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Table of Content

    31 December 2001, Volume 22 Issue S1
    Articles
    Preparation of Nano-Particle Pd/γ-Al2O3 Catalysts for Low-Temperature CO Oxidation by Solyated Metal Atom Impregnation Method
    Yang Xiu-Lin, Huang Wei-Ping, Zhang Shou-Min, Zheng Xiu-Cheng, Li Bao-Qing, Wu Shi-Hua
    2001, 22(S1):  1-4. 
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    Nano-particle Pd/γ-Al2O3 catalysts with different Pd content were prepared by solvated metal atom impregnation technique. The results of XRD and Chemisorption measurement showed that as the metal content increased the particle size of Palladium increased; but the diameter of Pd particles in all the Pd/γ-Al2O3 catalysts studied was in the range of 2.0-6.0nm. XPS study indicated that Paiiadium was in metallic slate. The Pd/γ-Al2O3 catalysts exhibited higher activity for CO oxidation at lower temperature. 100% CO conversion was achieved at 453K. As the particle size of Palladium increased the catalytic activity increased. The Pd/γ-Al2O3 catalyst with Pd panicle size of 2. Inm showed the highest activity.

    Synthesis, Crystal Structure and Quantum Chemistry Calculation of 2-(2-benzimidazlyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazolyl-3-oxide-1-oxy
    LIU Zhi-Liang, ZHAO Bin, JIANG Zong-Hui, YAN Shi-Ping
    2001, 22(S1):  5-8. 
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    The present paper describes the synthesis and crystal structure of 2-(2-benzimidazlyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazolyl-3-oxide-1-oxy (NITBzImH). The crystal structure was determined by X-ray single crystal diffraction technique. The crystal belongs to orthohombic system with space group Pbca. The unit cell parameter are:a=0.87446(4), b=1.55600(8), c=2.01139(1)nm, a=β=γ=90°,Z=8, V=2.7368(2)nm3, R=0.0478, wR=0.1101. The spin density distribution has been calculated by DFT method. It is confirmed that the spin density mainly distributes to N-O and of the radical.

    A New Technique for Preparation of the Cathode Material of Lithium-ion Battery
    WEI Jin-Ping, DENG Bin, YAN Jie, ZHOU Zhen, SONG De-Ying
    2001, 22(S1):  9-12. 
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    The cathode material LiCoO2 of lithium-ion batteries can be obtained from the reaction of LiOH·H2O and Co(OH)2-2xRx(R is the inorganic or organic acid radicals), which is the midst product of the electrolysis of the metal cobalt in a given electrolyte. The achieved cathode material LiCoO2 for lithium-ion batteries has a single phase and its granularity distribution relatively concentrates through the experiments of XRD. SEM and Laser Granularity Testing, The discharge capacity is relatively high which reaches 146mAh/g at the first time of discharging and still maintains 142mAh/g after 10 cycles of charge/discharge experiments. The cost for the preparation of the cathode material LiCoO2 can greatly be decreased through this technique, which has a well-promising application future.

    The Effects of Various Factors in Orthogonal Table on Charging Efficiency of Iron Electrode
    LIN Dong-Feng, CHEN Shuang-Rui, CAI Rong, SONG De-Ying, SHEN Pan-Wen
    2001, 22(S1):  13-15. 
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    High theoretical specific energy, rich raw material, cheap price and environmental protection are specific advantages of rechargeable Fe-Ni battery. It has a wonderful perspective for application. The advantages,disadvantages of Fe-Ni cells, and the preparation of iron electrode were summarized in this paper The effects of different factors, particularly additives in electrolyte solution, on the charge efficiency of iron electrode were discussed by means of orthogonal experiments in this paper. The chaise efficiency of iron electrode has been improved to 80% from 30%~60%, which will help to realize the seal of Ni-Fe cells.

    Study on Electrochemical Behavior of the Positive Electrode Mg1.2Mn1.8O4 in Magnesium Ion Battery
    YUAN Hua-Tang, CAO Jian-Sheng, WANG Yi-Jing, ZHOU Yong, Wu Xu-Li, LIU Jing-Wang
    2001, 22(S1):  16-18. 
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    Mg1.2Mn1.8O4 with structure of spinel was synthesized by the method of solid synthesis under high temperature and was studied by X-ray diffraction (XRD) and scanning electron microscope (SEM). The behavior of magnesium ion intercalation in nonaqueous organic electrolyte was studied by means of charge experiments and electrochemical impedance spectra (EIS). The results showed that the performance of magnesium ion intercalating is similar with that of lithium and the electrochemical process is mix controlled.

    Study on Characteristic of Novel Type Co-free Zn-containing MmxMl1-x(NiCuAlZn)5 Hydrogen Storage
    WANG Yi-Jing, YUAN Hua-Tang, CAO Jian-Sheng, LI Qiu-Di, SONG He-Nan, WANG Gen-Shi
    2001, 22(S1):  19-21. 
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    The influences of Mm on the characteristics of the MmxMl1-xNi4.14Cu0.5Al0.3Zn0.06 hydrogen storage alloys were investigated. With the increasing of the content of the the volume of unit decreases, the plateau pressure increases. When x=0.2, the alloy shows promising characteristics.

    The AgClO4 Complex of Bis(phenylthiol)ethane Forming Unique Clover-like Structure with (6,3) Net
    CHEN Wei, LI Jian-Rong, WANG Wen-Zhen, BU Xian-He, ZHANG Ruo-Hua, CHEN Rong-Ti
    2001, 22(S1):  22-24. 
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    The synthesis and characterization of the AgClO4 complex with bis(phenylthiol)ethane, [Ag(C14H14S2)1.5ClO4]n, has been reported. In the title complex, the Ag(Ⅰ) ions were bridged by the bpte ligands forming a unique clover-like Ag6L6 repeating units which fused into a two-dimensional (6,3) net.

    Synthesis and Hydrongen-bonded One-dimensional Structure of Novel Trinuclear Cu-Co-Cu Complex Incorporating Macrocyclic Oxamides
    TANG Jin-Kui, SI Shu-Feng, LIU Xin, LIAO Dai-Zheng, WANG Geng-Lin
    2001, 22(S1):  25-28. 
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    A novel oxamidato-bridged Cu-Co-Cu trinuclear complex incorporating macrocyclic oxamide (macrocyclic oxamide=l,4,8,11-tetraazacyclotradecanne-2,3-dione),has been prepared and spectroscopically, structurally characterized. The complex crystallizes in monoclinic space group P2(l)/c, with a=0.771 72(4) nm, b=1.531 30(3) nm, c=1.472 98(7) nm, β=98.540(2)°, V=1.72137(13) nm3, Z=2,R=0.0843. The structure consists of trinuclear units and free water molecules and hydorgen bonds involving water molecules interlink the trinuclear units to form a unique one-dimensional chain.

    Synthesis, Structure and Properties of Copper(Ⅱ) Complex with Pyrazole Ligands and Thiocyanate
    SUN Ying-Ji, ZHAO Bin, SHI Wei, CHENG Peng, YAN Shi-Ping, SHEN Pan-Wen
    2001, 22(S1):  29-32. 
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    This paper presents the synthesis, crystal structure and properties of copper(Ⅱ) complex[Cu(pz)4(NCS)2](pz=pyrazole). The complex was crystallized in the monoclinic system, space group C2/c, a=1.1520(4) nm, b=1.2247(4) nm, c=1.4188(5) nm, β=106.747(8)°, Z=4, R1=0.0554,wR2=0.1420. The Cu(Ⅱ) ion is in 4+2 environment with an elongated-octahedron geometry. The basal plane of the central copper atom is formed by the four pyrazole nitrogen atoms and the apical positions are occupied by two nitrogen atoms of two NCS- anions. IR, UV-Vis and ESR spectra were also measured and the results are well consistent with the crystal structure.

    Electrochemical Properties of Composite Hydrogen Storage Materials of Carbon Nanotubes and Mm(Ni-Co-Al-Mn)5
    GAO Xue-Ping, QIN Xue, WU Feng, SONG De-Ying, ZHOU Zuo-Xiang, SHEN Pan-Wen
    2001, 22(S1):  33-36. 
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    The composite hydrogen storage materials of carbon nantube-MmNi3.6Co0.7Al0.3Mn0.4 were synthesized firstly by ball milling method under different conditions. The electrochemical properties of carbon nantube-MmNi3.6Co0.7Al0.3Mn0.4 have been investigated in this paper. The discharge capacities of the carbon nantube-MmNi3.6Co0.7Al0.3Mn0.4and MmNi3.6Co0.7Al0.3Mn0.4 electrodes were measured to be 320 and 270mAh/g, respectively, under a current density of 250mA/g. The electrochemical properties of carbon nantube-MmNi3.6Co0.7Al0.3Mn0.4 electrode have been studied by cyclic voltammetry. It shows that the composites of carbon nantube & MmNi3.6Co0.7Al0.3Mn0.4 accelerate hydrogen adsorption.

    Simultaneous Determination of Inorganic Anions and Cations in Cosmetics by Capillary Zone Electrophoresis
    WANG Zong-Hua, YAN Liu-Shui, LUO Guo-An
    2001, 22(S1):  37-41. 
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    For thousands of years the extraordinary waters of the Dead Sea have healed and rejuvenated skin because of their unique mineral content. Natural Sea Beauty products use the power of these Dead Sea minerals. The capillary electrophoresis technique based on the electromigrative sample introduction from both ends of the capillary was applied for the simultaneous determination of inorganic anions and cations in the cosmetics of Natural Sea Beauty products. The optimized separations were carried out in 5 mmol/L imidazole and 2 mmol/L nitrate electrolyte neutralized with fumaric acid to pH 4.1, using indirect UV detection at 214 nm. Six inorganic ions (K+、Na+、Ca2+、Mg2+、Cl-、Br-) were well separated in less than 6 min. The comparison of the results with ion chromatography is presented. This method is one of ways used to test different produces.

    Enantioseparation of Chiral Drugs by Cyclodextrin-Mediated Capillary Zone Electrophoresis
    ZHANG Zhi-Chao, ZHANG Kai, JIANG Zheng-Jin, ZHOU Qi-lin, WANG Qin-Sunt, GAO Ru-Yu
    2001, 22(S1):  42-44. 
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    The effects of the cyclodextrin (CD) type on the enantioseparation of six chiral drugs were investigated, using 2 natural CD, namely β-CD and γ-CD, 2 commonly used uncharged functionalized CD, namely hydroxypropylated β-CD (HP-β-CD) and dimethylated β-CD (DM-β-CD), and 3 newly-developed charged CD, namely highly sulfated α-CD (HS-α-CD), highly sulfated β-CD (HS-β-CD), highly sulfated γ-CD (HS-γ-CD) as capillary zone electrophoresis additive, respectively. While the 2 natural CD showed no enantioselectivity of the 6 chiral drugs, the functionalized CD's enantioselectivity improved greatly. In particular, the HS-β-CD could baseline chirally resolved the enantiomers of all the 6 chiral drugs, indicating that the HS-β-CD is a versatile chiral selector and is worth developing further. The effects of the pH of the background electrolyte and the organic modifier on the enantioseparation were also examined and disscussed.

    Evaluation of Polymer Encapsulated-TiO2 Stationary Phase and Comparison to Related Phases Using Linear Solvation Energy Relationships
    LEI Rong, XING Yu-Jie, YANG Jun-Jiao, ZUO Yu-Min
    2001, 22(S1):  45-49. 
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    The retention behaviors of poly(ethylstyrene-divinylbenzene) encapsulated-TiO2 (ES-DVB-TiO2) were studied by means of linear solvation energy relationships (LSERs). On the ES-DVB-TiO2 stationary phase, 21 kinds of compounds were tested in mobile phase of methanol and water. Good relationships between log k' (ES-DVB-TiO2) and LSERs parameters are obtained. Besides, we compared the retention characteristics of ES-DVB-TiO2,PBD-TiO2,ODS and PRP-1. According to percent variance, retention on ES-DVB-TiO2 synthesized in our laboratory is dominated by three major factors:the solute size (V2)、hydrogen bond donor acidity(Σα2H)、and the solute hydrogen bond acceptor basicity (Σβ2H). The results suggest that ES-DVB-TiO2 stationary phase exhibits a more adsorption-like retention mechanism under room temperature.

    Preparation and Evaluation of Long-Alkenylene-PBD Coating Zirconia-Based Stationary Phases
    YANG Jun-Jiao, WANG Hui, LEI Rong, ZUO Yu Min
    2001, 22(S1):  50-54. 
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    Novel reversed-phase packings (C8-PBD-ZrO2, C18-PBD-ZrO2) were prepared by depositing and cross-linking 1-octene(C8) or 1-octadecene(C18) and polybutadiene(PBD) onto th surface of porous zirconia microspheres which were synthesized by PICA (polymerization-induced colloid aggregation) method. The reaction conditions for the synthesis of these stationary phases were studied. The neutral and basic compounds were separated on these column packings.

    The Effect of Strong Electrolyte on Nonionic Microemulsion
    LUAN Rui, HAN En-Shan, ZHU Ling-Zhi, WANG Fu-Peng
    2001, 22(S1):  55-58. 
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    By determining the conductivity and the biggest water tolerance of microemulsion, we researched that strong electrolyte nickel nitrate had salt out effect on nonionic microemulsion Triton X-100/n-hexanol/cyclohexane/Ni(NO3)2 solution. We found that the more the content of surfactant, the higher the conductivity of microemulsion whose disperse phase is water. The conductivity of microemulsion whose disperse phase is Ni(NO3)2 solution reduces along with the concentration of Ni(NO3)2 solution increasing. We also found the higher the concentration of Ni3)2 solution,the less the water tolerance of microemulsion.

    A Review of the Toxic Effects of Al on the Biological Functions of Fe, Ca and Mg and Related Toxic Mechanisms
    ZHANG Fu-Ping, BI Shu-Ping, GAN Ning, LIU Jian, YANG Li
    2001, 22(S1):  59-62. 
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    Aluminum (Al) is not an essential element for human body. On the contrary, Fe,Ca, and Mg are required to mediate many normal metabolisms. However, because of the resemblance of both ionic diameters and ionic charges between Al and Fe, Ca, and Mg,Al expects to disturb the biological activities of its analogues. In this paper, the recent progresses of the studies of the toxic effects of Al on the biological functions of Fe, Ca and Mg have been reviewed. The corresponding mechanisms of the toxicogenic action of Al in these cases are also discussed. A typical toxicity of Al is resulted from its promotion of the ability of Fe to produce free radical or reactive oxidants that will lead to 'oxidative stress',one of the factors of the pathology of Alzhmers disease and Parkinson's disease. The substitutions of Fe and Ca for Al in some biological functional components will result in anemia and osteopathia respectively as well. In addition, fifty references have been cited.

    Study on the Anticancer Activity of Indigo Derivatives
    MENG Ji-Ben, LI Ping, HE Yong-Zhi, XU Li-Li, WANG Yong-Mei
    2001, 22(S1):  63-65. 
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    Thirteen compounds of indigo derivatives were synthesized, among which six compounds were first synthesized, The structure of all the new compounds have been comfirmed by 1H NMR, MS and elemental analysis. The relationship between the compound's structure and anticancer activity was studied. It was found that most of the indigo derivatives have the similar anticancer activity to indirubin, and some superior than indirubin.

    Synthesis and Structure of Nonsymmetric Tetraorganodistannoxane Dimers[ClR2SnOSnR'2Cl]2
    LÜ Yan, LAN Zhi-Li, LI Jing, XIE Qing-Lan
    2001, 22(S1):  66-70. 
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    Nonsymmetric Distannoxane Dimers [ClR2SnOSnR'2Cl]2 were synthesized by the reaction of R2SnO(R=Bu, Pr) and R'2SnCl2(R=Me, Pb, Cy, Oct). The crystal structure of compound 1 and 5 show they are ladder-type dimers that contain a central planar Sn2O2 four-membered ring. Both endo- and exo-Sn atoms are five-coordinate.

    Synthesis of New Chiral Phosphorus Compounds as Ligand Catalysts for Some Asymmetric Reactions
    ZHOU Zheng-Hong, YANG Zhuo-Hong, LI Kang-Ying, LIU Jian-Bing, TANG Chu-Chi
    2001, 22(S1):  71-76. 
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    Twenty-six chiral phosphorus compounds have been synthesized from L-aminoacids,D-camphor, (-)-ψ-ephedrine, (-)-α-phenylethylamine, and (S)-(-)-binaphthol as optical active source. Their catalytic activities in the asymmetric borane reduction of prochiral ketone and imine, the asymmetric alkylation of aldehyde with Et2Zn,and the asymmetric silylcyanation of aldehyde were investigated. Among them, it was found that some compounds possess good catalytic activities.

    A Reaction of 2,2'-Propylidene and Dimethylgermyl Doubly Bridged Biscyclopentadiene with Iron Pentacarbonyl
    ZHU Bo-Lin, ZHANG Jian-Yong, XU Shan-Sheng, WANG Bai-Quan, ZHOU Xiu-Zhong, WENG Lin-Hong
    2001, 22(S1):  77-80. 
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    The reaction of boubly bridged ligand (Me2C)(Me2Ge)(C5H4)2(1) with Fe(CO)5 in refluxing toluene and xylene was found to give a novel complex (Me2C)[(η5-C5H3)[(Me2Ge)Fe(CO)2](η15-C5H3)[Fe(CO)2](2), a diiron complex (Me2C)(Me2Ge)[(η5-C5H3)Fe(CO)]2(μ-CO)2(3),having bridging carbonyl groups, and a degermylation product (Me2C)[(η5-C5H4)Fe(CO)]2(μ-CO)2(4). The molecular structure of 3 has been determined by X-ray diffraction. The possible mechanism was discussed.

    Study on Spectral Properties of Photochromic Spiropyrans Having a SchlfF Base Group and their Interaction with DNA
    ZHANG Peng, PANG Mei-Li, MENG Ji-Ben, Teruo Matsuura, WANG Yong-Mei
    2001, 22(S1):  81-85. 
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    The photochromic and fluorescence properties of six spiropyrans having a schiff base group were studied. Their interactions with DNA were investigated by UV-Vis absorption spectra and fluorescence spectra.

    Synthesis of Group 6 Metal Carbonyl Complexes Containing Asymmetric Substituted (3-phenylpyrazol-1-yl-5'-phenylpyrazol-1-yl) methane
    WANG Zhi-Hong, YANG Zhi, TANG Liang-Fu, CHAI Jian-Fang, WANG Ji-Tao
    2001, 22(S1):  85-88. 
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    The reaction of 3(5)-phenylpyrazole with CH2Br2 under phase transfer catalysis yields (3-phenyl pyrazol-1-y1-5'-phenylpyrazo-1-yl)methane, CH2(3-PhPz-5'-PhPz) and bis(3-phenylpyrazo-1-yl)methane. Upon treating the isomeric mixture with M(CO)6 (M=Cr, Mo and W) under UV irradiation at room temperature, (3-phenylpyrazol-1-yl-5'-phenylpyrazo-1-yl)methane tetracarbonylchromium, molybdenum or tungsten complexes is isolated, respectively.The molecular structure of CH2(3-PhPz-5'-PhPz)W(CO)4 is determined by X-ray crystallography, which clearly shows that phenyl groups lie in the 3 and 51-positions of pyrazole rings. The compound crystallizes in the monotriclinic space group P2(1)/n, with a=1.7976(7) nm, b=1.3210(5) nm,c=1.8681(7) nm, β=98.293(8)°, V=4.390(3) nm3, Z=8, R=0.0516, Rw=0.0898.

    Studies on the Reduction of Aromatic Oximes Using Borohydride Exchange Resin-Nickel Boride (cat.)
    CHENG Jun-Ran, WEN Jia, LI Yang-Zhou, GUO Xiang-Yun, HUANG Run-Qiu
    2001, 22(S1):  89-91. 
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    Aromatic oximes were reduced with borohydride exchange resin (BER)-nickel acetate in methanol as efficient reducing system, the catalyst nickel boride(Ni2B) was formed in situ.The products of reduction of aromatic ketoximes were the corresponding α-substituted benzylamines, and the products of reduction of aromatic aldoximes were symmetric dibenzyl secondary amines, which was different to the result of reference.Their structures were confirmed by 1HNMR,MS and elemental analysis.

    Studies on Syntheses and Biological Activities of 1H-1,2,4-Triazolo-1-yl Amine Compounds
    LIU Jian-Bing, ZHAO Guo-Feng, LI Yu-Chang, JIN Gui-Yu
    2001, 22(S1):  92-95. 
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    The title compounds 2 were prepared by 1, 4-nuclophilic addition different amine compounds to the precursor of diniconazole 1, which were reduced to give the compounds 3. From the screening results of biological activities, the compounds 3 possess good fungicidal and plant growth regulation activities to some degree, but low herbicidal activities.

    Studies on Syntheses and Biological Activities of Novel 1H-1,2,4-Triazole Compounds
    LIU Jian-Bing, ZHAO Guo-Feng, LIYu-Chang, JIN Gui-Yu
    2001, 22(S1):  96-99. 
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    We prepared the novel triazole compounds containing pyridinyl moiety by Aldol condensation of pyridinecarboxaldehyde with 1-(1H-1,2,4-triazolo-1-yl)ketone and characterized their structures by elementary analysis, 1HNMR and IR, MS spectral data. From the screening results of biological activities, we found that some compounds possess excellent fungicidal activities and good herbicidal and plant growth regulation activities.

    Synthesis and Isolobal Displacement Reactions of Heteronuclear Tetrahedral Clusters (η5-C5H5)(η5-RC5H4)MNiFeS(CO)5(M=Mo,W)
    HU Qing-Mei, ZENG Guang-Huai, SONG Li-Cheng, SUN Jie
    2001, 22(S1):  100-105. 
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    Through isolobal displacement reaction of (η5-RC5H4)MCoFeS(CO)8 (1a:M=Mo, R=H; 1b:M=Mo,R=MeO2C; 1c:M=Mo, R=Me; 1d:M=Mo, R=EtO2C:1e:M=W,R=H) with Cp2Ni, a series of MNiFeS clusters have been synthesized. Further isolobal displacement reactions of 2a,b with Co2(CO)8 and 2c,d with Fe2(CO)9 produce MoFeCoS clusters (η5-RC5H4)MoCoFeS(CO)8 (1a:R H; 1b:R=MeO2C) and MoNiFe2S clusters (η5-C5H5)(η5-RC5H4)MoNiFe2S(CO)10 (3a:R=Me; 3b:R=EtO2C), respectively. New cluster complexes 2c-e and 3a,b have been characterized by elemental analysis, IR, 1H NMR spectroscopy. In addition, the crystal structure of the previously reported analog of 3a,b (η5-C5H5)(η5-MeO2CC5H4)MoNiFe2S(CO)10 (3c) has been determined by X-ray diffraction techniques. 3c belongs to monoclinic system, space group Cc(#9), cell parameters a=1.0051(3) nm, b=1,5311(5) nm, c=1.7437 nm,β=105.5(3)°, Z=4. Final agreement factors R=0.025,Rw=0.033.

    The Fmoc-Strategy Solid-Phase Synthesis of O-Phosphopeptide
    CHEN Shui-Bing, LI Yan-Mei, ZHAO Gang, LUO Shi-Zhong, ZHAO Yu-Fen
    2001, 22(S1):  106-110. 
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    The phosphopeptide and corresponding nonphosphopeptide was synthesized with the Fmoc strategy solid-phase synthesis method. Using N,N-diethyl-dialkyl-phosphoramidity as phosphorylating reagent, some phosphopeptides were obtained by the use of the golble phosphorylation approach, others were obtained from the phosphorylated building block. The peptides were purified with HPLC. The longer the phosphopeptide, the lower the phosphorylating efficiency, Up to now, this Fmoc strategy solid-phase synthesis method with the step-wise phosphotylation approach only can be used in the synthesis of phosphopeptide with Tyr.

    Design, Synthesis, and Biological Activities of Novel Protox Inhibitors Based on Pharmacophore Model (Ⅲ)
    CHEN Kai, YANG Hua-Zheng, LI Yong-Hong
    2001, 22(S1):  111-115. 
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    The novel Protox inhibitors were synthesized by solid-phase organic synthesis. For biological tests, the bioassay method of Protox inhibitors was set up. The primary biological tests showed that the compounds anticipating good biological activities have Protox inhibitions in some degree.

    A Novel Cerebroside from the Marine Sponge Phacellia fusca Schmidt
    XU Xiao-Hua, YAO Guang-Min, LU Jian-Hua, LI Yan-Ming, LIN Chang-Jiang
    2001, 22(S1):  116-119. 
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    A novel cerebroside, Phacelliacerebroside A, has been isolated from the sponge Phacellia fusca Schmidt, collected from the XiSha Islands in the South China Sea. Based on the spectral analysis of HNMR、13CNMR, HMQC, 1H-lHCOSY、NOE DIFF, FABMS and GC-MS, its structure was determined as α-glucosylceramide containing three free hydroxyls in the long chain base(LCB), being named as Phacelliacerebroside A. It is the first report of a cerebroside compound isolated from the marine sponge Phakellia sp..

    Synthesis of Novel Bridged Dinucleosides
    XU XiaoHua, CHI Guo-Chen, LU Jian-Hua, YAO Guang-Min, LI Yan-Ming, CHEN Ru-Yu
    2001, 22(S1):  120-123. 
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    A methodology for the synthesis of novel bridged dinucleosides(4, 8) has been reported. The synthesis of target compounds was started from guanosine,uridine, the fully O-acyl-guanosine and uridine were treated with POCl3 in the presence of excessive 1, 2, 4-triazole to give the triazolide derivative (2, 6) which was treated with dialkylamine (0.5 equiv.) to afford the expected protected dimer(3a, 3b, 7a and 7b), after deprotected by MeOH/NH3 solution, the dimers (4a, 4b, 8a and 8b) were obtained, respectively.

    Study of a Novel Asymmetric Synthesis of α-Amino Acids
    HU Ai-Guo, WANG Shan-Wei, ZHAO Xue-Mei, WANG Ji-Tao
    2001, 22(S1):  124-129. 
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    The properties of a novel asymmetric synthesis which we advanced before have been studied. An appropriate mechanism was pushed forward based on these researches. Reaction conditions of this asymmetric synthesis were optimized according to the mechanism as well.

    Synthesis of New Chiral Hydrogenated Quinolinyl-Oxazoline Ligands
    ZHOU Yi-Bo, DUAN Xue-Xin, ZHOU Qi-Lin
    2001, 22(S1):  130-133. 
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    Chiral hydrogenated quinolinyl-oxazoline ligands 2a-c were synthesized from 8-quinolinyl carboxylic acid and chiral amino alcohols. The complex formed from [RuCl2(cymene)] and of 2c acts as an catalyst in asymmetric hydrogenation of acetophenone in #em/em#-PrOH, leading to 2-phenylethanol in 44%ee and 71% isolated yield. The optimizations of the reaction are ongoing in our laboratory.

    Cycloaddition of Bu3P-CS2 Adduct with the Compounds Bearing Unsaturated Bonds
    LIU Yu-Xiu, XU Cheng-Fu, WANG Wen-Hu, CAO Ru-Zhen, LIU Lun-Zu
    2001, 22(S1):  134-140. 
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    The one-pot reaction of Bu3P-CS2 adduct with the compounds bearing unsaturated bonds (electric rich alkynes, phosphonyl alkynes or alkenes) and aldehyde affords dithioles or dithiolanes in mediocre yields. Bu3P-CS2 adduct reacts with azo-compounds and aldehyde to give the thiodiazolidine thiones. The mechanism of reaction is discussed.

    Studies on NaOH-Catalyzed Conjugate Addition of Acetophenone with Chalcones under Solvent-Free Condition:Preparation of 1,5-Diketones
    LIU Wan-Yi, LI Jin-Fu, MA Yong-Xiang, LIANG Yong-Min
    2001, 22(S1):  141-144. 
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    The paper has reported that commerical NaOH efficently catalyzes Michael reactions of chalcones (1) with acetophenone (2) under solvent-free conditions. And a series of 1,5-di aryldiketones can be obtained in 71-90% yields. All the product structures were characterized satisfactorily by IR.1HNMR.MS spectroscopy and elemental analysis. The procedure is performed by grinding the components with an agate mortar and a pestile under solvent-free at room temperature or preheating at 45℃ less than 1.3 hours. The result indicated that the aromatic systems are more active than the ferrocenyl analogous.

    The Stereochemistry of Wittig Reactions of Allylic Diphenylmethyl Phosphorane with Aldehydes
    SHI De-Qing, CHEN Ru-Yu
    2001, 22(S1):  145-147. 
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    By using of 3-methoxycarbonyl-2-propenylidenediphenylmethylphosphorane as phosphorus reagent, 5-substituted-2,4-pentadienoic esters(ABA ester analogs) were synthesized in 76-92% yields under mild conditions. The Wittig reactions of this type of phosphorus ylid shows good stereoslectivity, a possible mechanism was suggested.

    Two New O- and C-glycosylxanthones from the Gentiana tizuensis Franch
    Xuan Tian, XiuZhi Xu, Huiying Zhan, Aili Wang
    2001, 22(S1):  148-150. 
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    Two New Xanthone glycoside, 3-O-β-D-glycopyranosyl-1,6-dihydroxy xanthone 1 and 3-C-β-D-glucopyranosyl-1-hydroxy-7-methoxyxanthone 2 have been isolated from the aerial parts of Gentiana tizuensis Their structures have been established by spectroscopic studies (FABMS, lHNMR, 13C NMR, DEPT and COSY) and by comparison wich closely related compounds.

    Reduction of Carbon Nanotubes
    LIU Lu-Qi, GUO Zhi-Xin, DAI Li-Ming, ZHU Dao-Ben, Czerw Richard Carroll David L.
    2001, 22(S1):  151-153. 
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    Single-walled carbon nanotubes (SWNTs) was cut by a mixture of concentrated sulfuric acid and concentrated nitric acid. The resulting cut SWNTs was converted to acid chloride and then reduced by lithium aluminum hydride. The product was characterized with Raman spectroscopy, FT-IR spectroscopy, and XPS.

    The Crystal Structure and NLO Property of Strontium Tetraborate SrB407
    PAN Feng, WANG Ru-Ji, WEI Jing-Zhi, SHEN Guang-Qiu, WANG Xiaoping, SHEN De-Zhong
    2001, 22(S1):  154-158. 
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    The crystal of strontium tetraborate SrB407 (SBO) with high optical quality has been grown by Kyropoulos method and its structure was determined, which was compared with the structures reported by Perloff & Block,Krogh-Moe and LIU Hong-Chao et al. respectively. The nonlinear optical property of SBO crystal was also investigated.

    Study of Molecular Recognition on Amino Acid Esters by Chirai SalenCo
    LIU Tao, RUAN Wen-Juan, LI Ying, JIANG Dong-Qing, ZHU Zhi-Ang, CHEN Yong-Ti, Albert S. C. Chan
    2001, 22(S1):  159-164. 
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    The molecule recognition of a chirai SalenCo compound towards four pairs of enautiomers of amino acid esters in CH2Cl2 was investigated with UV-vis spectral method. It was found that the SalenCo compound and the amino acid esters could form 1:1 complexes and the associative constants of the molecular recognition reactions were following tbe order KD>KL and K(LeuOMe)> K(AlaOMe)> K(SerOMe)> K(TyrOMe). The ΔrGθmrHθmrSθm values of the recognition processes were determined and the reactions were believed to be exothermic and entropy decreasing. In addition, the conformations with minimal energy of each host-guest molecular system complex were sought by molecular dynamics method. Quantum chemical calculations were performed on these conformations to explain the experimental data, and the model of the recognition mechanism was constructed.

    Preparation and Properties of ZnO-TiO2 and WO3-TiO2 Composite Film Photocatalyst
    CHENG Ying-Zhi, ZHANG Yuan-Ming, TANG Yu, MAO Xuan, CHU Lei
    2001, 22(S1):  165-167. 
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    ZnO-TiO2 and WO3-TiO2 composite film photocatalysts were prepared on porous titanium plates by sol-gel method. Their morphology and structure were characterized by XRD and DTA method. The photocatalystic activity of the film catalysts were investigated for photocatalysdc degradation of methyl orange. It was found that the Zn0-TiO2 film photocataiyst calcined at 450℃ for 1 h with 0.1 mol%(molar percent) of ZnO showed higher photocatalytic activity than that of pure TiO2 film by 77.0%, while the 0.5 mol% WO3-doped TiO2 film calcined at 450℃ for 1 h by 96.7%. TiO2 supported on the porous titanium plates consists of both the anatase phase and the nitile phase, indicating that the addition of appropriate ZnO and WO3 could effectively decrease the temperature of phase from anatase to rulile.

    Synthesis, Characterization and Antitumor Activity of The Complexes of Lanthanide Nitrates with Tris{2-[N-(4'-hydroxy-3'-methoxy-phenyl)-methylyimino-ethyl]amine}
    TAI Xi-Shi, TANG Yu, LIU Wei-Sheng, TANG Ning, TAN Min-Yu
    2001, 22(S1):  168-171. 
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    A tripodal ligand,Tris{2-[N-(4'-hydroxy-3'-methoxy-phenyl)-methyJyimino-ethyl]-amine (L), and its complexes with lanthanide nitrates have been synthesized. These new complexes with the general formula of Ln(NO3)3L·4H20 (where Ln=La, Pr, Eu, Gd, Tb, Er) were characterized by elemental analysis, IR spectra, thermal analysis and 1H NMR spectra. All the complexes are stable in air. The IR and 1H NMR spectra of the ligand and its complexes show that all the C=N groups take part in coordination to the rare earth ions. The thermal behaviors of the La and Eu complexes are similar. The losses occur at 70~75℃ and 176~185℃ corresponding to the loss of two H2O and two H2O, respectively. The weight losses found in this process compare with the theoretical values, so the complexes have lattice water and coordination water. The antitumor activities of partial complexes have been investigated.

    Study on the Ternary System:Cu(Ⅱ)-8-Hydroxyquinoline Functionalized Tetraamine Macrocycle-α-Amino Acid
    SU Xun-Cheng, LIN Hua-Kuan, ZHU Shou-Rong, LIU Tian-Fu, LENG Xue-Bing, CHEN Rong-Ti
    2001, 22(S1):  172-176. 
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    Two 8-hydroxyquinoline substituted dioxotetraamine macrocycles, L1 and L2, have been synthesized and their association constants with metal complexes in aqueous solution have been studied. At 25.0 ±0.1℃,I=0.1mol·dm-3 NaNO3,the stability constants of the ternary system: Cu(Ⅱ)-L(L1 or L2)-α-amino acid were investigated and the appropriate structures with respect to the titration species were proposed according to the literature and the obtained data.. The results show that good linear-free-energy relationship exist in the ternary systems.

    The Synthesis, Crystal Structure of 5,17-Di-(N-p-tert-butyl hydro-xyamino)-11,23-di-bromo-25,26,27,28-tetrainethoxycalix[4] arene and ESR Studies of Its Oxide
    WANG Qi, WANG Ru-Ji, LI Yong, WU Guo-Shi
    2001, 22(S1):  177-182. 
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    5,17-Di-(N-p-tert-butyl-N-hydroxyamino)-11,23-di-bromo-25,26,27,28-tetramethoxycalix[4] arene (Ⅱ),which is a precursor of nitroxide radical is synthesized by selective halogen-lithium exchange reaction of 5,11,17,23-tetrabromo-tetramethoxycalix[4]arene (Ⅰ) with n-BuLi and 2-methyl-2-nitrosopropane (MNP). Compound Ⅱ is characterized by IR lH NMR mass spectrum and elementary analysis. The crystal structure of compound Ⅱ has been determined. Crystals are monoclinic, space group C2/c (No. 15) with a=3.225 5 (7) nm, b=1.439 4 (3) nm, c=2.175 3 (5) nm, β=110.210 (9)°, V=9.478 (3) nm3 and Z=8, with final residuals R=0.073 8 and Rw=0.160 3. According to X-Ray analysis compound Ⅱ is presented in a flattened partial cone conformation, which is less common for calix[4]arenes in solid. The two opposite phenyl rings bearing hydroxyamino groups are in an syn orientation and each molecule exhibits two intramolecular hydrogen bonds, N…H-O, which can also be deduced from IR and NMR spectra. The bond length of N…H is about 0.2 nm and bond angle of N…H-O is about 150°. Compound Ⅱ in solution is easily oxidized to a stable nitroxide biradical and electron spin resonance (ESR) observation reveals that there exists magnetic dipole-dipole interaction and weak spin exchange interaction between the two unpaired electrons in the molecule.

    Crystal Structure of Complex[Hpip] [(salen)Fe(OX)] and Synthesis and Magnetism of Heterotrinuclear Complexes
    YANG Guang-Ming, ZHANG Lei
    2001, 22(S1):  183-187. 
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    The Fe(Ⅲ) complex with oxalate (OX) bridge [Hpip][(salen)Fe(OX)] has been synthesized and the crystal structure has been determind, where pip is piperidine,salen is ethylenebis (salicylideneiminate). Three new heterotrinuclear complexes were synthesized and characterized with the molecular block,namely [(salen)Fe(μ-OX)]2[M(H2O)2nH2O[M=Cu(1), Ni(2),Fe(3)]. The temperature dependence of the magnetic susceptibility of the complexes were measured over the 4.2-300 K range. These results reveal antiferromagnetic, not ferroraagnetic-Jike behaviour(irregular spin state structure) for the complexes. The prerequisite and full condition for Lhe presence of irregular spin state within heterotrinuclear complexes have been discussed theoretically and experimentally.

    Oscillating Reaction Produced from Hydrolysis of Bean Oil in Emulsion
    HE Zhan-Bo, ZHOU Ying-Hui, LI Dong-Mei
    2001, 22(S1):  188-191. 
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    Various effects, including acid strengths, metal ion, addition of surfactant or alkali, on oscillation produced from hydrolysis of bean oil in emulsion had been studied by systematic substitution of reaction components. The reactions were monitored by conductivity and Pt electrode at 30.0±0.1℃, It had been found from experiment that the magnitude of oscillation amplitude is correlative to acid strength. The more strong of the acid strength, the more large the amplitude is. There are very large effects on time oscillatory parameters for the coordination between metal ion and long chain carboxylic acid produced from hydrolysis of bean oil. The addition of assistant surfactants play very different roles for the oscillation, even if they are same kind of type.

    Synthesis and Properties of A Novel Aluminophosphate NK-101
    CHEN Ji-Xin, GUAN Nai-Jia, CHEN Tie-Hong, WANG Jing-Zhong, LI Bao-Hui, SUN Ping-Chuan
    2001, 22(S1):  192-195. 
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    NK-101, a novel aluminophosphate with a thermostable microporous structure, has been successfully synthesized, using a template of p-dimethylamine pyridine in hydrothermal system. And the calcined sample was characterized by adsorption of n-hexane, XRD, SEM, IR, 27Al and 3lP MAS-NMR. It has been proved that the novel zeolite has microporous property, with its pore size larger than 0.43nm. Its crystals are like rice com. It is called NK-101 zeolite.

    Synthesis, Characterization, Thermochromic Behavior of Some Schiff Bases PartⅢ
    ZHU Chuan-Fang, XU Han-Hong
    2001, 22(S1):  196-199. 
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    Bis-substituted-phenylaldehyde-bis-(p-aminophenyl)methane-schiff base (SB) of general formula (R)-phCH=N-ph-CH2-ph-N=CHph(R),where R is p-NO2, m-NO2,p-OH, o-OH, p-Cl,-H, p-OCH3, were synthesized and characterized. They are thermolabile and undergo thermochrocism and thermal decomposition after melting. The TG. and DSC measurement were recorded in dynamic air and interpreted.

    Studies on the Synthesis and Physicochemical Property of Mesoporous Titanosilicate with High Titanium Content
    TANG Xiang-Hai, WEN Xin, SUN Shi-Wei, JIANG Hai-Yan, CHEN Tie-Hong
    2001, 22(S1):  200-203. 
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    With a gel of relatively low template content and high n(Ti)/n(Si) ratio up to 1/4, mesoporous titanosilicate has been synthesized under static conditions by hydrothermal crystallization and post-treatment. The novel approach includes a separate hydrolysis procedure before mixing the titanium and silicon resources during gel preparation. By means of XRD, FT-IR, UV-Vis DRS and selective catalytic oxidation, it reveals that the new approach effectively prevents titanium ions from formation of indissoluble titaniosilicate species in the synthesis gel at high titanium content. The obtained material possesses a highly ordered, hexagonal MCM-41 structure and is thermally stable and catalytically reactive in selective catalytic oxidation. The addition of tetrabutylammonium hydroxide during gel preparation not only helps the formation of stable soluble titanium species hence to improve the efficiency of titanium, but also results in the framework of the material more cross-linked and ordered.

    Two-Dimensional Phase Transition in Mixed Monolayer of Hexadecane and Hexadecyltrimethylammonium Bromide at Air/Water Interface
    LEI Qun-Fang
    2001, 22(S1):  204-207. 
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    The ellipticity coefficients of mixed monolayers of hexadecane and CTAB (hexadecyltrimethyl-ammonium bromide) were measured using a Beaglehole ellipsometer at different temperatures. The experiment results showed that these mixed monolayers exhibit a two dimensional phase transition from condensed phase to expanded liquid phase as the temperature is increased. The phase transition occurs ca. 6℃ above the bulk melting point of hexadecane. The ellipticity coefficients were predicted by a simple physical model. The calculated results agree with the experimental data.

    Preparation and Characterization of Novel Polyethylene Supported Metallocene Catalysts
    ZHU Ning, SUN Wen-Hua, LI Zi-Long, SHAO Chang-Xing, HU You-Liang, HE Jia-Song
    2001, 22(S1):  208-210. 
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    Different meshes powder of polyethylene grafting 4-vinylpyridine copolymers (PEVP) has been produced through the irradiation method. After pretreated with Methylaluminoxane (MAO), the copolymers were used as the supports for Cp2ZrCl2 catalyst. Results of XPS and FTIR measurements show that the catalytic sites have been bridged through MAO on the polyethylene carrier. The percentages of grafting 4-vinylpyridine and supported Cp2ZrCl2 depend on the size of polyethylene powder. The smaller the polyethylene powder, the more percent 4-vinylpyridine group and the Cp2ZrCl2 on the polyethylene chains, and the polyethylene-supported catalyst has a much higher activity for ethylene polymerization.

    Studies on the New Route to Synthesize Microporous AIPO4-CJ2
    LI Niu, XIANG Shou-He
    2001, 22(S1):  211-213. 
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    By using phosphorous acid in place of phosphoric acid as the source of P. microporous aluminophosphate AIPO4-CJ2 has been first hydrothermally synthesized without the presence of organic template molecules. The single crystal of the compound has also been prepared. Structure refinement from single crystal x-ray diffraction has shown that the aluminophosphate prepared by new route,crystalline in the orthorhombic space group P212121 with a=0.942 l(4) nm, b=0.9589(4) nm, c=0.9.929(4) nm, corresponding with AIPO4-CJ2 reported by the researcher of Jilin University. By varying template, pH value as well as concentration of the starting materials, the key factor, which influence the crystallization of AIPO4-CJ2 were deduced In the presence of NH4F, AIPO4-CJ2 can be synthesized by using either o-dipropylamine or triethylamine as template. It can even been prepared in the absence of any organic compound. The existence of NH4F,and phosphorous acid may be the important conditions for the synthesis of AIPO4-CJ2.

    Studies on Molecular Recognition of Triazine Resin to Nucleic Base
    DUAN Yue-Qin, LIU Xiao-Hang, GAO Xian-Hao, LI Chen-Xi, LI Guo-Hua, HE Bing-Lin
    2001, 22(S1):  214-217. 
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    Polyacrylonitrile-divinylbenzene copolymers were synthesised and was modified. As a result, 2,4-diaminotriazines group was introduced into the polymer. The sorption of triazine resin to nucleic acid base molecule in methanol was studied.The interaction of recognition between 2,4-diaminotriazines groups of polymer and nucleic acid base molecule was also studied.

    Preparation of 3-(PolystyrylsuIfonyl) propanol and It's Application in Solid-Phase Organic Synthesis
    SUN Wei-Min, HUANG Wen-Qiang
    2001, 22(S1):  218-222. 
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    Synthesis of 3-(polystyrylsulfonyl)propanol resin and its application in solid-phase organic synthesis is reported. Polystyrene sodium sulfinate 1 reacted with 3-chloropropanol in the presence of the phase transfer catalyst Bu4NI and cocatalyst KI to give the 3-(polystyrylsulfonyl)propanol resin 2. The use of resin 2 as a solid support in solid-phase synthesis was discussed. Boc-L-Ala was immobilized onto resin 2 to give resin 3. Hie remaining hydroxyl group was blocked by benzoyl chloride. Then the Boc-protecting group was removed with 6 mol/L HCl in dioxane and then neutralized with Et3N to afford resin 5. Resin 5 was reacted with phenyl isocyanate to give polymer-supported urea 6. Resin 6 was treated with 6 mol/L hydrochloric acid or a saturated mixture of sodium methoxide in methanol to give N-phenyl-4-methyl hydantoin, while resin 6 was cleaved with a solution of dioxane/methanol/4 mol/L sodium hydroxide (V:V:V=30:9:l)(containing 0.1 mol/L NaOH) to afford N-(α-methyl) carboxymethyl-N'-phenyl urea.

    The Study of Resin Column Chromatographic Separation about Amines
    WANG Rui-Fang, SHI Zuo-Qing, SHI Rong-Fu, SUN Jiang-Xiao, HE Bing-Lin
    2001, 22(S1):  223-226. 
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    The static adsorptions of aniline, N-methylaniline and N, N-dimethylaniline onto ADS-17 in nonpolar solvent and water were studied. The results show that in nonpolar solvent, the adsorption sequence was aniline, N-methylaniline and N, N-dimethylaniiine. The adsorption mechanism relates to the form of hydrogen-bonding. But in water the adsorption sequence was opposite. This appreciates to hydrophobic interaction. In water those three amines could be isolated by dynamic chromatographic separation with the polycarboxylic ester sorbent. The results indicate the feasibility of chromatographic separation of alkaloid in normal press using special resin.

    Synthesis and Characterization of an ABA Triblock Copolymer Consisting of Poly(L-Alanine Acid) as A Component and Poly(Ethylene Glycol) as B Component
    ZHANG Guo-Lin, MA Jian-Biao
    2001, 22(S1):  227-231. 
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    N-Carboxy-L-Aianine acid anhydride (NCA) was synthesized by L-α-alanine and triphosgen. PEG was used to prepare amine-terminated poly(ethylene glycol) (PEG-NH2), which was used to initiate NCA open ring polymerization and produce PLAA-PEG-PLAA block copolymers of various contents and molecular weights. The structural characteristics of copolymers were shown by IR、1H NMR、DSC、WAXD、CD etc. The results showed that products of NCA open ring polymerization initiated by PEG-NH2 were block copolymers. Copolymer's contents and number-average molecular weights were obtained by 1H NMR. The hydrophilicity of PLAA were improved by adding PEG. The results of CD showed the copolymers in aqueous solution existed as α-helical conformation.

    Controlled Sequential Polymerization of PS-PMA-PS by ATRP
    GAO Li-Chao, SHI Lin-Qi, ZHANG Wang-Qing, GAO Jun-Gang, HE Bing-Lin
    2001, 22(S1):  232-235. 
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    Polystrene-Polymethyl acrylate-Polystyrene tri-block copolymer (PS-PMA-PS) was synthesized by modified atom transfer radical polymerization. Using CuCl/α,α'-Bipyridyl complex as catalyst, initiated by 1-PECl,styrene was first polymerized at 130℃. Then using the product as macroinitiator, the di-block (PS-PMA) copolymer were obtained. Meanwhile the tri-block copolymer has also been prepared after adding styrene and actone/l-propanol into the reaction system. PS-PMA-PS was characterized by 1H-NMR and GPC techniques. The results show that the molecular weight distribution of the tri-block copolymer is narrow (MwMn=1.19) as the conversion of monomer is around 70-85%. The molecular weight of the block is in good agreement with designed value. The NMR testified the structure of PS-PAA-PS which was obtained by hydrolyzing PS-PMA-PS.

    Removal of Tristearin with Histidine/Emulsion Liquid Membrane Composite System
    LI Zhan-Yong, SHI Lin-Qi, CUI Jun-Jie, YU Hong-Tao, HE Bing-Lin
    2001, 22(S1):  236-239. 
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    Composite purification material is a novel system, which combined selective adsorption capability derived from adsorbent with selective separation property obtained form membrane. Simulate enzyme/emulsion liquid membrane(ELM) composite systems were prepared to hydrolyze tristearin according to the metabolism of glycerides. Two kind of simulate enzyme were used and compared. The experimental results showed histidine is a good simulate enzyme and can effectively extract tristearin under nearly neutral pH value. The apparent degree of removal was 0.03 by this histidine/ELM composite system.

    The Effect of Adsorbate Molecules on the Particle Diffusion of the Adsorption Resin(Ⅰ)
    WANG Chun-Hong, Shi Rong-Fu, WEN Zhen-Zhen, Shi Zuo-Qing, HE Bing-Lin
    2001, 22(S1):  240-244. 
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    The adsorption dynamics for the several adsorbate moleculars with different size of the macroporous adsorbent based on polystyrene was studied. When the adsorption rate was governed by the particle difTusioa process, it is considered that the ratio of the molecular size of adsorbates to the pore diameter not only influenced the adsorption rate, but also influenced the rate-determination step of particle diffusion. Increasing with the molecular weight of the adsorbates, the rate-determination step of particle diffusion transferred from surface diffusion to pore diffusion. At last, diffusion mass-transfer parameters were measured based on the related diffusion equations.

    Studies on the Synthesis and Properties of the Aminated Polymer Adsorbent with High Specific Surface Area
    SHIRong-Fu, WANG Chun-Hong, SHlZuo-Qing, HE Bing-Lin
    2001, 22(S1):  245-248. 
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    The synthesis and pore structure of the new-type macroporous polymer adsorbent with the function of ion-exchange was studied. Based on the post-crosslinked macroporous polymers, the new adsorbents which have not only the high specific surface area but also the exchange group, were prepared after being aminated by the dimethylamine, trimethylamine and α-pyridine.Additionally,the adsorption properties of this kinds of resins for the phenol and Au(Ⅰ) were also studied.

    Laser Light Scattering Study on Fractal Behavior of Polystyrene Gelation
    NIU Ai-Zhen, AN Ying-Li, RAN Shao-Feng, LIANG De-Hai, ZUO Ju, HE Bing-Lin
    2001, 22(S1):  249-252. 
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    The fractal behavior of gelation of styrene (St) and divinylbenzene (DVB) free radical copolymerization was studied by using laser light scattering. The weight average molar mass (Mw) and the radius of gyration (Rg) of sols were used to monitor the gelation process by using the scaling laws of Mw and Rg with the reaction time t. On the basis of these scaling laws, one new method to obtain the gelation point time was reported.

    Dynamic FTIR Analysis of Stretching Polyurethane
    WU Qiang, LU Xiu-Shan, YANG Shu-Zhen, ZHANG Bang-Hua
    2001, 22(S1):  253-255. 
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    In-phase and quadrature dynamic FTIR spectra of polyurethane with 5Hz stretching under 100Hz phase modulation were presented. Four type carbonyl groups refer to molecular elastic and viscous changes in the polyurethane were clearly identified.

    Photochemical Properties of Poly[oxy[trans-4-(2-phenylethenyl) pyridiniomethyl]-1,2-ethanediyl chloride]
    ZHAO Shu-Na, ZHUANG Jun-Peng, ZHEN Yan, ZHANG Wen-Qin
    2001, 22(S1):  256-258. 
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    Poly[oxy[trans-4-(2-phenyIethenyl)pyridiniomethyl]-1,2-ethanediyl chioride] (Ⅰ) was synthesized by the nucleophilic substitution of trans-4-(2-phenylethenyl)pyridme with poly(oxy[(iodomethyl)-1,2-etlianediyl]], following by halogen ion exchange with sodium chloride. The photochemical properties of the phenylethenylpyridinium functionalized photosensitive oligomer I as well as the relevant compound N-butyl-4-(2-phenylethenyl)pyridinium chloride (Ⅱ) were thoroughly studied in aqueous solution. It was found that under the irradiation of medium pressure mercury lamp with water cooling glass sheath (λ>310 nm) the only photochemical reaction of Ⅱ is trans-cis isomerization, while, under the same circumstance, I undergoes not (only trans-cis isomerization, but also photocycloaddition. It was also found that under the irradiation of low pressure raercuiy lamp (λ=254 nm) the cycloadded polymer will be photolyzed to form its original linear oligomer.

    Studies on Synthesis, Structure and Properties of 1-(1-Napthyl)-2,5-pyrrolidinedione
    YUAN Jia-Long, WANG Guo-Chang, LI He-Xian, HE Bing-Lin
    2001, 22(S1):  259-263. 
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    The 1-(1-Napthyl)-2,5-pyrrolidinedione (NPr) was synthesized by reaction of 1-aminonaphthalene with succinic anhydride, the structure and properties of NPr were studied by FT-IR, DSC, NMR, X-ray diffraction and fluorescence spectra. The results of DSC and X-ray diffraction show that the correct melting point of pure NPr should be 158.3±0.2℃, which is inconsistent with that reported by John L. Hubbard et al.; the sample quenched from melting state in liquid N2 is partially crystallized and undergoes cold crystallization at definite temperature. FT-IR measurement indicates that the stretch vibration of the carbonyl groups splits into two bands at 1705 cm-1 and 1779 cm-1、which correspond to antisymmetrical and symmetrical vibrations, respectively, while the fluorescence spectra further suggest that NPr and naphthalene ring are quite similar in electron distribution structure, which is possibly due to the induction and conjugation effect of the carbonyl groups on the nitrogen atom.

    Fluorescence Studies on Morphological Change of St/DVB Crosslinked Gels During Chloromethylation
    LI He-Xian, WANG Guo-chang, WANG Lin, WANG Ying, HE Bing-Lin
    2001, 22(S1):  264-268. 
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    The morphological change of St/DVB crosslinked gels during chloromethylation was studied by fluorescence spectroscopy using St/DVB crosslinked and hypercrosslinked gels as control samples. It has been found that with increase of chlorine content, the excimer emission band (~325nm) approaches to vanish, while the intensity of multi-ring aggregate emission band (~420nm) quickly reaches a maximum,and then decreases sharply accompanied by appearance of a new broad band centred at ca 488nm which roughly coincides with the typical emission band of hypercrossllinked St/DVB gels. Mearwhile, the result of IR measurement suggests that methylene bridge between phenyl rings forms and increases with chloromethylation process. These results are explained in terms of a side reaction of post-crosslinking, which densifies the loosely crosslinked networks and undoes the densely entangled microgel nuclei. As a result, the morpology of the crosslinked gels becomes more homogeneous with chloromethylation.

    Study on Properties of ssDNA-Carbonized Resin Rheumatoid Arthritis Immunoadsorbent
    YU Yao-Ting, WANG Lian-Yong, LU Jing, CHEN Chang-Zhi
    2001, 22(S1):  269-272. 
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    In this paper, The adsorption properties of ssDNA-carbonized resin rheumatoid arthritis immunoadsorbent were studied,Its specificity for adsorption of RF、hemocompatibility、stability and using safety were evaluated. The results show that the optimum saturation adsorption opacities of the adsorbent for IgMRF、IgGRF and IgARF were 2458、2877 and 11OOIU/mL when immobilized amount of ssDNA was 0.4mg/mL,and the ssDNA-carbonized resin is a safe and effective immunoadsorbent for RA therapy, its potential clinical use is promising in the future.

    Synthesis of Comb Graft Copolymers (Ⅱ)
    LI Hong, ZHANG Wen-Fang, HE Bing-Lin
    2001, 22(S1):  273-277. 
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    Diels-Alder reaction of cyclopentadiene, refined from the by-product C5 fraction in petrochemical industry, and allyl chloride (AC) was carried out by a polymer supported BF3 catalyst to synthesize 5-chloromethyl-2-norbornene (NBCH2Cl). The latter was lithiated and used as an initiator for lhe living anionic polymerization of styrene. A norbornyl-PS macromonomer (NB-PS) was synthesized.Under the catalysis (initiation) of a polymer supported ruthenium carbene complex the macromonomer undergoes ring, opening metathesis polymerization (ROMP) and a comb-shaped graft copolymer was synthesized. The catalytic behaviour of the polymer supported boron trifluoride and ruthenium carbene catalysts is superior to that of their corresponding unsupported counterparts. The mechanism of effect of the polymer supports in increasing catalyst stability and lifetime of the labile propagation active species of metal carbene was discussed.

    Study on the Synthesis and Catalysis Application on Phase Transfer Reaction of Quaternary Ammonium Cyclodextrin Resins
    WANG Yong-Jian, ZHANG Zheng-pu, HE Bing-Lin
    2001, 22(S1):  278-282. 
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    Cyclodextrin resin with quaternary ammonium salt group was synthesized by activation cyclodextrin polymer with epichlorohydrm under alkali condition. The influences of experimental conditions, concentration of NaOH, reaction temperature, reaction time and other conditions, on activating results were studied in detail. The results show that the preparation method is very easy and various kinds of quaternary anrmonium cyclodextrin resins can be synthesized by this method. These resins can notably catalyzed the reaction of benzyl chloride with KSCN to produce benzyl thiocyanate.