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    24 February 1994, Volume 15 Issue 2
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    Articles
    Synthesis and Characterization of BaTiO3 Nanocrystals
    WANG Xiao-Hui, ZHAO Chun, WANG Zi-Chen, WU Feng-Qing, ZHAO Mu-Yu
    1994, 15(2):  159-162. 
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    BaTiO3 nanocrystals were synthesized by stearic acid-gel methd(SAG) ,using stearic acid, barium stearate and tetrabutyl titanate as raw materials.The synthesis temperature was 650℃ and the formation temperature of perovskites oxide was 950℃ by conventional solid phase reaction method.The transformations of precursor compound to gel and to crystalline phase were characterized by infrared spectroscopy,differential thermal analysis and thermogravimatric analysis.The nanocrystalline BaTiO3 samples were characterized by transmission electron microscope(TEM) and X-ray diffraction.Powders were further analyzed by optical emission spectroscopy and X-ray fluorescence techniques to determine impurity contents and Ba:Ti ratios.Using this synthesis method,small size and high purity BaTiO3 nanocrystal could be obtained.
    Linear Free Energy Relationship of Complexes(ⅩⅤⅡ)──Studies on the Stability of Copper(Ⅱ)-Dioxotetraamine Macrocycles-α-Aminoacids Ternary Complexes
    XIAN Jing-Chun, ZHU Shou-Rong, LIN Hua-Kuan, CHEN Rong-Ti
    1994, 15(2):  163-167. 
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    The stability of Cu( Ⅱ)-12-(2'-hydroxy-5- substituted benzyl) - 1,4,7, 10- tetraazacyclotridecane-11, 13-dione-a-aminoacids ternary systems has been studied by pHtitration method at 25.0±0.1℃and I= 0.1 mol/L KNO3.The formation constants of binary and ternary complexes were obtained.The structures of the complexes and effects of substituents were also discussed.
    Studies on Protonation of Template Molecule Tetramethylethylenediamine Trapped in Zeolite ZSM-35,ZSM-5 and Mordenite
    LONG Ying-Cai, ZHU Mei, SUN Yao-Jun, WU Tai-Liu, WANG Li-Ping, FEI Lun
    1994, 15(2):  168-172. 
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    The protonation of template molecule of tetramethylethylene-diamine( TMEDA) trapped in the channels of zeolite ZSM-35, ZSM-5 and mordenite was studied by using 13C CP MAS NMR and chemical analysis.Aresonance peaks at δ=34-37 ppm in 13C spectra can be assigned to the template molecule of TMEDA with one side protonated,which orderly locates at the main channels.The proton is close to-CH3 group,and far away from-C2H4-group.
    NMR Study of the Reaction of Pd2X2(dpm)2 (X=NCO-,CH3CO2-,SCN-,NO2-;dpm=Ph2PCH2PPh2) Complexes with H2S
    WENG Wei-Zheng
    1994, 15(2):  173-177. 
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    The reactions of Pd2X2(dpm)2(X=NCO-,CH3CO,SCN- and NO;dpm = Ph2PCH2PPh2)with H2Sin CD2Cl2 or CDCl3 were studied by NMRat room and low temperature (-78--60 ℃).In the case of X = NCO- and CH3CO2-, H2S at first reacted with the anions of the palladium complexes and generated HX and Pd2(SH)2(dpm)2 that was subsequently converted to Pd2(SH)2(dpm)2(μ-S)in the presence of excess amount of H2S.In the case of X=SCN- and NO3-,the reactions resulted in the formation of a dinuclear palladium complex with a possible structure of[Pd2(H)(SH)(μ-SH)(dpm)2]+.
    Synthesis and Magnetism of Novel Copper(Ⅱ)-Cobalt(Ⅱ)Oxalato-Bridged Binuclear Complexes Containing Phosphine Ligand
    BAO Jian-Chun, NI Xing, SUN Yue-Ming, XU Zheng
    1994, 15(2):  178-180. 
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    New heterobinuclear complexes,[ Cu( phen)(C2O4) Co(dpp)](ClO4)2(1)and [Cu(dien)(C2O4)Co(dpp)](ClO4)2·2H2O(2), which contain phosphine ligand, were synthesized,where phen, dpp and dien denote phenanthroline, bis( 2-diphenylphosphinoethyl) phenylphosphine and diethylenetrimine respectively.The complexes were characterized with variable temperature magnetic susceptibility.The exchange integral,J, was found to be -11.04 cm-1(1)and -18.34 cm-1(2), indicating that there exists a weaker antiferro-magnetic spin exchange interaction among the metal ions.
    Studies on the Effects of magnetic Field on Molecular Luminescence(Ⅴ) ──The Effects of Constant Magnetic Field on the Room-Temperature-Phosphorescence of Aliphatic Alcohol,β-Cyclodextrin,α-Bromonaphthalene Trimolecular Complex
    ZHANG Yong, HUANG Xian-Zhi, XU Jin-Gou, CHEN Guo-Zhen
    1994, 15(2):  181-184. 
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    The room-temperature-phosphorescence of a phosphorescent trimolecular complex which consists of aliphatic alcohol,β-CD,and α-bromonaphthalene can be enhanced by magnetic field effects(MFEs),and the mechanism of this effect was investigated preliminarily.
    Study on Transport and Separation of Zn(Ⅱ) from Cd(Ⅱ)and Other Metal Ions Through the Emulsion Liquid Membrane of Cyanex 272-Span 80-Toluene
    ZOU Chang-Ying, LI Ke-An, TONG Shen-Yang
    1994, 15(2):  185-188. 
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    The transport behaviour of Zn(Ⅱ)through the emulsion liquid membrane system of Cyanex 272-Span 80-to luene has been studied.The transport conditions of Zn(Ⅱ) with high efficiency and high speed are as follows:membrane phase:0.020 mol/L Cyanex 272+3% (W/V)Span 80+toluene;outer phase:pH 4-5 with SCN-,ClO4-,NO3-,Ac- and Cl- as mediums;inner phase:H2SO4,EDTA,or HCl in needed concentrations; the volume ratio of emulsion to outer aqueous phase: 1-2.5 mL:10 mL.The transport rate of Zn(Ⅱ)in 5min is above 95%.In this case, Many co-ions, such as Cd(Ⅱ), Co(Ⅱ), Ni(Ⅱ) ,Hg(Ⅱ), Cu(Ⅱ) etc.can only be transported a little through this emulsion liquid membrane.So Zn(Ⅱ) can be separated from these ions with satisfactory.
    A Study of Ascorbic Acid Sensor Based on Ascorbic Oxidase Immobilized in an Electropolymerized Poly(o-phenylenediamine) Film
    JIN Li-Tong, ZHAO Gui-Zhu, FANG Yu-Zhi
    1994, 15(2):  189-192. 
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    A chemically modified electrode biosensor is reported.The biosensor has been applied to determine ascorbic acid in human serum.The linear range of detection is 1.0×10-5-2.5×10-7mol/L and detection limit is 1.0×10-8mol/L.The response time is 7 s.The biosensor has advantages of high selectivity,sensitivity and short response time.
    A New Phosphate Ion Sensitive Electrode
    XIAO Dan, YU Ru-Qin, LI Jun, YUAN Kong-Quan
    1994, 15(2):  193-194. 
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    Near thirty years have passed since the first attempt to develop a selective electrode for phosphate and no substantial progress has been made because all reported electrodes have poor selectivity, reproducibility or short lifetime.In this report, we describe a phosphate ion sensitive electrode based on cobalt, which is easily available for practical application in determination of phosphate concentration.The detection limit of 8×10-6mol/Land a linear range of response from 1×10-5mol/L to 1×10-2mol/L for dihydrogen phosphate activity with a slope of 56mV/dec.are obtained in pH 4.0 buffer solutions.The electrode has an excellent selectivity for the dihydrogen phosphate with respect to many common anions such as sulfale,chloride,nitrate and acetate.The electrode shows a long term stability and reproducibility of response for the dihydrogen phosphate.
    The Sensitization of Cupric Ion to the Polarographic Adsorptive Wave of RE-DBF-Chlorophosphonazo System
    YAN Rong, SHI Wen-Zhao
    1994, 15(2):  195-197. 
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    It was presented that the sensitization of cupric ion to the polarographic adsorptive wave of RE-DBF-CPAsystem in this paper.The peak current of PAWcan be increased about 10 times in the solution of 0.1 mol/L NH4Cl in the presence of more than 1.0 mg Cu(Ⅱ) ion.Therefore, it has been established that a sensitive and selective method for determination of trace RE.The linear range is 1.43×10-9-3.0×10-8(RE)mol/L, the detection limit is 7.1×10-10(RE) mol/L.This method has been used to determine trace REin several sample of leaves.The mechanism of sensitization of Cu(Ⅱ) ion to this system has been investigated preliminarily.
    New Method for the Determination of Different Complex Composition Under Excess Reagent or Metal
    HE Xi-Wen, TANG Zhi-Xin, ZHANG Gui-Zhu, YANG Wan-Long, YU Gui-Ying, SHI Hui-Ming
    1994, 15(2):  198-200. 
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    A new method for the determination of different complex composition under excess reagent or metal is presented when complex ratio is unknown.Anew method model was developed, applying method of exhaustion to simulation by computer.The method is a progress to traditional methods and starts a new aspect for the studies of complex composition.
    Determination of Iron,Cobalt and Nickel as Chelates with4-(2-Thiazolylazo)Resorcinol by Liquid Chromatography with Electrochemical Detection
    GE Ri-Le, LI Hui-Mei, LI Nan-Qiang, WANG Er-Kang
    1994, 15(2):  201-203. 
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    It was determined that 4-(2-thiazolylazo)resorcinol(TAR)and the chelates of iron,cobalt and nickel with TARcan be oxided at a glassy carbon electrode.The above chelates andTARwere separated on a spherisorb ODScolumn with a mobile phase of methanol-water(55/45,V/V) containing0. 01 mol/L Na2HPO4-KH2PO4 buffer(pH7.0) and were detected at 0.86V.The calibration graphs were rectilinear from 0.1-5 ppm,0.01-5 ppm,0.08-1 ppm for iron, cobalt and nickel, respectively.The detection limits were 0.8,0.2,0.8 ng for iron,cobalt and nickel respectively.The method has been applied to the analysis of hair samples.
    AC Oscillopolarographic Titration of Norfloxacinum
    LI Yan-Wei, XUAN Chun-Sheng, LIU Yue-Hong, GAO Hui-Wen
    1994, 15(2):  204-206. 
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    This paper describes the determination of norfloxacinum(FPA)by ACoscillopolarographic titration, which is rapid and of good accuracy, and satisfactory results was obtained.The average recovery of samples was 100.1%and the relative error was less than 0.6%.
    Acidities of α-and para-Substituted Anilines and of the Corresponding Radical Cations in DMSO Solution
    ZHAO Yong-Yu, HUAN Zhen-Wei, CHENG Jin-Pei
    1994, 15(2):  207-210. 
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    Acidities of the α- and para-substituted anilines and their radical cations were determined respectively by an accurate spectrophotometric titration and by a thermochemical evaluation.The simple method used in estimating the acidities of radical cations involves combining the equilibrium acidities of the parent acids(HA) in DMSO with the oxidation potentials of the neutral molecules,Eox(HA), and of their conjugate bases,Eox(A-), defined from a thermodynamic cycle.The results were discussed in terms of the substituent effects.
    Preparation, Characteristics and Separation Mechanism of Thio Crown Ether Polysiloxane Stationary Phases
    WU Cai-Ying, HU Zhen-Bo, CHENG Jing-Song, LU Xue-Ran, ZENG Zao-Rui
    1994, 15(2):  211-215. 
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    A new kind of thio crown ether stationary pases, ω-undecylene thio-15-crown-5,was synthesized.This stationary phase indicates good thermal stability, medium polarity and excellent selectivity for n-alcohols, ester and aromatic compounds,their chromatographic characterization and separation mechanism have been investigated by measuring various thermodynamic parameters.The separations of di-chloro benzene, nitro toluene and di-nitro toluene position isomers on the column were made as examples.
    A Novel Aryl Rearrangement Reaction(Ⅱ) ──β-Aryl Rearrangement in the Tetral-1-ones
    LI Liang-Zhu, ZHAO Xiu-Min, ZHAO Ya-Jun, YAUN Jin-Fang
    1994, 15(2):  216-219. 
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    The aryl group of 3-aryltetral-1-ones was shifted to position-2 yielding 2-aryl-3-fluorotetral-1-ones when the enol silyl ethers derived from the 3-aryltetral-1-ones were treated with iodosobenzene- borontrifluoride complex(PhIO·BF3).As the aryl was Ph-,p-Cl-Ph-, p-Me-Ph-, and p-MeO-Ph-, the yields of the products was 80%, 61%, 10% and 5% respectively.The rearrangement mechanism was suggested to be a successive process.the end silyl ether 2 reacts with PhIO·BF3 to form an intermediate 6.3-Aryl group has a backside migration to C-2which is deficient in electron as iodine atom departs from it, and the fluorine atom attakcts C-3while the heterolysis of fluorine-boron bond is completed.
    Studies on Condensed Heterocyclic Compounds(X)──Synthesis and Biological Activities of 3-Aryl-6-benzoylamino-striazolo[3,4-b]-1,3,4-thiadiazoles
    ZHANG Zi-Yi, LI Ming, ZHAO Lan, LI Zheng-Ming, LIAO Ren-An
    1994, 15(2):  220-223. 
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    S-triazolo[3,4-b]-1,3,4-thiadiazoles are fused heterocyclic derivatives showing various biological effect, such as antifungal, antibacterial, hypotensive and CNSdepressant.In view of the pharmacological and synthetic interests of this kind of fused heterocycles, we investigate the reaction of 3-aryl-4-amino-5-mercapto-1,2,4-s-triazoles 1a-j with benzoyl isothiocyanate in the presence of absolute acetone and obtained a series of 3-aryl-6-benzoylamino-s-triazolo[3,4-b]-1,3,4-thiadiazoles,2a-j, whose structures were determined by elemental analysis, IR, 1H NMR and MS.The possible mechanism of this reaction has been suggested in the meantime.It was found that the representative compound 2h has moderate herbicidal activity.
    Syntheses and Bioactivities of Novel Trifluoromethylpyridine Derivatives
    QIAN Xu-Hong, TANG Jun, CHEN Wei-Dong, ZHANG Rong, HUANG De-Yin, NI Chang-Chun, GUO Qing-Ming
    1994, 15(2):  224-226. 
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    Nine trifluoromethylpyridines 1-9 with trifluoroethoxyl,ethoxyl or dimethylamino groups have been synthesized and their characterization studied by MS,1H NMR and TLC.The screen study of their bioactivities shows compounds 1, 2 and 5 have good insecticidal activities,compound 8 has some insecticidal, strong fungicidal and very strong herbicidal activities.
    Syntheses,Structure and SAR Study on Sulfonylurea Compounds(Ⅲ) ──Crystal and Molecular Structure of N-[2'-(4,6-dimethyl)pyrimidinyl]-2-ethyl Carboxylate-benzene Sulfonylurea
    LI Zheng-Ming, JIA Guo-Feng, WANG Ling-Xiu, LAI Cheng-Ming
    1994, 15(2):  227-229. 
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    Here we reported the crystal structure of title molecule.The crystal is monoclinic, belonging to space group P1 with unit cell parameter a=0.9134(2) nm,b=0.9567(4) nm,c=1.2647(3)nm,a=73.88(3)°,β-70.93(2)°,γ=64.05(4)°,V=0.9273 nm3,Dx=1.36g/cm3,μ=1.99 cm-1, F(000)=396 for 1818 reflections.R=0.063.Molecular structure has been discussed.There are three different planes in the molecule, in each of which a conjugated system was formed.The intra-moleucle hydrogen bond between Nand Hatom has been found.
    Phase Transfer-Catalyzed Wittig-Horner Reactions of Phosphorus-containing α-Carbanions
    LIU Zeng-Xun, LIU Shun-Yao
    1994, 15(2):  230-232. 
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    This paper reports Wittig-Horner reactions of phosphorus-containing a-carbanions derived from ethoxy carbonylmethyl phenyl phosphonate(Ⅰ) and cyanomethyl phenyl phosphonate(Ⅱ)with aldehydes and ketones by phase-transfer catalysis.The structures of ten compounds were determined by elemental analysis and 1H NMR.It was discussed that(E)-olefines were obtained by the reaction of(Ⅰ) with aldehydes, and that the mixed products of(E) and(Z)-olefins were obtained by the reaction of(Ⅱ)with aldehyde.
    The Reaction of Aldehydospiropyran with Rhodanine
    LI Zhong-Jie, LIU Xiang
    1994, 15(2):  233-235. 
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    In the presence of NaOAc/HOAc the reaction of 6'- aldehydo(8'-Hor NO2)spiroindolinobenzopyran with 3-methylrhodanine was investigated.It is found that the predominant product is 1,3-bisbenzylidenerhodanine derivative, and its structure was confirmed by quantitative analysis, spectrometries.Besides, intermediate condensation product and Fischer base isolated from the reaction mixture were identified.The reasonable mechanism was proposed.
    Comparative Studies of the Structure and Properties Between LaMnO3 and La0.927Φ0.073 MnO3
    HU Rui-Sheng, XUE Ping, SNEN Yue-Nian, SUN Yong-An, BAI Yu-Shan
    1994, 15(2):  236-239. 
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    Single phase perovskite-type rare earth composite oxides LaMnO3 and La0.927Φ0.073 MnO3, Φ refers to the number of cavities, were prepared by citric acid complex method.Their crystal structure, specific resistance, surface oxygen and catalytic activities for CO2 methanation and COwater-shift reaction were measured.Aprimary comment on their structure and properties was presented.
    Studies on Microstructure of Polyetheretherketone Containing Biphenyl and Properties of the Sulphonated Polymer
    GUO Chun-Xiao, ZHANG Wan-Jin, NIU Li, JIANG Da-Zhen, HUANG Dong-Lü
    1994, 15(2):  240-243. 
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    Using the results of optimized structure of PEEKby AMl programs and the structure similarity between the PEEK without biphenyl and containing biphenyl, we determined the optimized structure of the repeat unit of PEEK containing biphenyl! jd4he microstructure of it's molecule chain.In this work,we also studied experimentally the influence of sulphonation on FTIR spectrum of this polymer.
    A Theoretical Study for Spectra of CoF6n-(n=2,3,4) Complexes
    LIU Han-Xing, LI Bo-Fu, SUN Jia-Zhong
    1994, 15(2):  244-248. 
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    By combining irreducible tensor method with MS-Xa, a new procedure for solving many-electron Schrodinger equation of transition-metal complexes is proposed.As the application, the procedure was employed to calculate the excitation energy of d-d transition state of complexes CoF6n-(n=2,3,4).The mean-square root deviation between theoretical and experimental results is about 2×103cm-1.The influence of the overlapping term in MS-Xa.equation on the one-electron and many-electron properties is analyzed.
    LMO Studies on the Reaction:CNF→FCN
    YANG Jie, TIAN An-Min, LIANG Guo-Ming, YAN Guo-Sen
    1994, 15(2):  249-252. 
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    The localized molecular orbital theory is used to study the reaction mechanism of the isomerization reaction: CNF→FCN.The energy transition state(TS)of the reaction is obtained by Powell's method with 6-31Gbasis set.The localized molecular orbitals during the reaction are obtianed using Boys localization method.Some properties of these localized orbitals, such as orbital types, orbital energies, Mulliken populations and orbital centroids, are calculated.From these results the change of the bond behavior of the system during the reaction is discussed.The results show that the lone pair electrons of the system play an important role in the reaction.
    Catalytic Behaviour of the Oxidative Dehydrogenation of Isobutyl Acid on V-Substituted Molybdenum Heteropoly Compound
    WANG Guo-Jia, WU Tong-Hao, HUA Shi-Ying, YANG Hong-Mao, ZHANG Heng-Bin, JIANG Yu-Zi
    1994, 15(2):  253-256. 
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    The catalytic behaviour of oxidative dehydrogenation of isobutyl acid to methylacrylic acid on the V-substituted molybdenum heteropoly compounds was studied.The effect of vanadium on the stability and acidic property of the catalyst was also investigated by means of IRand DTA, The ESRresults show that the vanadium not only changed physical-chemical properties of the catalyst, but also participated in the reaction, becoming a new catalytic site.
    Application of Fourier Transform Infrared Photacousitc Spectroscopy to Porphyrin Studies(Ⅱ)─FTIR-PAS of Lanthanide Acetylacetonate-meso-Tetra-(Para-methoxyphenyl) Porphyrin Coordination Compounds
    SHI Tong-Shun, LIU Guo-Fa, CAO Xi-Zhang
    1994, 15(2):  257-260. 
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    The Fourier transform infrared photoacoustic spectra of tetra-(para-methoxyphenyl)porphyrin and its coordination compounds LnT(ρ-CH3O)PPacac(Ln : Sm, Gd, Tb, Dy, Ho,Er, Tm, Yb, Lu)in the range of 3600～225 cm-1 were measured and investigated.Because of the coordination bonding between the rare earth ion and nitrogen in T(ρ-CH3O)PPacac forms,the band near 400 cm-1,M-Ostretching vibration on the acetylacetonate ring,becomes weaker,this band is shifted to the lower wavenumber.The bands at 3318.0 and 968.4 cm-1, PN─H stretching vihration, disppears upon complex formation, the vibration coupling between the M-N stretching and the ring deformation appears.
    A Study of Redox Mechanism of Bi-Mo-Nb Complex Oxide Catalysts by ESR and XPS
    CHEN Tong, YUAN Song-Yue, ZHANG Rui-Feng, ZHAN Rui-Yun, YU Zuo-Long
    1994, 15(2):  261-265. 
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    α-Bi2MO3O12 and Nb-doped α-Bi2MO3O12 catalysts were studied by means of in situ ESR and XPS with Ar-ion sputtering.It was observed that the lattice oxygen diffusion and electron transition between Bi and Mo species in the catalyst during the redox cycle.Amodel for the redox mechanism in the catalyst was proposed.The substitution of small amount of Nb5+ for Mo6+ significantly enhances the redox rate due to forming oxygen vacancies caused by doping Nb5+ in α-Bi2MO3O12,which accelerates the transfer speeds of oxygen and electron in catalysts.
    Studies on the Solubilizing Location of Brilliant Yellow in CTAB Micellar Solution
    ZHANG Yun-Hong, LIANG Ying-Qiu
    1994, 15(2):  266-270. 
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    In this paper, the formation of the premicella and the transformation of the premicella to micella for brilliant yellow(BY) in the water solution of cetytrimethylammonium bromide (CTAB)were studied with UVabsorption spectra.With the Gouy-Chapman model, the relation between the change of BY's apparent dissociation constant(△PKm) and the micellar structure parameters was set up.According to the dissociation constants of BYmeasured in water solution and in CTABmicellar solutions with different concentrations of salt,the distances between BYand the surface of the micella were determined, which were used to demonstrate the solubilizing location of BYin CTAB micella and to characterize the property of CTAB micella adsorbing BY anions.
    A Study on ECID Spectra of Doubly Charged Ions Produced from Four Kinds of Chlorotoluene Isomers
    QIU Feng-He, LIU Shu-Ying, HUANG Cheng-Yi, ZHANG Fa-Yi, SUN Hong-Wei
    1994, 15(2):  271-274. 
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    The Electron Capture Indued Decomposition(ECID)spectra of[C7H7Cl]2+,[C7H6Cl]2+ and[C7H5Cl]2+doubly charged ions produced from four kinds of chlorotoluene isomers in the ion source of mass spectrometer under 70 eVelectron impact were studied in this work.The ECID spectra for[C7H7Cl]2+ from o-chlorotoluene can be distinguished with those from other isomers due to the ortho-effect, which implies the structures of the stable doubly charged molecular ions retain the characteristics of those of neutral molecules to some extent,while the ECIDspectra for[C7H6Cl]2+and[C7H5Cl]2+ from the isomers were identical,respectively,which means that the isomerizations occured prior to the decompositions.The dependence of the ECIDreactions on whether the parent ion is a odd or even electron ion was also discussed.
    Studies on ZnAl Hydrotalic-like Compounds Intercalated with Tungstophosphoric Heteropoly Compound and Their Acid-Base Catalytic Behavior
    LIU Ji-Guang, JIAO Qing-Ze, ZHANG Peng, GUO Jin-Fu, JIANG Da-Zhen
    1994, 15(2):  275-278. 
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    The Keggin-ion[NiPW11O39(H2O)]5-,[CoPW11O39 H2O)]5- intercalated ZnAl hydrotalic-like compounds were prepared.Their crystal structures were characterized by XRDand IR.The result of elementary analysis shows that the products have the composition ratio of ZPW11.Thermal analysis of the compounds was made by DTA.In isopropyl alcohol reaction,the products exhibit the characteristics of strong acidic catalyst while the ZnAl lavered double hydroxide is a typical base catalyst.
    The Catalytic Behaviour of Monosubstituted Heteropoly Compounds in the Oxidation of Cyclohexene with Molecular Oxygen
    QIN Du-Jie, WANG Guo-Jia, WU Yue
    1994, 15(2):  279-280. 
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    In this paper, it was found that the transition-metal substituted heteropolymolybdates,{[(n-C4H9)4N]5PMo11(Zn+L)}(Z=Mn, Fe, Cu; L=unknown), were remarkably effective catalysts for the selective oxidation of cyclohexene with molecular oxygen under mild coriditions.Based on this, the results obtained were compared with the results for the same reaction catalyzed by related substituted heteropolytungstates and metalloporphyrins.It was found that although Mo6+ and W6+ in monosubstituted polyoxometalates could participate in the reaction,the main active center in them, is substituting transition metal.
    Dispersion of SiO2 Powders in Non-aqueous High Concentration Polymer Solution
    CHEN Li-Fu
    1994, 15(2):  281-282. 
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    The dispersion of silica in concentrated courtelle/DMFsolution was studied(Courtelle is a copolymer of 94 mol%acrylonitrile and 6 mol%methyl acrylate).It is found that the agglomeration of silica is the combined results of surface energy and surface hydrogen bonding, The dispersibility of silica is markedly improved by the addition of 3-trimethoxysilyl propylmethacrylate(>1.2%).The improvement is believed to be caused by the chemical reaction between the silane and silanol groups on silica surface, reducing the concentration of hydrogen bonding, hence the attractive forces.
    Preparation of Monodispersed Particles of Barium Carbonate by Takiyama's Method
    WANG Shi-Quan, WANG Ze-Xin, WU Shi-Ying, CHEN Zong-Qi
    1994, 15(2):  283-284. 
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    Monodispersed dumbbell-shaped particles of barium carbonate were prepared by means of the decomposition of barium-EDTAcomplex with hydrogen peroxide in the presence of ammonium carbonate.
    The Study of Hydrogen Bonding Reaction Between 2,4-Dichlorophenol and Pyridine by Thermometric Titration
    LI Zhi-Wei, CHEN Ai-Tong, HU Ri-Heng
    1994, 15(2):  285-286. 
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    The authors have investigated the titled complex react ion.The result is in agreement with that of the infrared spectroscopy work.The reaction enthalpy △H=-21.0±0.2 kJ/mol,the equilibrium constant k=31±3 L/mol(at 20.0℃ and normal pressure).In addition, the authors have discussed the experiment design and given a new data processing methed for this sort of experiments.
    A Kinetic Study on the Thermal Decomposition of Diethyl 2,3-Di-cyano-2,3-di(X-Substituted phenyl) Succinates in Styrene
    QI Chen-Ze, WU Jing-Jia, DUAN Da-Yong, JIA Zhi-Sheng, ZHANG Bin, YANG Di-Lun
    1994, 15(2):  287-289. 
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    The kinetics of thermal decomposition of diethyl 2,3-dicyano-2,3-di(X-substituted 、phenyl) succinates(X=o-OCH3,1;p,m-di-OCH3,2; p-OCH3,3) in styrene at different temperatures was studied by means of dilatometry.The values of Ed for 1,2 and 3 are 134, 64.6 and 51.0 kJ/mol, respectively.The ring substituents of different position in these diesters give the following order of activity:o-OCH3>p,m-di-OCH3>p-OCH3.
    Studies of EO/THF Random Copolyether(Ⅰ)──NMR Analysis for the Liquid Hydroxy Terminated TEO
    ZHANG Jian-Guo, PEI Feng-Kui, WU Yi-Jie, JING Feng-Ying, ZHANG Xi-Tian, TAN Hui-Min
    1994, 15(2):  290-294. 
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    In this work, the chain structure of the liquid hydroxy terminated TEOwas described by 1D13C NMR and 2D COSYspectroscopies.Some difficulties in recognition of the 13C spectra of TEOcome from the overlap of peaks or small difference for chemical shifts.The assignment of the peaks in 13C spectra of TEOwas discussed deeply with information provided from 2D H-H COSYand C-H COSYexperiments.The diads and triads distribut ion were determined by the gated decoupling 13C NMR spectrum and based on the change of sequence structure with the content ratio of EO/THF.The four peaks in the high field of 13C NMR spectrum of TEO(50%EO) sample solution in CDCl3, obviously, were assigned to TTT, TTE, and ETE(-CH2-).In the lower field, the six peaks were identified as ETE(71.12 ppm), TTE(71.08 ppm), TEE 3nd EEE(70.85 ppm), EEE(70.55 ppm), EET(70.55 ppm), TTT(70.52 ppm),TTE (70.52 ppm), TET(70.02 ppm), EET(70.02 ppm).The experiment results indicate that the average functionalities(fn) are about 2, and the average alternated degree close to 50 per cent,so, TEO's are copolyether of the random and the alternation.
    Studies on LB Films of Monoarm Liquid Crystalline Crown Ethers
    HU Zi-Lun, JIANG Qing, QIN Jun, PAN Wei-Dong, XIE Ming-Gui, ZHU Yang-Ming, WEI Yu
    1994, 15(2):  295-298. 
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    Four monoarm liquid crystalline crown ethers(1-4) were first studied by the method of LBtechnique.Among them, 1, 2 and 3 were found to form stable monolayers at air-water interface but 4 not.Monolayers formed by 3 could easily be transferred onto glass substrate to assemble in and to form Ytype LBfilm, Furthermore, the mixed LBfilms of the four compounds with stearic acid(1:1) were studied and Ytype mixed LBfilms were obtained.All above were characterized by π-Acurves and low angle X-ray diffractions.The molecular configurations in the films were estimated with CPKatomic model which gave the same results as experiments.The effect of molecular structures on the stability of LBfilms was briefly discussed.
    Synthesis and Liquid Crystalline Behavior of Polyazomethineethers Containing Pendant Groups of Methoxy
    ZHANG Qi-Zhenl, LI Xiao-Fang, YANG Zhao-He
    1994, 15(2):  299-302. 
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    In this paper,seven main chain thermotropic polyazomethineethers (SAn, n=3～8 are 10synthesized from bis-(3-methoxy-4-hydroxybenzylidene)-4,4'-diimdophenyl.(BISPHENOL)and α,ω-dibromoalkane by phase-transfer-catalysis polyetherification reaction.Their structures and liquid crystalline properties have been characterized by 1H NMR, IR, UV,elementary analysis, polarized microscopy with a hot stage, DSC and X-ray diffractions.Their melting temperature and clearing temperature are affected by the number of methylene groups in the flexible spacer and the usual odd-even effect is observed.
    Studies on the Rigid-Rigid Block Copolymers (Ⅳ)──Preparation and Properties of Polyetheretherketone/Phenol phthalein Polyarylethersulfone Block Copolymers
    CAO Jun-Kui, SU Wen-Cheng, LUAN Tian-Gang, CHEN Yan, WU Zhong-Wen
    1994, 15(2):  303-307. 
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    Aseries of rigid-rigid block copolymers of PEEK/phenolphthalein polyarylethersulfone(PDC) were prepared by the condensation of hydroxyl-terminated PDColigomers and fluorine-terminated PEEKoligomers, and some properties of the copolymers were invest igated by DSC,TGA,WAXDand DMA.The results show that the copolymers exhibited no phase separation.The crystalline structure of the copolymer belongs to orthorhombic unit cell structure, PDCcontent in the copolymers has a great influence on the crystallization behaviour.The thermal stability of copolymers decreases obviously with PDCcontent increasing, The copolymers have very good mechanical properties, the modulus and the tensile strength of copolymer are higher than those of pure PEEK.
    Synthesis and Studies of Liquid Crystal Polymer with Rigid Side Chain
    LI Zi-Fa, GUO Yin-Zhong, ZHANG Chun-Xiao, ZHOU Qi-Feng
    1994, 15(2):  308-311. 
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    A new series of mesogenic monomers and polymers with three benzene rings linked by ester bond are synthesized for the first time by the means of radical polymerization.In this type of liquid crystal polymers, rigid mesogens are directly fixed onto the main chain backbone of polyacrylic ester vertically without flexible spacer, The glass transition temperatures of these polymers are very high and indicate the high rigidities of these polymers.The liquid crystalline behaviour of the monomers and polymers are characterized by DSC, polarized optical microscopy and X-ray diffraction.It is found that all monomers and polymers are nematic thermotropic liquid crystals.Therefore, they represented a new kind of rigid side chain liquid crystal polymers.
    The Effect of Coupling Agent on the Proprties of Flame-Retardant HIPS
    ZHAO Xiao-Guang, SHAO Yong-Ren, LI Hong, ZHOU En-Le, LIU Nan-An, YANG Yong-Kuan
    1994, 15(2):  312-314. 
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    This paper presents the effect of coupling agent on the mechanical properties of flameretardant high impact polystyrene(HIPS), Fire retarding HIPSis usually used with a certain amount of SiO2 as the filler.To improve the properties of HIPS/SiO2 composite material, coupling agent was used to reinforce the surface interaction between HIPSand SiO2. It was found that the concentration of coupling agent strongly affected the mechanical properties of HIPS/SiO2. There existed a critical concentration of coupling agent, at which the properties of HIPS/SiO2 composite material was enhanced apparently.Results obtained from electron microscope showed that after using coupling agent to treat the surface of SiO2, the interface microstructure of HIPS/SiO2 was changed, The mechanical properties of the HIPS/SiO2 can be improved by adding the coupling agent to this system.
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