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Table of Content

    24 March 1997, Volume 18 Issue 3
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    Articles
    Low-temperature EPR Studies on Axial Ligand-adducts of Imidazolyl Tailed Porphyrin Iron(Ⅲ) Complex
    JlAo Xiang-Dong, DUAN Xin-Hua, HUANG Jin-Wang, JI Liang-Nian
    1997, 18(3):  333-336. 
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    The low-temperature EPRof axial ligand-adducts of imidazolyl tailed porphyriniron (Ⅲ) complex, 5-o-[3-(1-imidazolyl) propoxyl ] pheny1-1O, l5, 2O-triphenylporphyrlnatoiron (Ⅲ) chloride [o-ImPrTPPFe(Ⅲ)Cl]was investigated.The effect of terminal imidazole group of o-ImPrTPPFe(Ⅲ)Cl on the coordination environment of ferric ion wasprobed.The unique magnet1c properties of the week-basicity pyridlnes-adducts of o-ImPrTPPFe (Ⅲ)Cl were observed at 77 K, and the crystal field EPRanalysis for the adductswas made.
    Synthesis,Characterization and Crystal Structure of Lanthanide β-Phenylacrylate Complexes
    LU Wei Min, CHEN Wei-Guo, LU0 Xiao-Yang, DONG Nan, LIANG Ke-Li, HUANG You-Qing, HU Sheng-Zhi
    1997, 18(3):  337-341. 
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    Fourteen coordinattion compounds of lanthanide, β-phenylacrylate, were synthesized and characterized as REL3(RE=Y, La-Yb, HL=β-C6H5CH=CHCOOH) by chemical analysis, IRand NMRspectra and X-ray structure analysis.The crystal of ErL3 crystallizes in monoclinic system with space group P21. Each Er atom was coordinated with sevenoxygen atoms from six β-phenylacrylate groups forming a distorted pentagonal bipyramidconfiguration.
    Dealumination of NaY Zeolite with Oxalic Acid
    LIU Xing-Yun, ZHANG Xu-Zheng, LI Xuan-Wen
    1997, 18(3):  342-347. 
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    The reaction of NaYzeolite with an aqueous oxalic acid solution under mild conditions yields zeolite with framework containing hydroxyl nests which are dewatered to lead tothe formation of the secondary pore when the zeolite is heated above 300℃.As the oxalicacid feed increases, the degree of dealumination of the zeolite increases, the crystallinity isreduced, but about 2O% framework aluminium is removed retaining 95% crystallinity whichdepends mainly on buffering of the system of the zeolite dealumination.There is a very goodlinear relationship with a slope of about 0.25 between mole numbers of the aluminium removed from the zeolite framework and those of the H+ depleted during the reaction of NaYwith oxa1ic acid.This result indicates that the eaction of an aqueous oxalic acid solution withNaYis stoichiometric by four H+ attack on one aluminium of the framework.
    Synthesis,Characterization and Crystal Structure of Ternary Complexes of Copper(Ⅱ) α,β-Unsaturated Carboxylic Acids with 1, 10-Phenanthroline
    WANG Yao-Yu, SHI Qi-Zhen, GAO Yi-Ci
    1997, 18(3):  348-352. 
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    Adetailed synthesis is described for ternary complexes of copper(Ⅱ) α,β-unsaturated carboxylic acids with 1, 1O-phenanthroline.Elementary analysis, IRspectra and thermal analysis show the ternary complexes as CuL2(phen).H2O, where L=CH2=CHCOO and CH2=C(CH3)COO-.The molecular structure of Cu (C4H5O2)2 (phen).H2Owas determined by single crysta1 X-ray diffraction, the result of which shows that the complex ismononuclear with distorted square pyramidal coordination from two monodentatecarboxylates, a bidentate 1,10-phenanthroline and one aquo ligands.The crystal is monoclinic with space group P21/n and unit cell parameters are: a=O.7322 nm, b=l.7948 nm,c=1.6014nm, β=97.12(2), Z=4.
    Studies on Quaternary System CsCl-PrCl3-13%HCl-H2O(25℃)and CsCl-PrCl3-42%HAc-H2O(30℃)
    Ll Ya-Hong, RAN Xin-Quan, CHEN Pei-Heng
    1997, 18(3):  353-356. 
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    The solubillties of the saturated solution of the quaternary system: CsCl-PrC13-13%HCl-H2O (25 ℃) and CsCl-PrC13-42% HAc-H2O (30℃) were studied and the corresponding equilibrium diagram was constructed.Two compounds CsCl.PrC13.6H2O and 3CsCl.PrC13.7H2O were found in each system.It is indicated that the effects of HCl andHAc on the system CsCl-PrC13-H2Oare the same.Wang Hong's interpretation to Meyer' Sreaction was verifled and the relevant properties of the compounds were also investigated.
    Synthesis and Characterization of Bis(amine) Iron(Ⅱ) Porphyrins
    ZHONG Xin-Hua, FENG Yao-Yu, HUANG Jie-Sheng, SHEN Pan-Wen
    1997, 18(3):  357-359. 
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    Aseries of bis(amine) iron(Ⅱ) porphyrin Fe(Ⅱ)TPP(NH2R)2 complexes (NH2R=PhNH2, C6H11NH2, n-BuNH2, PhCH2NH2, NHMe2; TPP=dianion of meso-tetraphenylporphyrin) were prepared by the reduction of Fe (Ⅲ) porphyrins with the correspondingamine in an antiformin system in air as well as by the sodium borohydride reduction method,respectively.The complexes were charaterized by UV-Vis, IRand elementary analysis, andsome important properties of them were discussed.
    A Study of the Electrchemical Characteristics of the Co(salen)-Nafion Modificd Electrode
    ZHENG Dong-Hong, ZHENG Jun-Wei, LU Tian-Hong
    1997, 18(3):  360-363. 
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    A Co(salen)-Nafion modified electrode was prepared by immersing a glassy carbon electrode coated with the Nafion film into the aqueous solution with saturatedCo(salen).The modified electrode showed a stable electrochemical reaction of Co(salen) atabout O V(vs.SCE).The result of XPSindicated the valence of cobalt in Co(salen) changesfrom +2 before to +3 after Co(salen) enters the Nafion film- It is due to forming axis coordination of cobalt with sulfonic group in Nafion film.It was found that the mode of electrontransfer in Co(salen)-Nafion modifled electrode was controlled by physical diffusion and electron hopping, It was also found that the modified electrode could catalyze the reduction of O2to H2O2. The real catalyst may be the adduct of CoⅡ(salen) and O2.
    Studies on Kinetic Method for Detecting Active Intermediate in Enzyme Reaction
    CAl Ru-Xiu, WU Xin-Guo, LIN Zhi-Xin, CHENG Jie-Ke
    1997, 18(3):  364-367. 
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    Anew kinetic method is proposed for detecting active intermediate in enzyme reaction.Due to the reactivity of the intermediate, a proper competition reagent which reactswith the intermediate while the intermediate changes to final product, can be found andadded.By detecting the klnetic process of intermediate reaction with reagent, the information of intermediate can be obtained.The method can be used to study free radical intermediate and non-free-radical intermediate, to study fast reaction and to follow transient process.With this method, the intermediate process in oxidation reaction of norepinephrine with hydrogen peroxide, catalyzed by horseradish peroxidase, is investigated.
    Studies on the Fluorescence Enhancement of Organic Solvents on 2, 3-Diaminophenazine
    ZHENG Qi, HUANG Hou-Ping, CAI Ru-Xiu
    1997, 18(3):  368-371. 
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    The effects of various organic solvents on spectral characteristics of 2, 3-diaminophenazine (DAP), which is an oxidized product of o-phenylenediamine catalyzed bysome oxidase, were investigated.It has been found that there is a little effect on the absorption features of the product by strong polar organic solvents.However, the fluorescence ofthe product is greatly enhanced by strong polar organic solvents, and the quantum yield canbe increased about 3O-fold by organic medium.Further experlmental results show that fluorescence enhancement of organic solvent on DAPare due to the solubility increasing actionand electron donating effect.
    Polarographic Adsorptive Wave of Zirconium-Calcium-Alizarin Red S Mix-polynuclear Complex
    LI Ju-Nan, ZHANG You-Fa, ZHAO Xian-Ju
    1997, 18(3):  372-375. 
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    The formation of zirconium-calcium-alizarin red Smix-polynuclear complex hasbeen investigated.The optimum conditions of the determination of Zr(Ⅳ) by use of the polarographic adsorptive wave of the mix-polynuclear complex have been reported.It can beused for the determination of trace Zr(Ⅳ) in mineral sample.Furthermore, its polarographicbehaviour and the electrode reaction mechanism have been studied.The molar ratio of eachcomponent in the complex has been estimated as nzr(Ⅳ): nca2+: nARs=1: 1: 4
    Preparation of Poly(fuchsin basic) Modified Electrode and Its Application
    SUN Deng-Ming, GU Hai-Ying, YU Ai-Min, CHEN Hong-Yuan
    1997, 18(3):  376-380. 
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    In this paper, the polymerization process and mechanism of fuchsin basic at the glassy carbon electrode were investigated.The polymerization conditions such as applied potential, time and buffer solution were found to affect the polymerzation process.In addition,the modified electrode showed a catalytic ability to the voltammetric response of dopamine.This ability was applied to the determination of dopamine in solution.In pH=7.0 phosphate buffer solution, the linear range of dopamine was 2 × 10－7～1× 10－5 mol/Land the detection limit was 1 × 10－7 mol/L.This modified electrode had a good stability, high selectivity and fast response.
    Electrochemical Studies on Vitamin B12 and Its Derivatives
    ZHENG Dong-Hong, LU Tian-Hong, XI Shi-Quan
    1997, 18(3):  381-387. 
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    The electrochemical studies on vitamin B12 and its derivatives were reviewed in this paper.The importance of eletrochemical studies for explaining the mechanism of B12 coenzyme in body was discussed.The latest results of electrochemical studies on vitamin B12 and its derivatives was reviewed.Aprospect for the electrochemical studies in vitamin B12 and its derivatives was suggested.
    A New Method For the Determination of Aniline by Polarography and the Studies of Its Mechanism
    WEI Jin-Bao, WANG Yu-Bin, TANG Zhi-Yong, XIAO Mei, ZHANG Lin
    1997, 18(3):  388-390. 
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    Anew method was developed for the determination of aniline in waste water.Aniline can react with sodium nitrite in the acid medium.Its diazonium products can react continually with sodlum sulfite and formaldehyde.The last reaction products can reduce at the mercury electrode with a sensitive adsorptive wave (Ep=-O.72 V, vs.SCE).The concentration of aniline is linear with peak current in the range of 1.00×10－7 ～ 5.00× 10－4mol/L.The detection limit is 5.00×10-8 mol/L.The behaviour of polarographic wave was studied and the mechanism of electrode reaction was explored.
    Mechanism and Energetics of the Reductions of Protonated N-Arylfluroenimine by BNAH
    LU Yun, LIU Bo, CHENG Jin-Pei
    1997, 18(3):  391-394. 
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    Free energy changes of each primary steps in one-step hydride transfer and multistep transfer mechanisms in the reductions of protonated N-arylfluorenimines by an NAD (P) Hmodel, BANH, were derived from approprlate thermodynamic cycles by combining PKa.and relevant electrochemical data, The mechanism of the reduction was proposed as onestep hydride transfer from thermodynamic points of view and the isotope-labelling experiments.
    Studies on the Design,Synthesis and Biological Activity of a Novel Type of Acylurea Compound
    YANG Xin-Ling, WANG Dao-Quan, CHEN Fu-Heng, LING Yun, ZHANG Zhong-Ning, SHANG Zhi-Zhen
    1997, 18(3):  395-398. 
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    In order to find new insectlcldes possessing a high activity and excellent selectivity, a novel type of diacylurea containing furan has been designed and prepared.Thus, by the nucleophilic addition reaction of 5-substituted futamide and benzoyl isocyanate, 21 compounds of N-benzoyl-N'-[5-substituted furoyl]urea were obtained in 74.5 % ～ 99.5 % yield.Their structures were confirmed by elementary analysis, IR, 1HNMR and MS.The result of preliminary bioassay demonstrates that some of them show chitin-inhibiting activity against mosqito larvae at 10 mg/L.Especially, compounds 1, 15 and 21 exhibited ＞8O%mortality to larval mosquitoes with the same dead symptom as IKI-7899.
    Studies on Synthesis of Thienyl and Furyl Tetrathiafulvalenes
    WANG Jian-Hua, KU Er-Ban, SHI Zhen, WANG Xiao-Gang
    1997, 18(3):  399-403. 
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    Amethod is proposed to synthesize thienyl and furyl tetrathiafulvalenes (TTF).Three new thienyl-TTF (Ⅶ a-c) and two furyl-TTF (Ⅶ d1-d2) were prepared by the method.The electrochemical property of the five TTFderlvatives prepared was studiedo by cyclic voltammetry.It was found that the value of E1/2 decreased when the electron-donating group was in the thienyl ring of thienyl-TTF, the value of E1/2 increased when electron-attracting groups was in the thienyl ring of thienyl-TTF.No peak appeared on the figure of cyclic valtammetry for furyl-TTF.The potential of reduction was higher than that of oxidation, the electrlc current of the highest peak increased by 50 times than the second peak in the figure of square wave voltarnmogram.The reason why thienyl-TTFderivatives only gave trans-isomers and furyl-TTFgave cis and trans-isomers was discussed.Charge-transfer complex of Ⅶb with TCNQ (1: 1) was also prepared.
    Syntheses and Characterization of Pentacoodinate Organo-Tin(Ⅳ) Complexes (Ⅲ)──Fe—Sn—Fe Containning Trinuclearorganometallic Complexes
    XU Yu-Ming, TAO Wei-Guo, YUAN Yao-Feng, WANG Ji-Tao
    1997, 18(3):  404-408. 
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    Seven novel Fe-Sn-Fe containing multinuclearorganometallic complexes were Prepared by the reaction of bis(cyclopentadienyldicarbinylferro)tin dichloride with Schiff Base or semicarbazones.All of the complexes wre characterized by elementary analysis,IR,NMRand MS, respectively.The central metal, Sn, was five coordinative and the complexes were the bicycloazastannoxides as that reported previously.The substituted group on the carbon atom of the amino acid influenced the chemical shift of Hat the ferrocenyl in the complexes formed.Mass spectra show that Sn-Fe bond is first cleavaged and gives similar fragments as reported previously.
    The Synthesis and Biological Activity of 1-Aryl-4-substituted Pyrazoloyl Thiosemicarbazides and Related Heterocyclic Compounds
    JIN Gui-Yu, HOU Zhen, ZHAO Guo-Feng, CAO Chun-Yang, LI Yu-Chang
    1997, 18(3):  409-412. 
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    Aseries of new acylthiosemicarbazide derivatives (Ⅲ) were synthesized by addition reaction of 1-phenyl-3-methyl-5-chloro-4-pyrazoloyl isthiocyanate (Ⅰ) with aroyl hydrazines (Ⅱ), which were cyclized under an acidic condition to obtain 2-substituted pyrazoloyl amino-5-aryl-1, 3, 4-thiadiazoles (Ⅳ).The preliminary biological tests indicate thatsome compounds of Ⅲ and Ⅳ show a good herbicidal activity.
    Studies on the Reaction of Hemimonothioacetals──The Reaction of 1-Benzoyl-1-methylthio-methanol and Ureas
    ZOU Jian-Ping, ZENG Run-Sheng, WEN Yu-Hua, LIU Xian-Jun, CHEN Ke-Qian
    1997, 18(3):  413-415. 
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    5-Phenyl-2, 4-imidazo1idione (4a) and 1-aryl-5-phenyl-2, 4-imidazolidinediones (4b-4g) have been syntheslzed by the reaction of 1-benzoyl-1-methylthio-methanol with urea (3a) or arylureas (3b-3g) in the slightly acidic medium.The structures of compounds 4a-4g were confirmed by the MS, 1HNMR, IRspectra and elementary analysis.This reaction provides a new convenient method for synthesis of 1, 5-disubstituted-2, 4-imidazolidinediones.
    A New Synthetic Route to Furofuran Lignans with Two Different Aryl Groups─Synthesis of (±)-Methyl Piperitol
    CHEN Ning, WU An-Xin, TIAN Yuan, QIN Bing-Chang, PAN Xin-Fu
    1997, 18(3):  416-417. 
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    (±)-Methyl plperitol, a representative example of furofuran lignans with two different aryl groups was synthesized starting from vanillin and piperonal by employlng a connecting of bromo-β-keto ester and sodium salt of another β-keto ester as the key step.
    Conformation and Polarization for Monodisperse Oligomers and Polymers of Poly(aryl ether ketone)s in Solution
    KE Yang-Chuan, FENG Ji-Kang, REN Ai-Min, ZHENG Yu-Bin, WU Zhong-Wen
    1997, 18(3):  418-423. 
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    By means of ab initio method the dihedral angle of 44° for 4, 4' -difluorobenzophenone and of 51° for MES3 are obtained.UVspectra frorn monodisperse oligomers and their molecular polarization in H2SO4 show that the protonation of H2SO4 acting on carbonyl group is one of the major factors of the polarization.The protonation produces a new absorption peak at λ=4OOnm or so (UV); Meanwhile, the overlapping of planar conformation from polarization produces another new absorption peak at λ=500 nm.Based on the protonation model, the configuration interaction(CI) calculation on it is made, the results of which are ln good agreement with those from experiment.All these prove that the absorption peak at λ=4OOnm for poly (aryl ether ketone)s is resulted from carbonyl polarization.Thus, the polymer molecular weight measured in H2SO4 should be corrected according to ketone content in the main chain.
    Butane Isomerization on SO42- Promoted Mixed Oxide Superacid Catalysts
    MIAo Chang-Xi, GAO Zi
    1997, 18(3):  424-428. 
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    Butane isomerization was catalyzed by a series of SO42-promoted mixed oxide superacid catalysts.Incorporation of Ni, Fe, Mn, or Vinto ZrO2 as a second or third metal component may enhance the isomerization activity of the catalysts under N2 atmosphere, but the catalyst deactivation is rapid.Change to H2 atmosphere can slow the coke formation and improve the activity and selectivity of some mixed oxide catalysts.Supporting Pt is of advantage for enhancing the activity and selectivity of SO42- ZrO2, but it does not work for the mixed oxide catalysts.In the course of reaction under atmosphere, the valence states of incorpordted metal components are unaltered as examined by XPS.The amount of coke deposited on the catalysts is related to their stability, and their initial activities are completely recovered after burning off the coke.Coking is probably the main reason for rapid catalyst deactivation.
    On the Configuration of the [NiH4] Complex in Cubic Mg2NiH4 Structure
    LIAO Meng-Sheng, ZHANG Qian-Er
    1997, 18(3):  429-433. 
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    The configuration of the [NiH4] complex in cubic Mg2NiH4 structure has been investigated by using relativistic density-functional method The crystalline environment was simulated by a cut-off type Made1ung potential.Asquare planar configuration of NiH42-and a tetrahedral configuration of Ni44-Hare assumed, respectively in the calculations.For the square planar configuration, a good agreement of the calculated bond length and force constant with experimental ones was obtained.However, the calculation on the tetrahedral configuration yielded too short Ni-Hbond length and too large Ni-H42-force constant.The comparison between the calculated results and experimenta1 ones gives a clear preference of the square NiH44-configuration over the tetrahedral NiHconfiguration in the cubic Mg2NiH4 structure.
    Studies on the ESR Spectra of Dawson-Molybdovanadophosphonic Compound in the Process of Phenol Hydroxylation
    ZHENG Ying-Guang, YU Jian-Feng, DONG Feng-Xia, YANG Yu, WU Tong-Hao, SUN Chia-Chung
    1997, 18(3):  434-438. 
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    ESRspectra of molybdovanadophosphonic compound with Dawson structure in the process of phenol hydroxylation with H2O2 were studied.Contrasting their ESRparameters at different reaction time, the change of V4+V5+ in the system was analyzed.The results indicated that in the initial stage, a few V4+ were produced in the process of the catalyst synthesized.After two hours, the amount of V4+ increased quickly and two kinds of signals of V4+, V(Ⅰ) and V(Ⅱ) appeared-The ESRparameters of V(Ⅰ) were the same as ones at the initial stage, but the signals of V (Ⅰ) were newly appeared.The increasing amount of V(Ⅱ) is higher than that of V(Ⅰ).We had calcuIated the de1ocalized extent of unpaired electrons by the method of Abragam Pryce and assigned that two kinds of V4+, V (Ⅰ) and V(Ⅱ) are all the active centre of the reaction.
    Kinetics of Dehydration and Desulfation Process of Titania Coated Mica
    ZHOU Jing-Hong, XIAO Wen-De, GU Yan-Fang, GU Hong-Chen, HU Li-Ming
    1997, 18(3):  439-443. 
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    Based on TGcurve, the Freeman-Carroll method was applied to calculate the kinetic parameters of the process of dehydration and desulfation of hydrous titanium oxide film on the titania-coated mica pearl pigments.As a result, the kinetic parameters were obtained.The dehydration period: E=93.32 kJ/mol, n=5.16, A=5.31×1011 min-1; desulfation period: E=l49.25 kJ/mol, n=5.13, A=2.75× 1011 min-1.Simultaneously, comparing with the kinetic parameters of the hydrous tiania powder obtained under the same condition indicated that both the dehydroation process and the desulfation process were more difficult in pigments than in powder.
    Synthesis of Silica-Polysiloxane-Supported Thiacrown Ether Platinum and Rhodium Complexes and Their Catalytic Behavior in the Hydrosilylation of Olefins with Triethoxysilane
    ZHANG Li-Feng, FANG Peng-Fei, LU Xue-Ran, CHEN Yuan-Yin
    1997, 18(3):  444-448. 
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    Silica-polysiloxane-supported thiacrown ether platinum, rhodium complexes were prepared from 6- (ω -undecenyloxymethyl)-1-thia-4, 7, 10, 13-tetraoxacyclopentadecane via hydrosilylation with trlethoxysilane.The products were immobilized on fumed silica, sequentially, followed by reacting with potassium chloroplatinite or rhodium chloride.The complexes exhibited high catalytic activities for the hydrosilylation of olefins with triethoxysilane.
    Studies on [Li+O-]Centers in Oxidation-dehydrogenation of Ethane to Ethene on Li+/MgO Catalysts
    CAI Bing-Xin, ZHANG Ji-Shuang, ZHENG Xiao-Ming
    1997, 18(3):  449-453. 
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    In this paper, the formation mechanism and characterization of [Li+O-] centers on Li+/MgOare investigated by the reaction of oxidation-dehydrogenation of ethane to ethene.The concentration of the centers increases with disappearance of free hydroxyl groups ln Li+/MgO.
    A Study of the Relationship Between the Orbital Exponent in WBEPM Wave Function and the Gradual Ionization Energy of the Electron in Configurations
    LI Gu Sheng, ZHENG Neng-Wu, SU Wei, ZHANG Yi
    1997, 18(3):  454-456. 
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    Racah parameters A, B, Cand spin-orbit coupling coefficientsξ3d are obtained directly from the energy formula of the weakest bound electron and the experimental values of the lonization energy adjusted by a parameter dk.The results are coincided with the experimental values very well.The relationship between the parameterξ and the weighted averages of each electron gradual ionization energy in configurations is discussed.
    Effect of Temperature on Intensity of Spontaneous Raman Spectra in Liquid Core Optical Fiber
    GAO Shu-Qin, LI Zuo-Wei, SUN Xin, ZHANG Wei
    1997, 18(3):  457-459. 
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    Intensity of CCl4 optical fiber Raman spectra is measured in the temperature range from O ℃to 65 ℃ It is indicated that there is a maximun-value of Raman spectral intensity.Several marn factors influencing the optical flber Raman spectral intensity are calculated.The result of theory is in accord with that of the experiment well.
    Interfacial Activity of HDEHP and Its Kinetics Mechanism of Nickel Extraction
    LIU Chang-Xin, CUI Yu, YANG Yong-Hui, SUN Si-Xiu, SUN Guo-Xin
    1997, 18(3):  460-462. 
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    The interfacial tension was determined with drop method for bis(2-ethylhexyl)phosphoric acid(HDEHP) in different diIuents, such as benzene, toluene, cycl0hexane and n-hexane, and the surface excess was calculated according to the different adsorption isotherms.The extraction kinetics of Ni(Ⅱ) with HDEHPhas been studied and an interfacial reaction mechanism was suggested.The relationship between the interfacial structure and this mechanism was discussed.The interfacial activity of extractant and the effect of diluents give a strong evidence qualitatively for supporting this mechanism.
    Analog Thermogram Method(Ⅱ)──Studies on Thermokinetics of Irreversible Consecutive First-order Reactions
    ZHANG Yuan-Qin, HU Qi-Shan, ZENG Xian-Cheng, TIAN An-Min
    1997, 18(3):  463-465. 
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    Based on our previous article, the research method of analog thermogram method for consecutive first-order reactions has been proposed in this paper.The rate constants of the consecutive first-order reactions can be obtained from the thermogram of conduction calorimeter with this method without using any apparatus constants.ln order to test the validity of thls method, the saponifications of diethyl phthalate and diethyl succinate in aqueous ethanol solvent have been studied.The rate constants calculated with this method are in agreement with those in literatures, and therefore, the analog thermogram meth0d for consecutive first-order reactions is believed to be correct.
    Studies on the Surface Wettability and Surface Structure of Polyester Treated with Low Temperature Plasma
    CHEN Jie-Rong
    1997, 18(3):  466-471. 
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    The surface wettability and surface structure of polyester treated with low temperature plasma in O2, N2, He, Ar, H, and CH4 gases are studied.The contact angles of the samples were measured and the critical surface tension yc was determined on the basis of the Zisman's plots- Furthermore, the values of non-polar dispersion force γsc, dipole force γsaband hydrogen bonding force to the surface tensions for the plasma-treated samples were evaluated by the extended Fowkes equation.Mainly because of the contribution of hydrogen bonding force, the surface free energy and surface wettability of polyester which was treated with O2, N2, He and Ar for a short time increased greatly.X-ray photoelectr0n spectroscopy (XPS) shows that the reason was the increase of O2 0r N2 polar functional group on the surface of polyester.
    Properties of Polyethylene Terephthalate/Polysulfonyldiphenylene Phenylphosphanate Flame-Retardant Systems
    WANG Yu-Zhong, ZHENG Chang-Yi, WU Da-Cheng
    1997, 18(3):  472-476. 
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    The molecular-chain-level interactions between polyethylene terephathalate(PET)and polysulfonyldiphenylene phenylphosphanate (PSPPP) have been investigated by FTlR.The existence of the interactl0ns shows the miscibility of PETand PSPPP.PET/PSPPPflame-retardant systems have a very high thermal stabillty, and do not decompose at the processlng temperature of PET.The limlting oxygen index (LOI) values of the systems increase with the content of PSPPP, and are almost not affected by the molecular weights of PSPPPand the blending methods.At the processing temperatures of PET, PSPPPwith lower molecular weights, say Mn＜4000, will cause the degradation of PET, which can be to a certain extent inhibited by adding a stabilizer to the systems.As the results of those, the apparent viscosities of PET/PSPPPsystems with lower molecular weights of PSPPPare higher than those with higher molecular weights of PSPPP.The addition of the stabilizer can decrease their viscosity differences.The apparent viscosities of varlous PET/PSPPPsyStems decrease with the increase of shear rate and the content of PSPPP, and do with the rise of temperature.
    Synthesis of Poly(ether-ester) with PEG Selectively Grafted onto Different Segments and Its Antithrombogenicity
    LIU Chun-Qi, RUAN Ji-Hong, ZHANG Hong-Zhi, FENG Xin-De
    1997, 18(3):  477-480. 
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    α-Methyl-ω-(2, 3-epoxy)propyl poly (ethylene glycol) (Ⅱ) was hydrolyzed to a glycol (Ⅲ) with a pendent poly (ethylene glycol) (PEG) chaln.Poly (ether-ester) (PEEs)with PEGgrafted ont0 the hard segments (H-PEEs) was synthesized by reacting the glycol (Ⅲ), terephthaloyl chloride and poly (butylene glycol) The macromer (Ⅱ) cationically copolymerized with tetrahydrofuran to give a copolyether (Ⅳ) grafted with PEG.Using copolyether(Ⅳ) having an average 1.25 grafts per molecule, the S-PEEs with PEGgrafted onto soft segments was synthesized.The recalcification time for SuPEEs remalned almost unchanged in comparing with ungrafted PEEs, while that for HuPEEs increased by about 100%, even though the hydrophlcillties both of S-PEEs and H-EEs were ralsed slgniflcantly.
    Synthesis and Characterization of Polynitrobenzene and Studies on Its Reaction Mechanism
    ZHENG Hai-Peng, ZHANG Rui-Feng, SHEN Jia-Cong
    1997, 18(3):  481-483. 
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    Astudy of polyphenylene (PP) is always a focus in all kinds of the conjugated polymers.Based on synthesis of poly (N, N-dimethylaniline) (PDMA), polynitrobenzene (PNB) is obtained by modifying PDMAwith concentrated nitric acid in acetic anhydride.This new nitro-substituted PPis soluble in common organic solvents such as acetone, DMFand THFat room temperature.Thls paper describes the synthetic process and confirms the characteristic of PNBby elementary analysis, NMR, FTIRand UV-Vis spectra, then discusses a possible reaction mechanism.
    A Full Aromatic Thermotropic Liquid Crystalline Poly(aryl ether ketone)
    ZHANG Shan-Ju, ZHENG Yu-Bin, YU Zhong-Wen, TIAN Ming-Wen, YANG De-Cai
    1997, 18(3):  484-485. 
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    The synthesis and characterizatiqn of a novel thermotropic liquid crystalline poly (aryl ether ketone)-DBCl based on the reaction of a liquid crystalline mesogenic monomer biphenol and a crystal-disrupting monomer 2-chlorohydroquinone with 4, 4' -difluorobenzophenone are investigated.The novel poly(aryl ether ketone) maintains the excellent properties of the common poly(aryl ether ketone)s and shows a typical nematic texture.
    Copolymerization of Glycolide with Lactide and Measurement of Reactivity Ratios
    LIU Gang, FANG Yue-E, SHI Tian-Yi
    1997, 18(3):  486-488. 
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    The copolymerization of glycolide-lactide is studied by using stannous octoate as an initiator.The contents of two monomer units in copolymers were determined by 1HNMRspectra.The reactivity ratios of monomers were evaluated by Kelen Tudos method and leastsquare-calculation.The monomer reactivity ratlos of glycolide and lactlde are r1=3.4O and r2=O.22 respectively.
    The Antiplastication Effect of Lubricant on Polyurethane Elastomers
    FANG Zhi-Qi
    1997, 18(3):  489-491. 
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    Small amount of lubricant in polyurethane elastomer can notably lmprove physical properties, such as hardness, tensile strength, wear and tear etc.The antiplastication effect can be explained in terms of reduced movement resistance of soft and hard segments, better microphase separation.The reactive lubricant molecular jointing to polyurethane molecular exhibited a better antiplastication effect than inert lubricant which takes a free state.This result can be explained in terms of lubricant-polyurethane thermodynamical non-miscibility,so inert lubricant may be repelled from the system whlle the liquid rubber is solidifying, in contrast to the reactive lubricant can form a stable lubricantion in phases boundary layers.
    Fluorescences and Forms of Water Soluble Copolymers of Styrelle and Acrylic Acid
    WUYUN Qimu-Ge, WU Hong-Ying, B-Gereltu, WU Ha-Shen
    1997, 18(3):  492-494. 
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    The relationship between the fluorescences and structrue of the copolymer of styrene and acrylic acid (ST-AA) was investigated in aqueous solution.When the concentration of ST-AAincreased, there exist monomer fluorescence (λex=258nm, λcm=27Onm) and excimer fluorescence(λcm=375 nm).The excimer fluorescence intensities increased with increasing the concentration of ST-AAand with decreasing pHvalues.When trace amount of molybdenum compound[Mo3O2(O2CCH3), (H2O)3].Br2.2H2O, was added into the aqueous solution of ST-AA, the excimer fluorescence intensities were increased
    The Reactioll Process and Structure of Polyaniline Thermal Doped with Dodccylbenzenesulfonate
    ZHENG Yu-Dong, LI Ji-Bo, HUANG Jiong-Liang
    1997, 18(3):  495-497. 
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    The distinguishing features and structures of polyaniline thermal doped with dodecylbenzenesulfonate at different temperatures without the use of auxiliary solvent have been investigated.The exothermic complexion has been observed during doping process at elevated temperature by calorimeter studies, which results in the formation of a transition responslble for the del0calized polarons observed by UV-Vis spectrum.The resulting complex is shown to form a layered structure with strongly anisotropic characteristics as determined by X-ray diffraction measurement.
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