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    10 March 2007, Volume 28 Issue 3
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    高等学校化学学报2007年第28卷第3期目次
    2007, 28(3):  0-0000.  doi:
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    研究论文
    Preparation, Characterization and Negative Thermal Expansion Property of ZrWMoO8 Powders with Different Morphologies
    LIU Qin-Qin, YANG Juan, SUN Xiu-Juan, CHENG Xiao-Nong
    2007, 28(3):  397-401.  doi:
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    ZrWMoO8 powders with different morphologies were obtained by using ammonium tungstate, molybdate tungstate and zirconium tungstate as the starting materials by dehydration of the precursor ZrWMoO7(OH)2(H2O)2. The precursor was studied by thermogravimetric and differential scanning calorimetry(TG-DSC). X-ray powder diffraction(XRD), scanning electron micrograph(SEM) and X-ray fluorescence spectrometer(XRF) were used to study the influence of the varieties of the gelling agents on the crystallization process and crystal morphology of the resulted products. The results show that the kinds of gelling agent has a great influence on the morphologies of the resulted products, the thermal expansion coefficients of cubic ZrWMoO8 prepared with HCl as the gelling agent is -3.84×10-6 K-1 from 100 ℃ to 700 ℃.
    Synthesis, Characterization and Electrochemical Properties of Porphyrin-nicotinic Acid Binary Compounds
    CHENG Xiu-Li, CHEN Zheng-Xia, SUN Er-Jun, SHI Yu-Hua, SHI Tong-Shun
    2007, 28(3):  402-405.  doi:
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    Three porphyrin-nicotinic acid binary compounds were prepared by the nucleophilic substitution reaction of 5-[(4-bromopropyloxy)phenyl]-10,15,20-triphenylporphyrin, 5-[(4-bromopropyloxy)phenyl]-10,15,20-tri(4-methoxyphenyl)porphyrin, and (4-bromopropyloxy)phenyl]-10,15,20-tri(4-chlorophenyl)porphyrin with naotin, respectively. These compounds were confirmed by IR, 1H NMR, UV-Vis, and elemental analysis. The electrochemistry properties were studied by cyclic voltammetry.
    Synthesis, Crystal Structure and Magnetic Properties of a Single-molecule Magnet [Mn4(CF3COO)4(hmp)6]
    NA Li-Yan1,2, NING Gui-Ling1, ZHANG Feng-Jie2, WANG Bing2
    2007, 28(3):  406-409.  doi:
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    The preparation, X-ray structure characterization and magnetic properties are presented for a new mixed-valence tetranuclear manganese complex that functions as a single-molecule magnet(SMM), [Mn4(CF3COO)4(hmp)6], where hmp- is the anion of 2-(hydroxymethyl) pyridine and is a N,O bidentate chelate. The compound crystallizes in the monoclinic system, space group P21/c(No.14) with unit cell parameters a=1.3663(3) nm, b=1.4705(3) nm, c=1.4734(3) nm, β=98.51(3)°, V=2.9276 nm3 and Z=2. The structure of the complex shows a novel coordination of the trifluoroacetate(TFA) anions, with one anion acting as a monodentate ligand while the second one coordinating through both oxygens to the same Mn centre. Direct current magnetic susceptibility measurement in the 2—300 K temperature range supports a high-spin ground state. The presence of a frequencey-dependent alternating current susceptibility signal indicates that the individual molecule is acting as the magnet.
    Synthesis of Precursors ZrMo2-xWxO7(OH,Cl)2·2H2O and Cubic ZrMo2-xWxO8 Thermal Contraction Compounds by Acidic
    GUO Shu-Rong1, DENG Xue-Bin2, Ma Hui3, ZHAO Xin-Hua2
    2007, 28(3):  410-414.  doi:
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    The precursors, ZrW2O7(OH,Cl)2·2H2O(x=0 ,0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8), of cubic ZrMo2-xWxO8 were synthesized successfully by acidic steam hydrothermal no-wash(ASH-NW) method, in succession the preparation of cubic ZrMo2-xWxO8 were made from the precursors. The relative XRD intensity was proposed to characterize the saturated order degree(η'T) of the metastable order-disorder phases and the correlation was found that the n(Mo)/n(W) ratio is reduced, the order degree(η'T) is risen under the preparation condition. An argumentation was presented to discuss the effect of raw materials on the morphology of the intermediate phase as well as the products. Furthermore, the outline of the micro-process in which the ammonium salt was used as the raw material during the preparation of precursor was discussed.
    Design and Synthesis of a Visible Light Driven Photocatalyst LaCo0.5Ti0.5O3 with ABO3-type Perovskite Structure
    YANG Li-Bin1,2, JING Li-Qiang1, LI Shu-Dan1, JIANG Bao-Jiang1, FU Wei1, FU Hong-Gang1
    2007, 28(3):  415-418.  doi:
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    A novel ternary metal complex oxide, LaCo0.5Ti0.5O3, with ABO3-type perovskite structure was designed and synthesized by a sol-gel method at relatively low temperature, and were characterized by means of several testing techniques such as TG-DTA, XRD, XPS and UV-Vis DRS spectra. The results show that, compared with LaCoO3 and La2Ti2O7, the as-prepared sample exhibits a higher photocatalytic activity under visible light irradiation, and can be obtained at lower temperature. It can be proposed that the charge compensation effects make Co2+ and Ti4+ ions in raw material co-occupy uniformly B site in perovskite both as the forms of +3 valence, which is responsible for the lower temperature synthesis.
    Preparation of Radiolarian-like Mesoporous Silica from Water-diethyl Ether Binary Solvent System
    ZHAO Xiang, LIN Hao-Xiang, CUI Kai, YAO You-Wei, CAI Qiang, FENG Qing-Ling, LI Heng-De
    2007, 28(3):  419-421.  doi:
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    An interesting radiolarian-like silica spherulite was prepared from a water-diethyl ether binary solvent system, which is characterized by SEM, TEM, XRD, and adsorption experiments. The results indicate that the silica have a particular morphology and hierarchical structure, i.e., hollow interior and a crust wherein two types of mesopores with radiate orientation are located. This silica product embodies a novel morphosynthesis involving unstable water-oil interface.
    Permeation Characteristics of Molecularly Imprinted Polymer Membranes Synthesized by Compounds of Vanillin Series
    ZHANG Mo1, LU Chun-Yang1, HE Xi-Wen1, LI Wen-You1, ZHANG YU-Kui1,2
    2007, 28(3):  422-426.  doi:
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    Using vanillin or o-vanillin as the template molecules, composite molecularly imprinted membranes(MIMs) with Nylon or PVDF as supporting membrane were prepared via in-situ polymerization by UV-irradiation. The interaction between the template molecule and the functional monomer(methacrylic acid) was evaluated by absorption spectroscopy. The permeation experiment which was carried out with the mixed solution containing template and its competitive analogue shows that the transport trend of the substances through the MIMs hardly has something to do with the supporting material. But a perfect separation will be obtained when the chosen supporting material is suitable. When the competitive analogue is smaller than the template, it preferentially transports through the MIMs because of the size effect. But when they are the same in size, the size effect doesn't work. Then the template transports faster due to its complementary functional groups and shape with the imprinted sites on the MIMs. And when the competitive analogue is bigger than the template, the facilitated transport of the template is attributed to both the size effect and its complementary functional groups and shape with the imprinted sites.
    Preparation of Bovine Serum Albumin Capillary Monolith for the Separation of Histidine Enatiomers
    ZHU Tao-Yu, WU Pin-Duan, ZUO Na-Na, WU Jing-Hong, MA Zhi-Ling
    2007, 28(3):  427-430.  doi:
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    A series of monolithic capillary columns were prepared by copolymerization of GMA and EDMA in the presence of a porogenic solvent containing cyclohexanol and n-dodecanol. The influences of the contents of the porogenic solvent and GMA on the monolith morphology and osmosis were investigated. The capillary monolith matrixes were prepared under the optimized conditions, and BSA capillary monoliths were gained by epoxy method using BSA as the model ligand. The BSA capillary monolith coupled with capillary electrochromatography was developed for the separation of D,L-histidine, and showed a good result.
    Studies on the Chemical Change in the Process of Microwave-assisted Extraction of Flavonoids from Acanthopanax Senticosus Harms
    LIU Zhong-Ying1,2, HU Xiu-Li1,2, BU Feng-Quan2, DING Lan1, ZHANG Han-Qi1
    2007, 28(3):  431-435.  doi:
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    In the process of microwave assisted extraction(MAE), the chemical changes of the flavonoids in Acanthopanax Senticosus Harms were studied by HPLC-UV and HPLC-ESI-MSn. The influences of pressure and MAE time on the chemical changes were investigated. The experimental results demonstrate that rutin in the extract can be partly decomposed when pressure is over 300 kPa, as a result, the content of quercetin increases by the loss of rutinosyl from rutin. With the increase of microwave extraction time, extraction yields of hyperin, rutin, quercitrin and quercetin are firstly increased and then decreased. The higher the pressure is, the faster the extraction rate and the decomposition rate are, the shorter the extraction time for obtaining the highest yield is.
    研究论文
    Investigation of Post-chemiluminescence Reaction in Potassium Periodate-luminol System
    MA Ming-Yang1,2, L<SPAN lang=EN-US style=
    2007, 28(3):  436-440.  doi:
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    The post-chemiluminescence(PCL) reactions of glucuronolactone, mecysteineh hydrochloride, isoniazid, dopamine hydrochloride, lincomycin hydrocholoride, hydrocortisone, amoxicillin, antondine, adrenaline hydrochloride and noradrenaline bitartrate in potassium periodate-luminol system were discovered. The possible mechanism for the PCL reaction was discussed via the investigation of the CL kinetic characteristics, the chemiluminescence reaction(CL) spectra and the fluorescence spectra of some related substances. The flow injection PCL method for the determination of the 10 kinds of substances was established. The post-chemiluminescence analytical system based on potassium periodate-luminol reaction was established.
    Near Infrared Chemical Fingerprinting Based on Wavelet Transform
    YE Zheng-Liang, YU Ke, CHENG Yi-Yu
    2007, 28(3):  441-444.  doi:
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    Based on wavelet transform and data visualization, a type of NIR fingerprinting was proposed and applied to assessing the quality of Danshen(Radix salviae miltirrhizae). First, wavelet transform was performed to extract the feature information from the raw NIR spectra. And then, the extracted information was represented by the data visualization. The integral pattern difference of the Danshen samples could be identified intuitively with the proposed method. HPLC fingerprints were also collected, and they were used as the reference. It was shown that the results obtained from NIR fingerprint was consistent with that of the corresponding HPLC fingerprint. As a fast and non-destructive method for quality assessment of natural products, the potential of NIR fingerprinting is exemplarily shown in this paper.
    Investigations on Gastric and Colorectum Cancer by FTIR Spectroscopy
    LING Xiao-Feng1, XU Yi-Zhuang2, WANG Li-Xin1, LI Wei-Hong2, ZHANG Yuan-Fu2, YANG Zhan-Lan2, HOU Chun-Sheng1, ZHOU Xiao-Si1, WU Jin-Guang2, XU Zhi1
    2007, 28(3):  445-449.  doi:
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    Thirty-one pairs of FTIR spectra of samples, including gastric and colorectal cancer and the corresponding normal tissues, were collected after surgery. FTIR spectra of cancerous tissue were significantly different from those of normal tissues. (1) Alterations of bands related to lipid: 2955, 2920, 2870, 2850 and 1740 cm-1 appeared less frequently in malignant tissue(P<0.001). The ratio of I1460/I1400 in malignant tissue decreased significantly(P<0.001), indicating that the relative quantity of lipid in malignant tissue decreased significantly. (2) Alterations of bands related to protein: in malignant tissue, the band of N—H and O—H shifted to a lower wave number(P=0.025), suggesting that the degree of hydrogen-bonding of N—H and O—H increased. In malignant tissue, the ratios of I3375/I1460, I1640/I1460, I1550/I1460 raised(P<0.01), respectively. These changes illustrate that the relative quantity of protein to lipid in malignant tissue increased significantly. The ratio of HW1550/I1550 increased obviously(P=0.036), while HW1550 decreased significantly(P=0.05), compared with those of normal tissue. We can conclude that the secondary structure of protein in malignant tissue changed. (3) Alterations of bands related to carbohydrate: in malignant tissue, the ratio of I1160/I1460 reduced(P=0.002). It might be due to the lessen of glycoprotein on the surface of malignant tissue, reversely, the ratio of I1120/I1460 raised(P= 0.019). The possible reason was that the glucogen grains on the surface of the malignant tissue increased. (4) Alterations of band related to nucleic acid: in normal tissue, the peak of PO antisymmetric vibration was at (1241.61±6.15) cm-1. In malignant tissue, the band shifted toward a higher wave number(P=0.033) due to the decreased hydrogen-bonding of PO. FTIR spectroscopy could be a powerful tool for cancer diagnosis.
    研究简报
    Application of DNA-overoxidized Polypyrrole Composite Biosensor
    JIANG Xiao-Hua, LIU Wei-Qiang, CHEN Jian-Jun
    2007, 28(3):  450-452.  doi:
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    A promising electrochemical microsensor was fabricated by electrochemical immobilization of DNA on a carbon fiber electrode(CFE) through an overoxidized polypyrrole(PPyox) template for simultaneous determination of serotonin(5-HT) and dopamine(DA). Such a nano-thickness DNA-PPyox biocomposite modification layer exhibited a superior selectivity and sensitivity towards these neuronal amines comparing with a simple PPyox or DNA coating. This microsensor gave three separated differential pulse voltammetric(DPV) peaks at 0.38, 0.20 and -0.02 V for 5-HT, DA and 25000-fold excess of ascorbic acid(AA). The utility of this composite biosensor was demonstrated by the determination of 5-HT content in healthy human blood serum and DA in its hydrochloric injection.
    研究论文
    Studies on the Binding Geometry of Intercalation of 4-(2-Diethylamino-ethylamino)-8-oxo-8H-acenaphtho[1,2-b]pyrrole-9-carbonitrile to DNA by Molecular Spectra
    YANG Yuan-Yuan1, ZHANG Zhi-Chao1, SHENG Hui2, LIU Feng-Yu1, QIAN Xu-Hong1,3, XU Qin1, ZHANG Jing1,4
    2007, 28(3):  453-457.  doi:
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    The binding geometry of a heterocyclic compound, 4-(2-diethylamino-ethylamino)-8-oxo-8H-acenaphtho[1,2-b]pyrrole-9-carbonitrile(A1) to CT DNA was studied by using molecular spectroscopy. Deduced from SYBR Green-DNA melt curve, fluorescence spectroscopy, UV-Vis spectroscopy and circular dichroism(CD), there were two different interaction mechanisms involved in the whole interaction process depending on the the molar ratios of A1 to CT DNA base pairs. The binding geometry of A1 to CT DNA was investigated by the induced CD spectroscopy based on the different n(A1)/n(CT DNA) ratio. The value n(A1)/n(CT DNA)=0.20 was the turning point; when n(A1)/n(CT DNA)≤0.20, the intercalation orientation of A1 to the dyad axis of DNA double helix was heterogeneous and stacking of A1 on the surface helix of DNA was available when n(A1)/n(CT DNA)>020.
    研究快报
    Synthesis of Oligo(ethylenediamino) Modified Permethylated-β-cyclo-dextrins and Their Interactions with Bovine Serum Albumin
    KANG Shu, CHEN Yong, SHI Jun, MA Yu-Hong, LIU Yu
    2007, 28(3):  458-461.  doi:
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    Two oligo(ethylenediamino) mono-modified permethylated-β-cyclodextrins were prepared, and the complex stability constants for the 8∶1 complexation of some permethylated β-cyclodextrin derivatives with bovine serum albumin were determined by fluorescence and UV-Vis spectroscopy at 25 ℃ in phosphate buffer solution(pH=7.2). The results indicate that the permethylated β-cyclodextrin shows obviously enhanced binding ability as compared with native β-cyclodextrin and 2,6-methylated β-cyclodextrin, and the oligo(ethylenediamino) modified permethylated β-cyclodextrin derivatives show much stronger binding abilities. The enhanced binding ability can be derived from the cooperative effect of hydrophobic, electrostatic and hydrogen bonding interactions.
    研究论文
    Synthesis of Pennogenyl Saponins via Three Methods
    ZHANG Shou-Qin, ZHANG Jin-Song, WANG Chang-Zheng
    2007, 28(3):  462-466.  doi:
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    The pennogenyl saponins(7—12) were synthesized by using three important methods of glycosylation. As donors(1—6), glycosyl halide, trichloroimidate and thioglycoside were chosen to react with the acceptor pennogenin to investigate the results of these reactions. In these reactions the difference of steric hindrance between 3-OH and 17-OH of pennogenin was utilized skillfully and only 3-hydroxyl group of pennogenin could be connected with each kind of donors selectively and there was no reaction at 17-hydroxyl group which had no protection. The characteristic above makes it convenient to synthesize the compounds of pennogenyl saponins.
    Chemical Synthesis and Stability of Oligonucleotides Modified by Alkyl- or Alkoxy- on the Phosphonates
    LIANG Yuan-Jun, HE Jun-Lin, XU Liang, ZHANG Di, LIU Ke-Liang
    2007, 28(3):  467-471.  doi:
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    Four novel phosphoramidites with isopentyl, phenethyl, isopentoxy, phenethoxy attached to the phosphorus residue were synthesized through Grignard reaction or a sequential three-step substitution on PCl3 respectively. Four model oligonucleotides(5'-dTTTx TT-3', where Tx was formed by introducing each of the novel phosphoramidites above-mentioned) were prepared with high coupling yields to study the compatibility of the new building blocks to the customized DNA/RNA synthesis, and the stability of the oligonucleotides were tested under four kinds of deprotection conditions. Based on HPLC analysis and MALDI-TOF-MS measurement, the fast-deprotection strategy(concentrated ammonia, room temperature, 4 h) was suitable for the solid-phase synthesis of oligonucleotides containing above new building blocks. Undoubtedly, these novel phosphoramidites could be used as the building blocks for nucleic acids research.
    Synthesis and Properties of Photochromic 6-Chloro-8-bromo-spiro(indoline-2,2'[2H]benzopyran) Compounds
    TAN Ting-Feng1,2, HAN Jie1, PANG Mei-Li1, GAO Yong-Bin1, MENG Ji-Ben1
    2007, 28(3):  472-475.  doi:
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    A series of novel 6-chloro-8-bromo-spiropyrans were designed and synthesized. The structures of all the compounds were characterized by 1H NMR, IR, MS, and elemental analysis. Single crystals of 1',3',3',5'-tetramethyl 6-Cl-8-Br-spiro(indoline-2,2'-[2H]-benzopyran) were determined by X-ray single diffraction. Combined with UV-Vis absorption spectra, the photochromic properties of these compounds were studied intensively in different solvents. Moreover, the relationship between the structure, solvent polarity and photochromism were analyzed. The results show that and the compound takes on excellent photochromism in the strong polarity solvents, electron-donor groups in indoline moiety and solvents with a strong polarity made the maximum absorption wavelength to hypochromic shift.
    Growing Behavior of Cells on Single-walled Carbon Nanotubes Nonwoven Films
    MENG Jie1, SONG Li2, MENG Jie3, KONG Hua3, WANG Chao-Ying2, ZHU Guang-Jin1, XU Liang-Hua4, XIE Si-Shen2, XU Hai-Yan3
    2007, 28(3):  476-480.  doi:
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    Carbon nanotubes have attracted intensive interests in biomedical research in recent years. In this paper, a novel type of carbon nanotubes material so called nonwoven single walled carbon nanotubes(nonwoven SWNT) with nanotopographic structure and macroscopic volume was used as cell growing scaffold. The morphology and surface chemistry of nonwoven SWNT were observed and characterized by scanning electron microscopy(SEM) and X-ray photoelectron spectroscopy(XPS) respectively. The cells were cultivated in nonwoven SWNT and in other types of substrate as the control. The cells growth behavior including adhesion, proliferation and cytoskeletal development was investigated by using cell viability assay and confocal observation. The experimental results indicate that nonwoven SWNT exhibited a significant enhancement to the cells adhesion and proliferation in at least 3 weeks. Numerous and well organized cytoskeletal structures were observed when the cells were cultured in nonwoven SWNT. Additionally, an obvious promotional influence of the cells cultivated in nonwoven SWNT scaffold upon the proliferation of those growing in the other kind of substrate through cell-cell communication were found. The results obtained in this work are of significance to in vitro cell amplification in a large scale, tissue regeneration or guided repair, as well as biomedical device application.
    研究简报
    Regioselective Synthesis Mechanism and Crystal Structure of 2’，4”-O-Bis(trimethylsilyl)-6-O-methylerythromycin A 9-O-(1-methoxycyclohexyl) oxime
    LIANG Jian-Hua, YAO Guo-Wei, CAO Zhi-Ling, GAN Qiang, SHAN Chun-Yan
    2007, 28(3):  481-483.  doi:
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    2',4"-O-Bis(trimethylsilyl) 6-O-methylerythromycin A 9-O-(1-methoxycyclohexyl) oxime was regioselectively synthesized and characterized and its crystal structure was determined by the single crystal X-ray structure analysis. The crystal belonged to tetragonal system with I4 space group and a=b=2.9720(4) nm, c=1.4939(3) nm, V=13.195(4) nm3, Z=8, R=0.0587, wR=0.1263, S=1.004 for 11526 unique reflections. The crystal structure shows that the attack of methylation reagents was blocked by 9-oxime ether as result, a hydrogen bond formed between 11-OH and nitrogen of 9-oxime, and the attack of methylation reagents was blocked by 9-oxime ether, whereas the orientation of 6-OCH3 was located in the cave surrounded by several rings so that 6-OH was unique one to be exposed to methylation reagents. However, the congestion around 11-OH was loosened, which resulted from the orientation of protective group so that much 6,11-O-dimethyl product was yielded. Additionally, the crystal structure of 2',4"-O-bis(trimethylsilyl) erythromycin A 9-O-(1-methoxy-1-methylethyl) oxime was first disclosed as a comparison.
    Isolation and Identification of a New Furosteroidal Saponin from Fruits of Tribulus Terrestris L.
    XU Ya-Jiuan1,3, HUANG Xiao-Lie3, XIE Sheng-Xu3, XU Tun-Hai2, XU Dong-Ming3, ZHANG Yu-Jing1
    2007, 28(3):  484-486.  doi:
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    Traditional Chinese Medicine “jili”(Tribulus Terrestris L.) is the important medicine used to treat cardiovascular diseases. A new furosteroidal saponin, together with a known steroidal saponins, were isolated from the fruits of T. Terrestris L.. The structure of the new furosteroidal saponin, named Tribuluside A, was elucidated as 26-O-β-D-glucopyranosyl-(25R)-5α-furost-3β, 22α,26-triol-3-O-[β-D-Xylopyranosyl(1→3)]-[β-D-xylopyranosyl(1→2)]-β-D-glucopyranosyl(1→4)-[α-L- rhamnopyranosyl(1→2)]-β-D-galactopyranoside mainly by using 1D, 2D NMR techniques, ESI-MS analysis as well as chemical methods.
    研究论文
    Studies on Aggregation Behavior of α-Oxygen-bearing Substituted Phthalocyanines
    HUANG Xin1, ZHAO Fu-Qun1, LI Zhong-Yu1,2, ZHAO Peng1, TANG Ying-Wu1, ZHANG Fu-Shi1
    2007, 28(3):  487-491.  doi:
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    3-Phen/methoxyphthalonitrile was obtained via the reaction of 3-nitrophthalonitrile with phenol/methanol under the catalysis of anhydrous potassium carbonate. α-Aryl/alkoxy substituted phthalocyanines were synthesized by treating the corresponding substituted phthalonitriles in refluxing dimethylaminoethanol with or without metal acetate and were fully characterized by UV-Vis, 1H NMR, MS spectra and elemental analysis. It was found that α-oxygen-bearing substituted zinc phthalocyanines 1 and 3 can form J-type aggregates easily in non-coordinating solvents. The MALDI-TOF MS for the samples of 1 prepared from chloroform solutions gives the monomer and aggregate signals. The aggregates are broken up when a coordinating solvent is added to the solution. A possible mechanism on the formation of this self-assembly was proposed, which it was driven by the complementary coordination of the ether oxygen in the aryl/alk-oxy groups of one molecule to the core Zn of another molecule of phthalocyanine.
    Studies on Thermochemical Properties of Ionic Liquid Based on Transition Metal Ions System BMIC/ZnCl2
    YANG Jia-Zhen1, LI Ji-Guang1, FANG Da-Wei2,3, ZHANG Qing-Guo2,3, FENG Rong-Kai1, TAO Chuang1
    2007, 28(3):  492-495.  doi:
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    A colorless and transparent ionic liquid BMIC/ZnCl2 was prepared by mixing 1-butyl 3-methylimidazolium chloride(BMIC) and ZnCl2 with a molar ratio of 1:1 at 363.15 K under stirring in a glove box filled with dry argon. The molar dissolution enthalpies, ΔsHm, of BMIC/ZnCl2 in water with various molalities were determined by a solution-reaction isoperibol calorimeter at 298.15 K. In terms of Pitzer electrolyte solution theory, the molar solution enthalpy of BMIC/ZnCl2 at infinite dilution, ΔsH0m, and Pitzer parameters: β(0)LMX, β(1)LMX and CφLMX were obtained, respectively. According to Lecocq's viewpoint, ionic liquid BMIC/ZnCl2 with a molar ratio of 1:1 is a single compound BMIZnCl3. In terms of Glasser's theory and thermodynamic cycle, the standard molar hydration enthalpy of ionic liquid BMIZnCl3, (ΔH0+ +ΔH0-)=-497 kJ/mol, was calculated. The standard molar enthalpies of hydration of individual ions can be obtained from those of electrolytes, provided that the value of one ion is known. The standard molar enthalpies of hydration of cation BMI+ were estimated ΔH0+(BMI+)=-225 kJ/mol in literature so that the standard molar enthalpies of hydration of ZnCl-3 was obtained, that is, ΔH0-(ZnCl-3) =-272 kJ/mol.
    Investigation in Extremely Improved Ability of Resisting Ca2+ and Mg2+ for Alkyl Carboxylates Flooding System with Adding DSB
    XU Jun1,2, SUN Wen-Qi3, LI Gan-Zuo1, XU Jian1, ZHENG Li-Qiang1, WANG Hong-Qin2, ZHANG Gao-Yong1
    2007, 28(3):  496-501.  doi:
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    The natural mixed carboxylates(abbreviated as SDC) can be used to extremely improve the ability of resisting Ca2+ and Mg2+ when adding 3-(N,N-dimethyldodecylammonio)-2-hydroxy-propanesulfonate(abbreviated as DSB). SDC and SDC-DSB flooding system are tolerant to Ca2+ and Mg2+ up to 400 mg/L and 5.0×103 mg/L respectively. Their IFTmin are 10-3 mN/m, and the oil recovery reach 20% by using the core flood experiment. The surface tension and the critical micelle concentrations were measured for the systems of the sodium dodecanoate and DSB. By analysis the solubility product(Ksp) of fatty acid salt, we can know that the concentration of Ca2+ and Mg2+ ions in solution is increased along with the decrease of concentration of free fatty acid group. The interaction parameter βm between sodium dodecanoate and DSB can be calculated as -3.111, which reflects more strong reaction force. The mole fraction xm1 of sodium dodecanoate in the mixed micelles is 0.51. By the software Gaussian 03, we calculated the minimum energy for compound of DSB/dodecyl acid/Ca2+, and obtained the charge of dominating atom in this compound. These results show there are probably many “negative-charge hole” in the surface layer of micelle, thus, the Ca2+ and Mg2+ in solution can combined in the surface layer of micelles. So we can explain why the alkyl carboxylates flooding system extremely improved the ability of resisting to Ca2+ and Mg2+ with adding DSB.
    Synthesis of Styrene Carbonate Catalyzed Efficiently by Zinc Bromide and Tetra-n-butylammonium Halides
    SUN Jian-Min, WANG Lu ,WANG Ya-Li, QU Xue-Jian, JIANG Da-Zhen, XIAO Feng-Shou
    2007, 28(3):  502-505.  doi:
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    In this paper chemical fixation of CO2 was introduced for the synthesis of cyclic carbonate. Styrene carbonate can be synthesized via two routes, one is the cycloaddition of CO2 to epoxides and the other is oxidative carboxylation of styrene. The latter route couples the two processes, epoxidation of styrene and subsequent cycloaddition of CO2 to the epoxide formed. In the present work, it is shown that a catalyst system of ZnBr2 and n-Bu4NX(X=Br,I) has an excellent activity and selectivity for the cycloaddtion of CO2 to styrene oxide. At the n-Bu4NI/ZnBr2 molar ratio of 2, styrene oxide is quantitatively transformed to styrene carbonate with in a very short time(30 min). This catalyst system can be also applied for the oxidative carboxylation of styrene by combining with an epoxidation catalyst of Au/SiO2. Under the mild reaction conditions(80 ℃, 4 h, CO2 pressure 1 MPa), styrene carbonate was obtained in a yield of 42% without any organic solvent. In separate runs, it was found that Au/SiO2 is active for the epoxidation of styrene, and ZnBr2 and n-Bu4NBr cooperatively catalyze the subsequent CO2 cycloaddition to epoxide. The styrene carbonate yield obtained in the present study is the highest among those reported, but it is not still satisfactory for practical application.
    Structural Parameters for Hydrogen Bonding Networks Formed in Systems of Aa1Dd1-Aa2Dd2 Type
    JI Yuan-Yuan1, WANG Hai-Jun1,2, LI Yuan-Feng3
    2007, 28(3):  506-509.  doi:
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    Structural parameters of hydrogen bonded network formed in a model system of hydrogen bonding solutions were studied on the basis of the sol-gel partition theory. With the proposed method, the gelation condition, the theoretical and numerical results of these structural parameters were presented in the cases that there exist the activity differences between the proton-donors and proton-accepters. It is shown that the activity difference can give rise to influence on the hydrogen bonded networks. This provides a possible theoretical clue to control the hydrogen bonded networks.
    E.coli Microbial Fuel Cell Using New Methylene Blue as Electron Mediator
    ZOU Yong-Jin, SUN Li-Xian, XU Fen, YANG Li-Ni
    2007, 28(3):  510-513.  doi:
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    A microbial fuel cell was constructed by using new methylene blue as the electron mediator and E.coli as the biocatalyst. The open circuit voltage of the MFC is 0.760 V and the short circuit current is 1.108 mA. The maximum power output is 116 mW/m2 with the corresponding current density 390 mA/m2. The performances of MFCs which use neutral red or new methylene blue as the electron mediator were also compared. The results show that the MFC which uses new methylene blue as the electron mediator has a lower open circuit voltage and higher steady short circuit current than those MFC which use neutral red as electron mediator. When the discharge current density is larger than 114 mA/cm2, the former has a higher power density and better stability than the latter.
    Photoelectrochemical Study of Poly(3-methylthiophere) Modified Q-PbS Anchored Nanostructured TiO2 Film
    HAO Yan-Zhong, WANG Wei
    2007, 28(3):  514-517.  doi:
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    The PbS quantum dots(Q-PbS) were formed in situ on a nanocrystalline TiO2 electrode by using chemical bath deposition techniques and the PMeT were prepared with electrochemical method on TiO2/Q-PbS film. The photoelectrochemical properties of TiO2/Q-PbS film and poly(3-methylthiophere)(PMeT) modified Q-PbS anchored nanostructured TiO2 film were studied by using the photocurrent action spectra and the photocurrent dependence of potential. The bandgap of Q-PbS films was 1.68 eV. The energy level of Q-PbS film was determined with photoelectrochemical method. The results indicate that PMeT and Q-PbS respectively modified TiO2 film and PMeT modified Q-PbS anchored nanostructured TiO2 film produced photocurrent in the longer wavelength region under a certain condition. In infrared light region, the conversion efficiency of light to electricity for the composite semiconductor nanoporous films was greatly improved comparing with that of the nanostructured TiO2.The experiment result shows that the p-n heterojuction existed in the nanostructure TiO2/Q-PbS/PMeT film electrode, which resulted in the separation of electron/hole pairs generated by photoexcitation, thus photoelectric conversion performance was improved.
    Molecular Dynamics Simulation and Experiment Measurement of Infinite Dilute Diffusion Coefficients of Methanol and Ethanol in Supercritical CO2
    SHI Jian, ZHANG Min-Hua, DONG Xiu-Qin
    2007, 28(3):  518-521.  doi:
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    A new approach to represent the infinite dilute diffusion coefficients of organic compounds in supercritical carbon dioxide was proposed. The infinite dilute diffusion coefficients of methanol and ethanol in supercritical CO2 were investigated by molecular dynamics(MD) simulation. In order to compare the simulation results, according to Taylor dispersion principles, the infinite dilute coefficients of methanol and ethanol were determined by Supercritical Chromatography. As Taylor dispersion method was easily to reach to supercritical condition, it was suit for the calculation of supercritical diffusion coefficients. In this work, the results of the MD simulation of the infinite dilute diffusion coefficients of methanol and ethanol behaved good accordance with the experiment and literature data. This new method can be used to predict the diffusion property of supercritical systems effectively and be employed for engineering design conveniently. Therefore, as an advanced research means, molecular dynamics simulation will be used more widely.
    Fabrication of Au Tips for Tip-enhanced Raman Spectroscopy
    WANG Xi, CUI Yan, REN Bin
    2007, 28(3):  522-525.  doi:
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    Tip-enhanced Raman spectroscopy is a newly developed technique that can provide a very high sensitivity and spatial resolution. It requires tips with a very sharp apex and smooth surface free of any contamination to provide the necessary enhancement effect. Au tips with a smooth surface and a radius ranging from 10—30 nm were fabricated by electrochemical etching of Au wires at a constant potential in a mixture of fuming HCl and absolute ethanol with a volume ratio of 1:1. The ending point was monitored by a feeback control with a preset etching current smaller than the base current. The influence of the etching voltage on the sharpness and surface structure of the tips were systematically investigated and it was found that Au tips with a high quality could be obtained at an etching voltage of 2.2 V versus Au wire. By comparing the current-time curves of the etching process and the SEM images of each individual tip, we found that the current-time curves recorded during the etching process could be effectively used to evaluate the possible quality of tips. A curve with a good periodicity at the ending point of etching process results in a tip with a good shape and sharp apex. As a consequence, it is not necessary to use SEM to characterize the tips in the future preparation of tips, which will not only improve the efficiency during the experiments but also avoid to a large extent any possible contamination. The quality of the tip was demonstrated by getting STM image of the terrace on a HOPG surface. The obtained Au tip can also be used as micro-(nano-)electrodes and the electromagnetic field enhancer in tip-enhanced spectroscopy.
    Role of Threonine on Antifreeze Activity of Insect Antifreeze Protein
    ZHOU Yan-Xia1, ZHANG Yong1, TAN Hong-Wei1, JIA Zong-Chao2, CHEN Guang-Ju1
    2007, 28(3):  526-529.  doi:
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    A series of mutants of the insect antifreeze protein(CfAFP) were designed, their best ice-binding modes were generated by using molecular dynamic simulations, and the interaction energy with ice was computed by semi-empirical molecular orbital methods AM1 and PM3. The results show that the contribution to the CfAFP-ice interaction of the threonine residues depends on the position and number in CfAFP, and Thr residues in TXT-motif play key roles on the recognition and binding of CfAFP and ice. Replacement of thr by other kinds of hydrophilic or hydrophobic amino residues reduced the interaction with ice, resulting in a moderate loss of antifreeze activity. Additionally, based on the structure complement of CfAFP and ice, increasing the size of hydrophobic residues could gain more stable interaction with ice and enhance the antifreeze activity.
    Synthesis of MCM-36 Molecular Seive and Studies on Catalytic Performance of MCM-36 on Benzene Alkylation with Propylene
    ZHANG Yu1,2, XING Hai-Jun1, WU Shu-Jie1, WU Peng1, YANG Piao-Ping1, JIA Ming-Jun1, WU Tong-Hao1, SUN Chia-Chung3
    2007, 28(3):  530-534.  doi:
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    Pillared layered MCM-36 zeolites were prepared from MCM-22 and MCM-49 precursors with polymeric silica as the pillaring agent, respectively. The structure and acid properties of samples were studied by means of N2 adsorption, XRD, and FTIR. A higher BET specific surface area and a significant mesopore volume is obtained for MCM-36(A). The amount of Brnsted and Lewis acid sites in MCM-36(A) decreases obviously compared to MCM-22 resulting from the same precursor. For MCM-36(B) synthesized from MCM-49 precursor, the intensity of low angle XRD peak is lower than that of MCM-36(A), and the amount of acid sites decreases moderately compared to MCM-49. Under our operation conditions, the MCM-36(A) zeolite shows a higher activity and selectivity to cumene than MCM-22 zeolite. MCM-36(B) exhibits a higher activity but lower selectivity to cumene compared to MCM-36(A). Combined with the characterization results of acidic properties and textural parameters, we suppose that the increase of the selectivity to cumene in MCM-36 should be mainly due to the decrease of the density of Brnsted acidity, while the improvement of the catalytic activity of MCM-36 can be mainly assigned to the presence of a larger amount of structurally accessible acid sites in this material.
    Structures and Stabilities for CoGe-n(n=1—12) Alloy Clusters
    CHEN Jian-Cheng, XING Xiao-Peng, TANG Zi-Chao, GAO Zhen
    2007, 28(3):  535-538.  doi:
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    The electronic affinity energies, EA values, geometric and electronic structures of CoGe-n(n=1~12) clusters are studied experimentally and theoretically. The EA values measured by a photoelectron spectroscopy agree with the computational ones for CoGe-8, CoGe-9 and CoGe-10. From the PDOS, the interactions of p, d and s electrons were analyzed. The stability of CoGe-n was discussed and CoGe-10 was considered as a cluster with magic number.
    QSAR Studies on Herbicidal Activities of Sulfonylurea Compounds
    LI Ji-Lai1, HANG Ye-Chao2, GENG Cai-Yun1, HUANG Xu-Ri1, LI Fang-Shi2, SUN Chia-Chung1
    2007, 28(3):  539-542.  doi:
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    Using the density functional theory method, the theoretical quantum chemical descriptors of twenty-three sulfonylurea compounds were calculated at B3LYP/6-31G(d) theoretical level. Described by the descriptors from eighteen compounds and optimized by multiple regression, a new QSAR model was established to correlate the herbicidal activity(R=0.96, r2adj=0.88, F=26.26, q2=0.71, p<0.01, SE=0.36). To obtain new products with a higher herbicidal activity, it is suggested that it is feasible to increase the electron density of the 13th nitrogen atom and to increase the hydrophilicity of the substituents in benzene and pyrimidine. Those predictions are in good agreement with the results obtained from 3D-QSAR method. The present study may be helpful for probing the mechanism of herbicidal activities and understanding the herbicidal chemistry in-depth study in the future.
    Interaction and CoMFA Studies on A. thaliana Acetohydroxyacid Synthase by Sulfonylureas
    BAN Shu-Rong, NIU Cong-Wei, CHEN Wen-Bin, REN Xiao-Bai, YU Zhi-Hong, XI Zhen
    2007, 28(3):  543-547.  doi:
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    Acetohydroxyacid synthase(AHAS) is the target for sulfonylurea, imidazolinone, triazolopymiding sulfonaniline and pyrimidin-2-yl salicylate herbicides. The interactions between wild type A. thaliana Acetohydroxyacid synthase(AHAS) and 85 synthesized sulfonylureas in vitro were studied, obtained Kiapp values of all compounds by the method of Westerfeld and Singh. The structure-activity relationship and 3D-QSAR was investigated by using comparative molecular fields analysis(CoMFA). The cross-validated q2 and the relation coefficient r2 for the model established by the study are 0.811 and 0.934 respectively, with a F value of 246.506 and a standard deviation(s) of 0.419. The obtained satisfied QSAR model was is consistent with those based on in vivo data and showed a high ability to predict the biological activity(-lgKiapp) for ten test set compounds. These results will be useful for design and synthesis of highly active compounds.
    Dissipative Particle Dynamics Study on Morphology Changes of Cyclic Diblock Copolymer Microphase Under Shear
    LIU Wei, QIAN Hu-Jun, LÜ Zhong-Y
    2007, 28(3):  548-551.  doi:
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    The morphology changes of cyclic diblock polymer microphases under simple shear were studied via DPD technique. For LAM, parallel reorientation and parallel-perpendicular orientation transition phenomena were reproduced. Moreover, the undulation instability was observed. For PL, PL-HEX transition occurs under a strong shear. For HEX, parallel reorientation was identified. A two stage reorientation mechanism involving break-up and phase reformation was proposed to describe the reorientation process for both LAM and HEX, and the PL-HEX transition. For BCC phase, shear-induced melting was found.
    Molecular Dynamics Simulation of Storage Hydrogen in Hydrate
    LI Xiao-Sen
    2007, 28(3):  552-555.  doi:
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    The structures of hydrogen hydrates with structure Ⅰ(SⅠ) and structure H(SH), are studied systematically with molecular dynamics simulation, and the stable structures of hydrogen hydrates are obtained. The structures shows the occupation of hydrogen: there are two H2 molecules in a small cage and three H2 molecules in a big cage in SⅠ hydrate; there are two H2 molecules in a small cage, two H2 molecules in a middle cage, eleven H2 molecules in a big cage in SH hydrate. The radial distribution function(RDF) for hydrogen-hydrogen in each cage of hydrogen hydrate is also investigated. Furthermore, the stable positions of hydrogen in each cage are determined. With these stable positions, the hydrogen storage capability of the hydrate is 5.085%(mass fraction) for SⅠ and 6.467%(mass fraction) for SH. Compared to experiment, it is found that the hydrogen storage capacity of the SH hydrate with the stable structure is most excellent.
    研究快报
    Studies on the 4-Amino-dimethyl-aniline Hydrochloride Degraded by a Bio-electro Reactor
    KANG Bo1,2, HUANG Wei-Min1,2, ZHANG Ying-Jiu3, ZHANG Xue-Na1,2, LIN Hai-Bo1,2
    2007, 28(3):  556-558.  doi:
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    4-Amino-dimethyl-aniline hydrochloride is one of the main components of the wastewater from vanillin production plant. So it is used for the target contamination to be degraded by microorganism, electrochemical oxidation and bio-electro reactor in this paper. We found out a economical, efficient and non-polluted methods for the treatment of wastewater from vanillin production plant. The results indicate that there are a lot of special microbes and bacteria eating 4-amino-dimethyl-aniline hydrochloride in the activated sludge after 20 days' incubation, at the same time, a stable bio-filmed electrode was formed. Under the condition of 25 ℃, pH=6—7. The use of bio-electro reactor not only increased the biodegradability and decreased the electrical energy consumption, but also solved the problem which the second pollution of organic compounds containing chlorine in the process of indirect electrochemical degradation on the organic pollutants.
    研究简报
    Effect of Cerium/Zirconium Molar Ratio on the Property of Series OSM Ce0.3+xZr0.6-xY0.1O1.95
    MAO Xiao-Bo, CHEN Yao-Qiang, ZHONG Jun-Bo, WANG Jian-Li, ZHAO Ming, GONG Mao-Chu
    2007, 28(3):  559-561.  doi:
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    A series of materials Ce0.3+xZr0.6-xY0.1O1.95 were prepared by co-precipitation routine and the property of these materials was studied by means of oxygen storage capacity, temperature programming reduction, X-ray diffraction, transmission electronic microscope, and X-ray photoelectron spectroscopy. The results indicate that the materials with a low Ce/Zr molar ratio possess higher cerium atom utilization ratio, reducibility and thermal stability than the materials with a high Ce/Zr ratio, and Ce0.35Zr0.55Y0.1O1.95 possesses the best properties.
    Size Effect of Conductivities of Polyaniline Nanowires
    QI Li, ZHOU Jian-Zhang, WENG Shao-Huang, CAI Cheng-Dong, YAO Guang-Hua, LIN Zhong-Hua
    2007, 28(3):  562-564.  doi:
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    The study of size effect of conductivity of conducting polymer nanowires can be significant not only in the instruction of fabrication of the devices with nanodimension but also in basic research of inherence of nanomaterials. PANI nanowires was fabricated in AAO templates by potentiostatic method. A new strategy of chemical modification of AAO template was introduced to prepare nanowires with smaller diameter. FTIR and contact angle measurements were used to characterize the modification. Tunneling Electron Microscopy results showed that the smaller PANI nanowires in diameter can be obtained in surfactant modified AAO templates. Conductivity of single PANI nanowire had been measured by Conductive Atomic Force Microscopy. The results displayed that the conductivity of PANI nanowire increase while the decrease of the diameter of PANI nanowires, which was called size effect of conductivity of PANI nanowires. The size effect had been attributed to order polymer chains orientation of PANI nanowire, which had been confirmed by electron diffraction diagrams.
    Influence of Ultrasonic Wave-activating Treatment on Structure and Oxidation Reactivity of Microcrystalline Cellulose
    WANG Xian-Ling, FANG Gui-Zhen, HU Chun-Ping
    2007, 28(3):  565-567.  doi:
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    Microcrystalline cellulose(MCC) was activated with ultrasonic wave. The changes in supramolecular structure and morphology structure of MCC were studied by XRD and SEM. The influence of ultrasonic treatment on accessibility and oxidation reactivity of MCC with periodate sodium was investigated. The mechanism of the change of reactivity after ultrasonic treatment was discussed. The results showed that crystalline type of cellulose was not changed and no significant changes in crystalline size of cellulose were observed. However, after treatment with ultrasonic wave the crystallinity of cellulose decreased and morphology changes of the treated MCC was significant. These changes contributed to the increase of specific surface area and WRV, which implied the increase of accessibility. The reactivity of MCC with periodate sodium was successfully improved after ultrasonic treatment. The aldehyde content of its oxidized products dialdehyde cellulose(DAC) was improved from 71.3% to 85.0%. As the increase of ultrasonic treating time the aldehyde content first increased and then decreased.
    Preparation and Characterization of Large-area Superhydrophobic Nanostructured Carbon Films
    ZHANG Ya-Nan1,2, XIA Fan3, WANG Nü3, FENG Lin1
    2007, 28(3):  568-570.  doi:
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    Large-scale carbon films were prepared using a simple pyrolysis method, on which nanostructured loose pores can be found by SEM observation. The as-prepared carbon films are superhydrophobic after the modification of low-surface-energy material fluoroalkylsilane, with the water contact angle of 162.3°±2.1°. XPS measurement indicates that the films were hydrophobilized. It's considered that nanostructures are important to the superhydrophobicity since air exist beneath water and the contact area between water and carbon film decrease. Such superhysrophobic carbon films can be widely applied in many fields.
    研究论文
    Structure and Properties of Polystyrene-encapsulated Multi-walled Carbon Nanotubes Composites Prepared Through Ultrasonically Initiated in situ Emulsion Polymerization

    WANG Zhang-Yu, WANG Qi, CHEN Ying-Hong, XIA He-Sheng

    2007, 28(3):  571-574.  doi:
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    Polystyrene-encapsulated multi-walled carbon nanotubes(MWNTs) composites were prepared by ultrasonically initiated in situ emulsion polymerization. The structure and properties of the obtained composites were investigated by TEM, FTIR, UV, XPS and GPC etc.. The results show that the in situ formed PS layers were encapsulated on the surface of MWNTs and there were strong interactions between them. Element oxygen was found to be introduced onto the surface of MWNTs during the polymerization process. Meanwhile, MWNTs also consumed the macromolecular free radicals generated nearby, leading to the transfer of PS macromolecular chains onto the surface of MWNTs and the termination of polymerization process. As a result, the relatively lower molecular weight and broader molecular weight distribution of the formed PS occurred in the obtained composites. TGA analyses proved that the thermal properties of the PS/MWNTs composites were greatly improved.
    Investigation on the Rheological Characteristics and Interactions of PVP-LiCl-DMF Solution System
    HAO Chao-Wei1,3, ZHAO Ying1, ZHOU Yong1,3, ZHOU Li-Juan1,3, XU Yi-Zhuang2, WANG Du-Jin1, XU Duan-Fu1
    2007, 28(3):  575-579.  doi:
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    The interaction between poly(vinyl pyrrolidone)(PVP) and lithium chloride was studied by rheological method, 13C NMR and FTIR spectroscopy. The results showed that the apparent viscosity, the activation energy and the critical shear thinning rate of the concentrated PVP-LiCl-DMF solution are obviously influenced by lithium chloride. The apparent viscosity increases with the increasing of the content of the lithium chloride, and the activation energy of the solution increases as well, while the critical shear thinning rate decreases with increasing the content of lithium chloride. 13C NMR spectra proved the interaction between Li+ ion and the carbonyl group from PVP and DMF molecules in PVP/LiCl/DMF solution. These results indicate that the obvious interactions between Li+ ion and PVP in the solution result in the variation of the aggregation state of PVP molecules. The IR spectra of the PVP/LiCl composites showed that there are interactions between Li+ ion and carbonyl group in the lactam of PVP unit, and the curve fitting results also indicated the existence of several coordination structure between Li+ ion and carbonyl groups.
    New Method of Preparing Chloromethylated Crosslinking Polystyrene Microspheres
    SHEN Yan-Ling, YANG Yun-Feng, GAO Bao-Jiao, LI Gang
    2007, 28(3):  580-583.  doi:
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    The chloromethylation reaction of crosslinking polystyrene microspheres(white-sphere) was performed at room temperature by using self-made chloromethylation reagent, 1,4-bis(chloromethoxy)butane(BCMB), as the chloromethylation reagent and adopting Lewis acid catalysts, and the chloromethylated crosslinking polystyrene microspheres(chloro-sphere) with a chlorine content of 17% was obtained. The chemical structure and composition of the product were characterized by FTIR and Volhard methods, and the effects of various factors on the chloromethylation reaction were mainly examined. Various factors not only affect the chloromethylation degree of the white sphere, but also inhibit or accelerate the Friedel-Crafts crosslinking reaction between macromolecular chains and affect the strength of the chloro-sphere.
    Synthesis and Properties of a Novel Red Electroluminescent Conjugated Polymer Containg Naphthothiadiazole
    HUANG Zhe, ZHANG Yong, ZENG Wen-Jin, XU Wei, YANG Jian, PENG Jun-Biao, CAO Yong
    2007, 28(3):  584-587.  doi:
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    A series of aminoalkyl-substituted polyfluorene copolymers with 4,7-dithien-2-yl-2,1,3- naphtho-thiadiazole(SNS) with different contents were synthesized by Suzuki coupling reaction. The polymers are soluble in organic solvent, such as chloroform, toluene. All the polymers emit red light (more than 700 nm) under UV excitation in the solid state. It was found that the PFN-SNS polymers show a good device performance when high work-function metals, such as Al, are used as the electron-injection cathode replacing conventional low work-function cathodes such as Ca and Ba. The maximum external quantum efficiency is more than 1.3% with Al as cathode.
    Synthesis and Characterization of Poly(phthalazinone ether)s Containing Cyano Groups
    CHEN He-Guo, WANG Shuan-Jin, XIAO Min, MENG Yue-Zhong
    2007, 28(3):  588-591.  doi:
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    Three kinds of cyano-containing poly(phthalazinone ether)s with high molecular weights were successfully prepared from bisphthalazinone containing cyano groups and different activated dihalide monomers via a N—C coupling reaction. The properties of these polymers were determined by TGA, DSC, GPC, viscosity and solubility tests. TGA results demonstrate that all polymers exhibited an excellent thermal stability with 5% mass loss at T>492 ℃. Poly(phthalazinone ether)s had very high glass transition temperatures(Tg) ranging from 263 to 320 ℃ due to their rigid bisphthalazinone structure. All polymers were soluble in chloroform and polar aprotic solvents such as N,N-dimethylacetamide(DMAc), N,N-dimethylformamide(DMF), N-methyl-2-pyrrolidinone(NMP).
    Studies on Epoxy Resin/Montmorillonite Nanocomposites Cured with 4,4'-Diamino Diphenyl Ether Diphenyl Ketone
    CUI Ji-Wen1,2, YU Lian-Xiang1, ZHANG Chun-Ling3, MI Xin-Yan1, FU Tie-Zhu1, NA Hui1
    2007, 28(3):  592-595.  doi:
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    Ca-montmorillonite was directly modified by ion-exchang method using hexadecyl trimethyl ammonium bromide. The interlamellar spacing of the montmorillonite, corresponding to the(001) plane peak, increases from 1.49 nm for the purified MMT to 2.21 nm for the organophilic clay(C16-MMT). The epoxy resin/BADK/MMT nanocomposites were prepared. The effects of content of montmorillonite and mixing conditions including mixing temperatures and mixing time on the intercalation and exfoliation behavior of epoxy/alkylammonium-montmorillonite nanocomposites after curing with curing agent(BADK) were investigated by X-ray diffraction(XRD). The X-ray patterns reveal that organoclay was intercalated by the epoxy resin during mixing process. When E51 was cured with equimolar amounts of BADK, either an intercalated or an exfoliated nanocomposites were obtained. Only under certain mixing conditions, the exfoliation nanocomposite materials could be formed.
    Preparation and Properties of Solar Cell from CdSe Nanocrystals and Conjugated Polymer Composites
    LIU Yan-Shan, WANG Li, CAO Yong
    2007, 28(3):  596-599.  doi:
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    CdSe nanospheres(ns-CdSe) with diameters of 5 nm were prepared through an organometallic method at a relatively low temperature, by using cadmium stearate as the precursor and oleic acid as the surfactant. The TEM, UV-Vis absorption and PL spectra indicate that the CdSe nanocrystals were monodispersed nanospheres with the first exciton absorption peak at around 625 nm and the emission peak at around 652 nm. The ns-CdSe can be readily dispersed in organic solvent and form a homogeneous blend with conjugated polymers. The PL spectra of the ns-CdSe/polymer composite films show that the photoluminescence of the conjugated polymers are effectively quenched upon the addition of ns-CdSe. Solar cell were fabricated from the composites of ns-CdSe and conjugated polymers(MEH-PPV or P3HT). Under AM1.5 illumination(100 mW/cm2), the ISC, VOC, FF and η reached 1.56 mA/cm2, 0.75 V, 34.5% and 0.40% for the device from the ns-CdSe/MEH-PPV(15∶1 mass ratio) and 1.93 mA/cm2, 0.65 V, 38.4% and 0.48% for the device from the ns-CdSe/P3HT(10∶1 mass ratio) respectively.
    研究快报
    Synthesis and Properties of a Novel Crosslinkable Poly(aryl ether ketone) Containing Pendent Phenylethynyl Moieties
    MA Xiao-Ye, GUAN Shao-Wei, CHEN Chun-Hai, WANG Gui-Bin, JIANG Zhen-Hua
    2007, 28(3):  600-602.  doi:
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    A type of novel crosslinkable poly(aryl ether ketone)s containing pendent phenylethynyl moieties(PEP-PAEK-Fn) were synthesized. The polymers were prepared by copolycondensation reaction of difluoro-monomer with potassium salt of 4-phenylethynylphenyl hydroquinone(PEP-PH) and 4,4'-isopropylidenediphenol(BPA). The Mns and Mw/Mns of polymers determined by GPC with polystyrene standard were 46700, 100000 and 1.6, respectively. The resulting polymers were thermally crosslinked at 370 ℃ for 2 h in N2 atmosphere. The glass transition temperature is increased after crosslinking. The cured polymers show a good chemical resistance and high thermal stability up to 500 ℃ under nitrogen.
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