Bo, YANG Ji-Chun, LI Zhi-Nian, LIU Chang-Ling, LI Zheng-Ming
    2009, 30(7):  1348-1352. 
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    Strobilurins are one of the most important classes of agricultural fungicides. To discover new strobilurin analogues with high pesticidal activity, a series of new N-methoxycarbamate derivatives containing substituted pyrazoles 3a—3r were synthesized from substituted aryl alkyl ketones as starting material by esterification, cyclization and condensation. The structures of substituted pyrazole derivatives were confirmed by 1H NMR, IR and elemental analysis. Preliminary biological evaluation show that compounds 3 have good fungicidal activity against P. oryzae, P. cubensis and E. graminis at 400 mg/L. The compounds with R1=methyl or methoxy substituted phenyl have best activities against P. oryzae. The compounds with R1=phenyl or methyl substituted phenyl have higher activities against P. cubensis and E. graminis than the others and the compounds with R2=methyl have higher activities against fungi than that with hydrogen.

    Novel Trifunctional Salicylaldehyde Schiff Base Derivative with GPX, SOD and CAT Activities
    LI Huan-Min, GAO Nan, LIU Lei, SHEN Si-Le, LUO Gui-Min*
    2009, 30(7):  1353-1356. 
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    Glutathione peroxidase(GPX) is one of the most crucial antioxidant enzymes in a variety of organisms; it catalyzes the reduction of H2O2 by reduced glutathione(GSH). We used sodium salicylaldehyde-5-sulfonate as the parent of the mimic, then the catalytic group of GPX, —SeH, was introduced to obtain a salicylaldehyde Schiff base compound, which was chelated with Mn and oxidized in air to obtain the final product. Its structure was proved by NMR, MS, IR and its antioxidant ability was tested. The product was demonstrated to have GPX, SOD and CAT activities at the same time, good solubility in water and strong ability to resist oxidative damage. Thus, the trifunctional enzyme mimic possesses a good potential in medicinal application.

    Cyclopropanation Reaction and Diastereoselectivity of Propargyl Sulfur Ylide with Acrylates
    LIU Wen-Jian, LU Hui-Zhe, XIAO Yu-Mei, WANG Ming-An, DU Feng-Pei, FU Bin, LI Nan
    2009, 30(7):  1357-1360. 
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    The cyclopropanation of propargyl sulfur Ylide with acrylate usually gave poor yield because of several competing reactions such as [2,3]-σ atropic rearrangement were also involved in this system. In our research, a higher yield(75%) and high diastereoselectivity(96%d.e.) for trans-2-ethynyl cyclopropane carboxylate were obtained by changing the structure of sulfur ylide and optimizing the reaction conditions. The mechanism and diastereoselectivity of the reaction were studied via the density functional theory method. High selectivity toward trans cyclopropanes are predicted on the basis of the relative activation energies of diastereomeric torsional transition states and the thermodynamic satbility of products. The energy differences between these transition states could be rationalized with the help of weak intramolecular stereoelectronic interactions.

    3D-QSAR Study of Novel 5-Substituted Benzenesulfonylurea Compounds
    WANG Mei-Yi, MA Yi, LI Zheng-Ming*, WANG Su-Hua
    2009, 30(7):  1361-1364. 
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    Comparative molecular field analysis(CoMFA ) method was applied to the study of the three-dimensional quantitative structure activity relationship(3D-QSAR) on 26 novel 5-substituted benzenesulfonylurea compounds. A reasonable model with predictive ability was obtained from the investigation(R2=0.948, F=91.364, SE=0.141). The results show that herbicidal activity is closely related to the steric and electronic properties of the 5-position of the benzene ring. The contour maps based on the analysis of steric and electrostatic CoMFA coefficients can not only explain the relationship between the structures and biological activity, but also lead to insight into the further design of highly active title compounds.

    Studies on Graft-polymerization of Polystyrene Surface by Plasma Technology
    WAN Hai-Yan, WEI Yan-Lin, ZHAO Bao-Ming, CHEN Ya-Shao*
    2009, 30(7):  1365-1370. 
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    Polystyrene(PS) was pretreated by O2 plasma, then N-vinylpyrrolidone(NVP) was graft-poly-merized on PS surface in the Ar plasma environment. The effect of O2 plasma pretreatment on surface free energy of PS was investigated by means of contact angle(CA) and surface free energy(SE) measurements. As the result, the optimum conditions of O2 plasma pretreatment on PS surface were power 50 W, pressure 40 Pa and time 3 min. The surface composition and properties of the modified PS between pre- and post O2 plasma treatment and graft polymerization were studied by ATR-FTIR, XPS, and DCA measurement. The results show that the NVP is successfully graft-polymerized on PS surface by plasma technology and the hydrophilicity of the modified PS surface markedly increased. The PS surface graft-polymerized was easily spreaded by water due to the increase of polar group and roughness. Further, the receding angle decreased obviously and the contact angle hysteresis was significant because of the reconstruction of the polymer chain on the PS surface.

    Preparation of Aluminum Superhydrophobic Surface with Nano-Micro Mixed Structure by SDBS/HCl Etching Method
    PAN Li-Ning, DONG Hui-Ru*, BI Peng-Yu
    2009, 30(7):  1371-1374. 
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    The SDBS/HCl mixed solution was used to etch aluminum surface, and some nano-micro mixed structures were appeared on the surface. After modified by 1H,1H,2H,2H-perfluorodecyltriethoxysilane(FDTES), the aluminum surface was reached superhydrophobility, and the water contact angle was more than 160°. The SEM experimental results showed that the aluminum superhydrophobic surface was of nano-micro mixed structure. According to the phenomenon, the bubble assisted etching mechanism(pit-etching and dislocation etching) was used to primarily explain the cause of the two-step mixed structures. Moreover, the experiments of different pH and different exposure time showed the aluminum superhydrophobic was very stable.

    Asymmetric Hydrogenation of Ethyl Pyruvate on Chirally Modified Pt Catalysts Supported on Periodic Mesoporous Resols
    SHEN Ya-Li, LI Xiao-Hong*, SONG Li-Ying, WANG Hong-Na, WU Peng
    2009, 30(7):  1375-1379. 
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    5.0%(Mass fraction) Pt catalysts supported on FDU-14, a kind of periodic mesoporous resols, were prepared by an impregnation method using two different Pt precursors, H2PtCl6 and Pt(NH3)4Cl2. These Pt/FDU-14 catalysts were characterized by XRD, N2-sorption, TEM and CO chemisorption. The Pt/FDU-14 catalysts can be effectively applied in the asymmetric hydrogenation of ethyl pyruvate after chirally modified with cinchonidine. The Pt/FDU-14 catalysts derived from H2PtCl6 afforded better conversions of ethyl pyruvate due to higher Pt dispersion and smaller Pt particle size, the initial activity (TOF) reaching 21092 mol/(mol?h) in acetic acid. While the Pt/FDU-14 catalysts derived from Pt(NH3)4Cl2 exhibited higher chiral induction ability and as high as 81.4% e.e. value of (R)-(+)-ethyl lactate was achieved in acetic acid. Due to the strong hydrophobicity of FDU-14 with pure organic framework, Pt/FDU-14 also worked well in water and can be recycled easily for more than 10 times without distinct loss of activity or enantioselectivity.

    Catalytic Performance of MCM-56 Molecular Sieve for Benzene Alkylation with Propylene
    ZHANG Yu, ZHAO Fei, LI Zheng, ZHAO Yin, DENG Guang-Jin, XING Hai-Jun, ......
    2009, 30(7):  1380-1385. 
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    MCM-56 zeolite was prepared by hydrothermally dynamic method. The as-made MCM-56 was detemplated by treating with a 30%H2O2 solution to obtain MCM-56(H2O2) zeolite instead of being treated with high-temperature calcination. The structure and acid properties of samples were studied by means of XRD, N2 adsorption-desorption, NH3-TPD and FTIR. The BET surface area of MCM-56(H2O2) can be improved significantly by hydrogen peroxide detemplation. A higher external surface area of 301 cm2/g was obtained for HMCM-56(H2O2) compared with 134 cm2/g for HMCM-56(C). The amount of acid sites has been increased by hydrogen peroxide treatment, while the acid strength has not been modified. Both the HMCM-56 zeolite detemplated by H2O2 and by calcination were used in benzene alkylation with propylene in liquid phase. Under our operation condition, HMCM-56(H2O2) shows a relative high activity and selectivity to cumene than HMCM-56(C), especially under a relative low reaction temperature and benzene-to-propylene molar ratio.

    Volumetric Properties of Binary System C6H5CH3-DMF at 293.15 K
    HOU Hai-Yun*, WANG Xiao-Xian, PENG San-Jun, GENG Xin-Peng
    2009, 30(7):  1386-1391. 
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    The densities of binary solution C6H5CH3-DMF(toluene-N,N-dimethylformamide) at 293.15 K were measured by use of the Anton Paar 4500 vibrating-tube densimeter and the dependence of density on molar fraction was fitted by the least-square method with the standard deviation 0.005 kg/m3, the molar fractions of toluene for the binary solution is from 0 to 1. The apparent molar volumes of C6H5CH3 and DMF in the binary system C6H5CH3-DMF were separately calculated from the density data, and the optimized dependences between apparent molar volumes and molar fractions and mass fractions were also determined respectively by the nonlinear least-square regression, and further more, the limiting partial molar volumes, the standard partial molar volumes and the molar volumes of C6H5CH3 and DMF were also obtained from the functions limits. At the same time, the excess molar volumes for the binary solution were calculated and were fitted by the fourth-order Redlich-Kister equation well, so the Redlich-Kister coefficients and the excess molar volume extremum were obtained. Furthermore, the excess partial molar volumes of C6H5CH3 and DMF were calculated and the dependences of the excess partial molar volumes on molar fractions of C6H5CH3 were fitted with the three-parameter polynomial. The limiting excess partial molar volumes of C6H5CH3 and DMF were also obtained from the polynomials limits as well as from the Redlich-Kister equation coefficients.

    Electronic Structures and Spectroscopic Properties Studies of Phosphorescent Iridium(Ⅲ) Complexes with Phenylpyrazole Ligands by Density Functional Theory
    GU Xin, ZHANG Hou-Yu*, FEI Teng, DUAN Gui-Hua, MA Yu-Guang*, LIU Xiao-Dong
    2009, 30(7):  1392-1396. 
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    The electronic structures and spectroscopic properties ofphosphorescent Ir(Ⅲ) complexes Ir(ppz)3, Ir(ppz)2(pic), Ir(ppz)2(acac) and Ir(ppz)2(dbm)(ppz=phenylpyrazole, pic=picolinate, acac=Pentane-2,4-dione and dbm=dibenzoylmethane), were investigated theoretically. Density functional theory(DFT) and time dependent DFT calculations were performed on the ground and excited states of the investigated complexes to provide insight into the structural, electronic, and optical properties of these systems. Calculated results testify that ancillary ligands have little influence on the highest occupied molecular orbital(HOMO) and great effect on the lowest unoccupied molecular orbital(LUMO) by lowering the LUMO energy levels dramatically. The transition of Ir(ppz)3 is attributed to d(Ir)+π(ppz)→π*(ppz); whereas that of Ir(ppz)2(pic) is related to d(Ir)+π(ppz)→π*(pic); Ir(ppz)2(acac) and Ir(ppz)2(dbm) are categorized as d(Ir)+π(acac/dbm)→π*(acac/dbm) charge transfer. Emission color of iridium complexes could be tuned by choosing congruent ancillary ligands.

    Photochemical Synthesis and Characterization of Gold@Palladium Core-Shell Composite Nanoparticles
    DONG Ying-Nan, DONG Shou-An*, TANG Chun
    2009, 30(7):  1397-1401. 
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    The combined gold and palladium bimetallic nanoparticles were received significant attention because of their special catalytic properties and Surface-enhanced Raman scatterings. In this paper, we report a new synthesis of Au@Pd core-shell composite nanoparticles by the photochemical method. The bimetallic nanoparticles with an Au core@Pd shell composite structure were synthesized in PEG-acetone solution by UV photochemical reduction, using both approaches of simultaneous reduction of Au(Ⅲ) and Pd(Ⅱ) ions and Au seeding growth in the presence of Pd(Ⅱ). The bimetallic nanoparticles sizes obtained by two approaches are between 5.6—4.6 and 4.6—6.2 nm, respectively. The sizes of composite particles and the thickness of the palladium shell can be tuned by varying molar ratio of Au(Ⅲ) or Au(0) and Pd(Ⅱ). Based on the characterizations by UV-Vis, XPS, TEM and HR-TEM, an Au core@Pd shell nanostructure was confirmed and a special changing tendency of the composite particle size with a changing of Au∶Pd molar ratio was found. The effect of the Pd shell gaining d-electrons from the Au core and the mechanism of forming Au core@Pd shell nanostructure were discussed.

    Studies on Molecular Structure of Hypericin and Its Interactions with HIV-1 Protease by Molecular Modeling
    QU Xiao-Bo, SU Zhong-Min, HU Dong-Hua, BAO Yong-Li, MENG Xiang-Ying, WU Yin, ...
    2009, 30(7):  1402-1405. 
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    Hypericin is a virucidal agent with activity against cancer and a broad range of viruses. However, its pharmacology and mechanism of action are still unclear. This investigation focus on the possible inhibits activity of hypericin on HIV-1 protease(HIV-IP) function and related pathways. Results indicate that hypericin is rigidly held in the catalyst active site of HIV-1P close to the catalyst residues of ASP-A25 and ASP-B25 with hydrogen bond interaction. These results may provide insights for study on antivirus activity of traditional Chinese medicine.

    DFT Theoretical Study on Nitrogen-rich Compounds C6H6-n(N3)n(n=1—6)
    LIU Xiao-Fang, XU Wen-Guo*, LU Shi-Xiang
    2009, 30(7):  1406-1409. 
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    The heats of formation(HOFs) were calculated for nitrogen-rich compounds C6H6-n(N3)n(n=1—6), via density functional theory(DFT) with 6-31G* basis set. We chose be nzene and HN3 as reference compounds in the process of designing isodesmic reactions. The relationship between the HOFs and the molecular structures is discussed. The results show that the HOFs of the title compounds linearly increase with increasing number of azide groups. The relative stabilities of the title compounds are discussed in terms of Mulliken charge, bond order, and the energy gaps between the frontier orbitals. All of the geometries of the title compounds were fully optimized without applying symmetry or structural constraints. This was accomplished via the default Gaussian convergence criteria. All of the optimized structures were characterized as true local energy minima on the potential energy surfaces, without imaginary frequencies.

    Specific-site PEGylation of Hirudin on Ion-exchange Column and Theoretical Prediction and Analysis of Modified Sites by Molecular Dynamics Simulation
    ZHAO Jun, LI Xue-Qin, XIU Zhi-Long*
    2009, 30(7):  1410-1416. 
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    Hirudin, a remarkably stable molecule with blood anticoagulant activity, is the most potent thrombin inhibitor in nature. But the short half life in blood plasma limits the application of hirudin in medical care. PEGylation is widely used to prolong the half life of proteins and peptides in plasma. However, the potential PEGylation sites of hirudin are numerous and it is difficult to confirm the actual PEGylation sites. In this paper, based on our experiment results of PEGylated hirudin in solution phase PEGylation and on-column PEGylation, hirudin and hirudin/thrombin complex had been simulated using molecular dynamics to predict the Lys PEGylation sites of hirudin. The results show that during the liquid-phase PEGylation, lysine residues are easy to be PEGylated except for Lys47, while during the solid-phase PEGylation, only Lys35 and Lys27 are easy to be PEGylated. And the PEGylation product can be stable when Lys35 is chosen to be the PEGylation site.

    Theoretical Study of One- and Two-photon Absorption Properties for Two Series of Star-burst-typed Pseudo Octupolar Molecules
    YANG Zhao-Di, FENG Ji-Kang*, REN Ai-Min
    2009, 30(7):  1417-1422. 
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    The systemically theoretical study for the one- and two-photon absorption properties of two series of star-burst-typed pseudo octupolar molecules were completed(a series are benzene-centered and b series are triphenylamino-centered). The calculation results show that series b have larger TPA cross-sections and longer one- and two-photon absorption maximal wavelength. The TPA cross-sections of three-branches pseudo octupolar molecules increase over 3 times relative to their single branch because of dipolar interaction between branches. The molecule containing 1,3,4-oxadiazole has larger TPA cross-sections in comparison with that containing 2,1,3-benzothiadiazole, however its TPA maximum wavelength is not located in IR or near-IR region.

    Homology Modeling and Docking Studies of Novel α/β Hydrolase Fold Proteins W14 and W15
    ZHOU Yi-Han, LUO Quan, HAN Wei-Wei, YAO Yuan, LI Ze-Sheng*
    2009, 30(7):  1423-1426. 
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    Three dimensional structure of novel α/β hydrolase fold proteins W14 and W15 were modeled by using homology and molecular dynamics methods. On the basis of the modeling, the components and the structures of active sites in W14 and W15 were analyzed and compared. The docking of 1-naphtyl acetate with the two proteins was also performed and compared. Gly82 and Val13 were key residues to form the oxyanion-hole and stabilized the negatively charged transition state that occurs during hydrolysis. Other important residues for binding were also identified.

    SnCNN: A Molecule Containing Sn≡≡C Bond
    ZHANG Wen-Bin, SHI Guo-Sheng, DING Yi-Hong*, SUN Chia-Chung
    2009, 30(7):  1427-1430. 
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    Triply bonded compounds RE≡CR′ that comprise higher-row elements are known to differ significantly in chemical bonding and reactivity from those of the traditional alkyne species. So they have formed the recent hot topic of the main-group chemistry researches. Unfortunately, these triply bonded species are usually unstable in kinetics towards conversion to doubly bonded SnC(R)R′, making their experimental study rather difficult. To our knowledge, there was only one experiment that indirectly suggested the existence of Sn≡C bonding through the de-nitrogen of ArSnC(N2)SiMe3 via spectroscopic technique. Therefore, search of kinetically stabilized Sn≡C compounds still remains a great challenge in main-group chemistry. For this sake, we report a detailed potential energy surface study on the four-atomic molecule [SnCN2] at the CCSD(T)//B3LYP level. It was shown that the linear isomer SnCNN possesses good thermodynamic and kinetic stability. Structural and bonding analysis indicates that the isomer has a Sn≡C triple bond. Further stabilization of the SnCNN skeleton could be realized via effective coordination by transition-metal carbonyls. Our study is expected to provide theoretical support for future experimental synthesis and characterization of the kinetically stabilized Sn≡C compounds.

    Letters
    Studies on Intermolecular Synergistic Antioxidant Activity in Glyceride Tri-ferulate
    YAO Tong-Wei, DU Li-Bo, YANG Yi, XU Yuan-Chao, JIA Hong-Ying, LIU Yang*
    2009, 30(7):  1431-1433. 
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    A glyceride containing three ferulic groups was first synthesized in order to investigate intermolecular synergistic antioxidant activity. The antioxidant activity was evaluated via a radical-scavenging reaction of DPPH˙ radical. Although the scavenging capacities of both antioxidants, ferulic acid and glyceride tri-ferulate, were roughly equal, the apparent activation energy(Ea) of 19.50 kJ/mol for glyceride tri-ferulate is obviously lower than that of 28.80 kJ/mol for ferulic acid. The synergistic effect on Ea was further explained by a parallel π-π-stacking interaction.

    Articles
    Soap-free Seeded Dispersion Polymerization Toward Monodisperse pH- and Temperature-Responsive Microgels
    LI Xin*, ZUO Ju, LIU Ru, LI Yong
    2009, 30(7):  1434-1438. 
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    Monodisperse core-shell microgels with pH- and temperature-sensitivity were prepared by soap-free seeded dispersion polymerization with N-isopropylacrylamide and 2-vinylpyridine as main monomers. Scanning electron microscopy and dynamic laser light scattering were employed to investigate the structure and property. Independent and unperturbed pH- and temperature-sensitivity were observed in the swelling investigation, i.e., the volume phase transition temperature (VPTT) of the microgels keeps almost the same as that of pure poly(N-isopropylacrylamide) (PNIPAM) gels. It is concluded that pH-ionizable monomer with local distribution does not perturb the VPTT of PNIPAM gels.

    Preparation and Bioactivity of the Composite of PLGA and Hydroxyapatite Nanocrystals Surface-grafted with L-lactic Acid Oligomer
    YU Ting, LIU Ya*, WANG Yu, JING Xia-Bin, ZHANG Pei-Biao*, CHEN Xue-Si
    2009, 30(7):  1439-1444. 
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    The hydroxyapatite(HA) nanocrystals of 100—200 nm in length and 20—30 nm in width were hydrothermally synthesized by the reaction of phosphoric acid and calcium hydroxide. Lactic acid oligomer surface grafted HA(op-HA) nanoparticles were obtained by oligomeric lactic acid with a certain molecular weight grafting onto the HA surface to form a Ca carboxylate bond in the absence of any catalyst. The op-HA was further blended with poly(lactide-co-glycolide)(PLGA) to prepare the nanocomposite of op-HA/PLGA. FTIR, TGA, ESEM and EDX were used to analyze grafting reaction, the graft ratio of op-HA, surface topography and calcium deposition of the composites, respectively. The rabbit osteoblasts were seeded and cultured on the surface of composites in vitro. The cell morphology, adhesion, proliferation and gene expression were evaluated with FITC staining, NIH image J software and the analysis of real-time PCR, respectively. The results show that the graft ratio of op-HA is 8.3%(mass fraction). The op-HA/PLGA nanocomposite possessed more suitable surface properties, including roughness and plenty of calcium and phosphor. It exhibited better cell adhesion, spreading and proliferation of rabbit osteoblasts compared to pure PLGA. Its gene expression of Collagen-I, Bone Morphogenetic Protein 2(BMP-2) and Osteonectin were higher than that of PLGA. It indicated that the biocompatibility and osteogenic bioactivity of the op-HA/PLGA nanocomposite were improved obviously than that of the pure PLGA.

    Preparation and Characterization of Acetylene-terminated Polyimide
    DU Ying, DANG Guo-Dong, HU Nan-Tao, ZHOU Hong-Wei, CHEN Chun-Hai*
    2009, 30(7):  1445-1448. 
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    A new acetylene-terminated pre-polyimide was synthesized from 2,2-bis[4-(3,4-dicarboxyphenoxy) phenyl] propane dianhydride(BPADA) and 3-ethynylaniline(APA). The crosslinking behavior of the prepolymer was studied by differential scanning calorimetry and infrared measurements. The prepolymer bearing isopropylidene moiety exhibits a much lower melt viscosity at low temperature, and thus provides a wider processing window. The polyimide film cured at 250 ℃ had a glass transition temperature(Tg) at 363 ℃(tanδ). The thermal properties of the cured films were also evaluated. TGA curves show that the temperatures of 5% weight loss(Td5) of the cured film are 490 ℃ in nitrogen and 492 ℃ in air.

    Morphology of pPDA/ODA-PMDA Block Copolymer
    ZHAI Yan, ZHU Rong-Qi, GU Yi*
    2009, 30(7):  1449-1453. 
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    pPDA/ODA-PMDA block copolymers(b-PIs) with different segment length of two components were prepared. Morphology and properties of their films were investigated by polarizingmicroscope(PLM), wide-angle X-ray diffraction(WAXD), transmission electron microscope(TEM) and tensil test. Measured results show all films of b-PI are crystalline. At first, phase separation of rigid segment of pPDA-PMDA takes place, forming nuclei. Then, semi-rigid segment of ODA-PMDA grows around the nuclei and forms small and imperfection grains. The number of nuclei is dependent of the ratio between pPDA and ODA and segment length of pPDA-PMDA(PP), while the size of grains is depended on the movability of ODA-PMDA(PO)segment. Morphology and properties of films can be controlled by changing the ratio of dianmines and segment length of two components.

    Influence of Polyether Segment Length on Mechanical Properties of Cured Epoxy Resins Based on Amino-terminated Poly(ethylene glycol) and Diglycidyl Ether of Bisphenol
    ZHAO Li-Ying, MA Hui-Ru, GUAN Jian-Guo*
    2009, 30(7):  1454-1458. 
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    An advanced amorphous AB-type thermosetting resin without nanophase separation was synthesized via directly moulding diglycidyl ether of bisphenol A(DGEBA) and α,ω-bisaminophenyl terminated poly(ethylene glycol)(BATPE). The stress-strain curve, dynamic mechanical thermal analysis and morphologies of impact fracture surfaces of the cured products were investigated as functions of flexible poly(ethylene glycol) segment length(MPE). The results show that the homogeneous epoxy resin without nanophase separation are available by incorporating poly(ethylene glycol) segments into epoxy crosslinked networks via chemically linked with DGEBA at both terminals, beneficial for increasing free volume fractions and strain relax rates. When MPE is extended, the glass transition temperature, the room-temperature Young′s modulus and tensile strength of the cured products decrease while toughness, elongation and modulus loss factors increase. The elastic mo-dulus of the cured products at low temperature(i.e. -40 ℃) enhances with increasing MPE. Consequently, thermosetting epoxy resins based on BATPE-DGEBA which exhibits excellent tensile strength, modulus and impact strength at moderate and low temperature are obtained by facile optimization of MPE.

    Preparation and Characterization of Pd Nanoclusters Templated by PAMAM Dendrimers
    LU Wen-Ting, LUO Yun-Jun*, LI Guo-Ping, ZHANG Xin-Qian, JIN Yu-Juan
    2009, 30(7):  1459-1463. 
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    Pd nanoclusters templated by methoxycarbonyl-terminated poly(amidoamine)(PAMAM) dendri-mers were successfully prepared in methanol. The complexation between Pd2+ ions and dendrimers was investigated by UV-Vis and FTIR spectophotometric method. These results show that Pd2+ ions are coordinated with the interior amine groups of PAMAM dendrimers. As shown in HRTEM images, reduction with NaBH4 resulted in well-dispersed and nearly size monodisperse Pd nanoclusters(2 nm, fcc) encapsulated in dendrimers. The investigation of UV-Vis data indicates that the size of particle increases with the metal-to-dendrimer molar ratio. Besides, due to the close-packed spherical periphery and rich ligands in interior cavities, dendrimers of higher generation are more effective for preparing Pd DENs with smaller size and better dispersion.

    Preparation of Honeycomb Pattern Organic-inorganic Hybrid Films by Breath Figure Method
    SHEN Yan-Ming*, WU Jing, LU Xin, TANG Yang-Jun, LIU Dan, LI Chang-Long, LI Tian-
    2009, 30(7):  1464-1468. 
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    PS/SiO2 organic-inorganic hybrid films with honeycomb patterns were prepared by Breath Figure method using organic solution of polystyrene and TEOS as casting solution. The prepared films were characterized by SEM, EDS, FTIR and XRD. Some effects such as PS concentration, PS/TEOS mass ratio, PS structure and solvent type were investigated. The results show that the perfect Honeycomb pattern films without defects within area of 0.8 cm2 can be obtained at the PS concentration ranges from 20 mg/mL to 50 mg/mL and PS/TEOS mass ratio less than 2. The films cast from the chloroform solution of dicarboxyl terminated PS were more perfect than those cast from the chloroform solution of monocarboxyl terminated PS. The perfect Honeycomb structure films could be obtained with both chloroform and benzene as solvents, but the pore diameter of films cast from benzene solution of PS was larger than that of films cast from chloroform solution of PS. Partial hydrolysis of TEOS occurred during the precursor was cast onto the substrate and both the partial hydrolyzed TEOS and complete hydrolyzed product SiO2 presented in the resulting membrane. Silicon and oxygen distributed uniformly in the resulting membrane.

    Dissolubility of the Cellulose in [AMMor]Cl/[AMIM]Cl
    WANG Mei-Ling, ZANG Hong-Jun*, CAI Bai-Xue, CHENG Bo-Wen
    2009, 30(7):  1469-1472. 
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    The mixed ionic liquid solvent N-methy-N-allylmorpholine chloride [AMMor]Cl/1-allyl-3-methylimidazolium chloride [AMIM]Cl can dissolve cellulose effectively. We surveyed the influence of the dissolution time and temperature to the dissolution properties. The chemical construction and thermostability of regenerated cellulose from the [AMMor]Cl/[AMIM]Cl were investigated with Fourier transform infrared(FTIR) spectroscopy, thermogravimetry(TG) and X-ray diffraction(XRD) measurements. Results show that the solubility cellulose in [AMMor]Cl/[AMIM]Cl is better than [AMIM]Cl under the same conditions. The cellulose samples without any pretreatment were readily dissolved in [AMMor]Cl/[AMIM]Cl in a relatively short time. In the course of dissolution, no other derivatizing reaction occurred and degrades slightly.

    Investigation on the Photo-polymerization of PDLC
    WANG Hao-Ming, RUAN Sheng-Ping, PENG Zeng-Hui, WU Feng-Qing, DONG Wei, ......
    2009, 30(7):  1473-1476. 
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    Polymer dispersed liquid crystal(PDLC) has extensive applications in non-linear optical material, displays and optical attenuation devices. In this paper, Ar+ laser was used as radiation source and Rose Bengal, N-phenyl glycine(NPG), dipentaerythrol hydrixy penta actylate, 1-viny-2-pyrrolidone were applied as photoinitiator, coinitiator, pre-polymer, thinner respectively to prepare PDLC with liquid crystal TEB30A. Ultraviolet spectra and spectrofluorimetry were applied to analyze the mechanism of the photo-polymerization reaction. The result indicates that by absorbing the photo energy, the initiator interacts with NPG to produce free radical, which induces the polymerization to produce the phase separation between the pre-polymer and the liquid crystal.