1992 Volume 9 Issue 3

CORBONBALLS: C60 AND C70
Li Sidian , Yang Pin
1992, 9(3): 1-6
[Abstract](524) [FullText HTML] [PDF 409KB](0)
Abstract:
A brief introduction has been presented to the discovery, laboratory preparation, and structure and spectral characteristics of C60 and C70. The general rule of formation of the closed cage-like fullerenes and their possible applications are also described.
SYNTHESIS OF DUAL COPOLYMER OF METHYLHYDROSILOXANEDIME-THYLSILOXANE AND ITS GRAFT COPOLYMER WITH OLIGOOXYETHYLENE SIDE CHAIN
Ni Jianlong , Lin Yunqing , Wang Fosong
1992, 9(3): 7-10
[Abstract](274) [FullText HTML] [PDF 289KB](0)
Abstract:
The ring opening copolymerization of D4 (octamethylcyelotetrasiloxane) and D4H (tetramethyleyelotetrasiloxane) was studied. The linear copolymers were obtained using toluene sulfonic acid as catalyst.The micro amounts of H2O presented in reaction system was found to be a chief factor influencing the average molecular weight of the product. The molecular weight of polysiloxane decreased markedly on addition of hexamethyl disiloxane (HMDS). Polysiloxanes with olgooxyethylene side chain which might be used as polymer electrolyte after eomplexing with alkali metal salts were obtained through hydrosilylation of the above mentioned polysiloxane and α-allyl oligooxyethylene ether.
HETEROGENEOUS CATALYTIC HYDROGENATION OF 4,5-EPOXY-2-PENTENAL
Song Shuzhong , Yu Junxue , Xi Zuwei
1992, 9(3): 11-14
[Abstract](939) [FullText HTML] [PDF 298KB](0)
Abstract:
The catalytic hydrogenation of 4,5-epoxy-2-pentenal on Pd and Ni catalysts has been studied.For Pd catalyst the products obtained were 4,5-epoxypentanal (1) and 2-hydroxytetrahydropyran (2), and for Ni catalyst they were (2) and 1,5-pentadiol (3).The maximum yield of 1,2 and 3 is 58.8%, 62.0% and 84.7%, respectively. The influences of various catalysts on the composition of hydrogenation products were discussed.
ADSORPTION OF GOLD BY IMPREGNATED RESIN N503 AND ITS APPLICATION IN ANALYSIS OF GOLD IN ORES
Chen Jianrong , Zhou Zhirui , Tang Fulong
1992, 9(3): 15-19
[Abstract](400) [FullText HTML] [PDF 343KB](0)
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The characteristics and mechanism of the adsorption of gold in hydrochloric acid medium by impregnated resin N503 N,N-di(sec-octyl) acetamide have been studied. The ratio of gold to N503 in the adsorbate is 1:2. IR and chemical analysis show that the gold is adsorbed in form of AuCl4-. The adsorption is an ion association reaction:2N503+H++AuCl4-=(N503)2·H+·AuCl4- Gold in ores has been seperated and determined by N503 satisfactorily.
SYNTHESES AND STRUCTURES OF COPPER(Ⅱ)-PHTHALOCYANINE DERIVATIVES AND THEIR MOLECULAR FILMS
Jin Shangde , Guan Jingwen , Shen Qi , Chen Wenqi , Wang Xinping
1992, 9(3): 20-25
[Abstract](267) [FullText HTML] [PDF 455KB](0)
Abstract:
In this paper, copper(Ⅱ)·tetra-4-(2-methoxyethanoxy-carbonyl) phthalocyanine (A) and copper(Ⅱ)-tetra 4-(2-butoxyethanoxy carbonyl) phthalocyanine (B) were synthesized and characterized by elemental analysis, FT-IR, 1H NMR and ESR. UV-vis spectra indicate that most of them are dimeric compounds in CHCl3 solution. X-ray diffraction patterns of the powder samples showed that the stacking arrangments of the molecules are inter-parallel in the tilted way. Presence of organic substituents in phthalocyanine ring somewhat lowers its thermostability. Surface(π)-area(A) isotherms for both compounds in CHCl3 solution onto subphase(water) at 20℃ showed the existence of the obvious interchange among the "gas", "liquid", "solid" phases and both compounds could form a better monomolecular layer film.
SYNTHESIS OF POLY-4,7-DITHIANONYLSESQUISILOXANE PLATINUM COMPLEX AND ITS CATALYTIC ACTIVITY ON HYDROSILYLATION OF OLEFINS WITH TRIETHOXYSILANE
Chen Yuanyin , Lu Xueran , Zhong Zhenlin
1992, 9(3): 26-30
[Abstract](344) [FullText HTML] [PDF 331KB](0)
Abstract:
Fume silica-bound poly-4,7-dithianonylsesquisiloxane platinum complex was prepared from 4,7-dithianonyltrimethoxysilane and fume silica via hydrolysis, followed by treatment with potassium chloroplatinite in acetone under Ar atmosphere. The complex exhibited a high catalytic actvity on the hydrosilylation of olefins with triethoxysilane. Even at a molar ratio of olefin to complex of 105, the hydrosilylation reaction took place smoothly with the turnover number more than 80,000.
SYNTHESIS,CHARACTERIZATION AND ANTITUMOR ACTIVITY OF COMPLEXES OF 2-CARBONYLPROPIONYL (PYRIDINE-4-FORMYL) HYDRAZONE WITH RARE EARTHS
Yang Zhengyin , Wang Liufang , Wu Jigui , Li Xingyu
1992, 9(3): 31-36
[Abstract](300) [FullText HTML] [PDF 420KB](1)
Abstract:
2-Carbonylpropionyl (pyridine-4-formyl) hydrazone (H2PPPH) has been synthesized by a simple method. It is a weak acid, and the complexation was carried out in the water solution of rare earth carbonates. 13 complexes have general composition of RE2(PPFH)3·nH2O (RE=La~Yb, n=2~3). The structures and properties of the complexes were characterized by elemental analysis, IR, UV spectra, TGA-DTA, molar conductance and 1H NMR measuramcnts. Eu2(PPFH)3·3H2O was showed to have a certain antitumor activity.
MANGANESE(Ⅲ) COMPLEXES OF SCHIFF BASES DERIVED FROM β-DIKETONE AND β-ALANINE
Chen Ke , Wu Zhiping
1992, 9(3): 37-40
[Abstract](379) [FullText HTML] [PDF 303KB](0)
Abstract:
Di and trinuclear manganes(Ⅲ) complexes:Mn2 (Hacala-β)2 (O2CMe)4 and Mn3O(bzalaβ)2(O2CMe)3·4H2O,where Haeala-β- and bzala-β2- are the Schiff base anions prepared by condensing β-alanine with acetylacetone and benzoylaeetone respectively, have been synthesized and studied by electronic conductivity, magnetic susceptibility, thermal analyses, IR and UV-Vis spectra measurements.
ON PHOTOCHROMISM OF DMF AND DMSO COORDINATED METAL DECATUNGSTATES IN NON-AQUEOUS SOLVENTS
Zhu Sisan , Yue Bin , Wan Guojiang , Shi Xiaoqun , Gu Yidong
1992, 9(3): 41-45
[Abstract](741) [FullText HTML] [PDF 357KB](0)
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The photochromism of some DMF and DMSO coordinated metal decatungstates in DMF DMSO, and acetonitrile has been studied through ESR,1H NMR, risible spectra and W(Ⅴ) determination. The photochromism is found mainly to be related to the decatungstate W10O324-, the ligands coordinated with metal ions and the solvents used.
EFFECT OF SUBSTITUENTS ON THE MISCIBILITY OF POLY (PROPYLENE CARBONATES) AND ESTERS OF CARBOXYLATED POLY(2,6-DIMETHYL-1,4-PHENYLENE OXIDE)
Huang Yuhui , Liu Yan , Xue Wei , Zhao Shulu , Cong Guangmin
1992, 9(3): 46-48
[Abstract](296) [FullText HTML] [PDF 213KB](1)
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Poly(propylene carbonate)(PPC)(copolymer of 1,2-epoxypropane and carbon dioxde) was blended with the esters of carboxylated poly(2,6-dimethyl-1,4-phenylene oxide),(E(x)C,PPO).The effects of the degree of substitution and chain length of the substituents in E(x)-CyPPO on the miscibility of PPC/E(x)-CyPPO blends were discussed.The miscibility of the blends is increased with the increase of the content and the chain length of the substitute groups in E(x)-CyPPO;however,the blend is immiscible when the content of substitute groups in E(x)-CyPPO was low and the chain length was short. FTIR data indicated that there is a specific interaction between PPC and E(12)-C32PPO.
STUDY ON MASS SPECTRA OF N-SUBSTITUTIVE BENZIMIDAZOLE AND N-SUBSTITUTIVE-2-THIOTHIAZOLIDONE COMPOUNDS
Jia Weiping , Liu Shuying , Cao Jie , Wang Dazhuo , Wang Duhu
1992, 9(3): 49-53
[Abstract](360) [FullText HTML] [PDF 317KB](0)
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The electron impact mass spectra of seven new N-substitutive benzimidazole and N-substitutive-2-thiothiazolidone compounds are reported. General fragmentation mechanism has been discussed by using high resolution precise mass determination and linked scan techniques.
INVESTIGATIONS ON if-E CURVE IN CYCLIC DERIVATIVE CHRONOPOTENTIOMETRY Ⅳ.OSCILLOGRAPHIC VOLTAMMETRIC REDOX TITRATION
Shen Xueming , Chen Hongyuan , Gao Hong
1992, 9(3): 54-57
[Abstract](341) [FullText HTML] [PDF 261KB](0)
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Study on the use of oscillographic voltemmetric titration with if-E curve in redox reaction is carried out. It is shown that if-E curve shifts in the electrode potential axis at the time when the peak of faradaic current of depolarizer appeasror disapears at the end point of titration.This indication technique is highly sensitive and directly visual.
ON THE ERROR ANALYSIS OF THE METHOD OF ESTIMATING NUMBER AVERAGE MOLECULAR WEIGHT OF POLYMER
Yin Mingdong , Fu Yanzen , Li Jigen
1992, 9(3): 58-62
[Abstract](647) [FullText HTML] [PDF 324KB](0)
Abstract:
An error analysis was made to evaluate the method of estimating number average molecular weight of polymer samples from the intrinsic viscosity and GPC chromatogram[2]. The evaluation was made according to a mcdel chrematogram of normal distribution and the result was in good agreement with that obtained from the real polymer samples.
THE INHIBITION COEFFICIENT OF ADSORPTION INHIBITOR
Zou Jinyun , Yang Baohe , Kuang Fugui , Jiang Jia
1992, 9(3): 63-65
[Abstract](488) [FullText HTML] [PDF 213KB](0)
Abstract:
The corrosion inhibition of quinoline, thiourea and benzyltriphenyl phosphonium bromide for carbon steel in acid medium have been investigated by weight loss method.The following relationship between inhibition coefficient γi (ratio of the corrosion velocity without inhibitor to that with inhibitor) and concentration of inhibitor (Ci) was found:logγiiilogCi. In the case of mixed inhibitor systems the over all inhibition coeffiieient γ:can be expressed as:logγ333log C1(concentration of the second inhibifor=constant) and logγ3=logγ1+blogγ2(b31). When b>1, the inhibitors showed a synergistic inhibition effect.
CRYSTAL STRUCTURE OF 4,4'-DIMETHOXY CHALCONE
Zheng Jimin , Zhang Dong , Sheng Panwen , Wang Honggen , Yao Xinkan
1992, 9(3): 66-69
[Abstract](328) [FullText HTML] [PDF 249KB](0)
Abstract:
The molecular structure of 4,4'-dimethoxy chalcone single crystal has been determined by X-ray diffraction method. The crystals are orthorhombie with space group P212121 and a=5.268(3), b=30.639(8), c=8.652(4)Å, Z=4, V=1396.56Å3 and Dx=1.276g/cm3.The structure was solved by direct mothods and refined by full metrix least squares method to the final R=0.082 for 991 reflections having I≥3σ(I). Being irradiated by 1064nm Nd3+:YIG laser beam 4,4'-dimethoxy chalcone crystal produces a light of 532 nm wavelength.
SYNTHESES OF AMPHIPHILIC PORPHYRINS AND THEIR LANGMUIR-BLODGETT FILMS
Wen Ke , Cao Xizhang
1992, 9(3): 70-71
[Abstract](429) [FullText HTML] [PDF 180KB](0)
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Tetra-(N,N-dimethylaminophenyl)porphyrin(TDMAPP) reacts with n-C16H33Br to give quaternary bromides of the amphiphilie porphyrin containing four long aliphatic chains. Its Cu, Zn and Co complexes have been prepared. These porphyrins are capable of forming Langmuir-Blodgett films. The UV-Visible spectra of the L-B films as well as of the solid compounds indicate that the interations between molecules in two cases are different.
STEREOSPECIFIC POLYMERIZATION OF ISOPRENE BY BINARY LANTHANIDE CATALYST
Cai Xiaoping , Gong Zhi , Wang Foshong , Zhu Xinghao
1992, 9(3): 72-75
[Abstract](357) [FullText HTML] [PDF 249KB](0)
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Nd(OPri)Cl2 in combination with AlEt3 is a binary lanthanide catalyst of higher activity for the stereospecific polymerization of isoprene. In this paper, the catalytic activity, as well as the microstruture of the polyisoprene are investigated. The experimental results show that it is a highly effective c talyst for the polymerization of isoprene to produce high cis-1,4 polyisoprene. The catalytic activity and the inherent viscosity[η] of the polyisoprene depend greatly on the amount of catalyst, the molar ratio of Al/Nd as well as the polymerization temperature. The cis-1,4 content of the polyisoprenes obtained is over 93% (determined by IR spectra) and the cis-1,4 level depends slightly on the polymerization conditions.
POLYMERIZATION OF EPICHLOROHYDRIN BY YTTRIUM ACETYLACETONATE
Zhang Yifeng , Shen Zhiquan , Zheng Ronghua , Chen Xianhai
1992, 9(3): 76-78
[Abstract](560) [FullText HTML] [PDF 204KB](0)
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Y(acae)3-H2O-Al(i-Bu)3 was used for homopolymerization of epichlorohydrin(ECH) and copolymerization of ECH with propylene oxide(PO) or ethylene oxide(EO). The molecular weight distribution of PECH determined by GPC showed that the number of the active species in the catalyst depends on the method of catalyst preparation. For copolymerization the monomer reactivity ratios obtained by NMR as follows:2.08/0.21 for PO/ECH, 11.9/0.21 for EO/ECH.
IMPROVED METHOD OF SYNTHESIS OF COUMARIN
Zhou Chengdong , Xie Guolong , Lin Fuqin
1992, 9(3): 79-82
[Abstract](951) [FullText HTML] [PDF 262KB](0)
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The synthesis of coumarin has been improved with good yield by yarying the adding order of the starting materials and using polyethylene glycol as phase transfer catalyst. Optimum molar ratios were salicylaldehyde:acetic anhydride:potassium acetate=1:3.7:0.5 and salicylaldehyde:acetic anhydride:potassium fluoride=1:3.7:0.35.
STUDIES ON THE COMPLEXES OF RARE EARTH WITH SULPHUR CONTAINING ORGANIC LIGANDS Ⅳ.SYNTHESIS AND CHARACTERIZATION OF SOLID COMPLEXES OF LIGHT RARE EARTH WITH 3-PHENYL-5-(FURYL-2)PYRAZOLINE DITHIOFORMATE
Zhang Weiguang , Tang Ning , Gan Xinmin , Tan Minyu
1992, 9(3): 83-86
[Abstract](288) [FullText HTML] [PDF 264KB](0)
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Five solid complexes of rare earth with 3-phenyl-5-(furyl-2)pyrazoline dithioformate RE(S2CNC13H11NO)3·nH2O(RE=La, Pr, Nd, Sm, Eu; n=2,4) have been synthesized in dry N2 atmosphere and characterized by elemental analyses, IR spectra, molar con uctance, thermal analyses and fluorescence spectra. The results show that ligands are ccordinated to RE ion through two sulphur atom donors.
ON THE NONIONIC SURFACTANTS OF AROMATIC ETHER WITH 1,3,5-TRIAZINE RING
Zhao Tongfeng , Li Xuanrong , Liao Xianxin
1992, 9(3): 87-90
[Abstract](385) [FullText HTML] [PDF 266KB](0)
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Twenty nonionic surfactants were synthesized from aromatic ethers with 1,3,5-triazine ring and oxirane. The relationship is discussed among the surface activity, latherability, emulsibility, dispersibility, solubilization behavior of the surfactants and the chain lengths of the oxirane segment and hydrophobie groups.
THE SURFACE PHOTOVOLTAGE SPECTRA OF TPP AND ITS DERIVATIVES
Han Mingyong , Liu Wang , Wang Yongqiang , An Qingda , Li Tiejin
1992, 9(3): 91-93
[Abstract](338) [FullText HTML] [PDF 193KB](0)
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The surface photovoltaic properties of TPP and its p-phenylsubstituted derivatives as well as metallo derivatives were studied by surface photovoltage spectroscopy(SPS). The results showed that the p-phenylsubstituted groups (-NH2-N(CH3)2,-N+(CH3)3I-) in different degree influenced the surface photovoltaic properties of porphyrins.For-N+(CH3)3I- substituted tetraphenylporphine particularly,the B band in SPS spectra was splitted into two reverse symbolic peaks:-400nm and 469nm. of metalloporpbyrines with FeCl2+,Co2+,Ni2+, Cu2+, and Zn2+, only CuTPP and ZnTPP have the surface photovoltaic property
ENHANCEMENT OF OXYGEN-NITROGEN PERMSELECTIVITY OF PTMSP MEMBRANES BY PLASMA TECHNIQUE
Lin Xiao , Wen Jiumian , Chen Jie , Xu Jiping
1992, 9(3): 94-96
[Abstract](435) [FullText HTML] [PDF 175KB](0)
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PTMSP membranes were modified by plasma technigue in the presence of hexamethyldisiloxane.The oxygen permeation rate Po2 and oxygen-nitrogen separation coefficient α(O2)/N2 of the modified membranes were 1590 barrer and 3.16, respectively.
OXIDATION OF STYRENE IN THE PRESENCE OF CLUSTERS OF TUNGSTEN AND MOLYBDENUM
Zhao Yuying , Zhao Rigetu , Wu Di , Xi Rimo
1992, 9(3): 97-99
[Abstract](286) [FullText HTML] [PDF 201KB](0)
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The catalytic activities of two catalysts, (W3O2(CH3COO)6(H2O)3) Br·2H2O and (W2MoO2(CH3COO)6(H2O)3)Er·2H2O in the oxidation of styrene have been studied. The results showed that these two clusters have better catalytic properties than those given by Irclco(pph3)2 and Rhcl(pph3)2. The catalysts can be used repeatly without change in their structure and activities.
BENZYLATION OF DIPHENYLAMINE CATALYZED BY POTASSIUM FLUORIDE-ALUMINA
Wang Wen , Ma Chen , Yang Yuwei , Hao Shuxuan
1992, 9(3): 100-101
[Abstract](333) [FullText HTML] [PDF 166KB](0)
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The benzylation of diphenylamine was successfully performed in the presence of KFalumina as catalyst.The optimum conditions are diphenylamine:benzyl choride:KF-alumina=1:1.2:0.5(moi ar ratio),DMF as solvent,160±1℃,14h.Yield 88.4%.
CATALYTIC CYCLOPROPANATION OF TETRAMETHYL ETHYLENE
Li Zhengning , Chen Huilin , Yu Zhenyuan , Guo Hefu
1992, 9(3): 102-105
[Abstract](310) [FullText HTML] [PDF 303KB](0)
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Cu(Salad)2, Cu(gly)2H2O, Cu(o-NH2C6H4CO2)2, Cu(ClO4)26H2O, Cu(CH3CN)4ClO4 were use first time for catalyzing cyclopropanation of ethyl diazoaeetate (EDA) with tetramethyl ethylene (TME). Cu(Ⅱ) amino acid salts showed no catalytic activity, when they were used directly. High catalytic activity appeared only cohen they were pre-reduccd to Cu(Ⅰ) High TME/EDA ratio, high EDA/Cat ratio, longer addition period of EDA-TME mixture, and high reaction temperature benefited the product yield. Cu(salad)2 and Cu(gly)2H2O showed higher catalytic efficiency for the reaction under suitable conditions.
SYNTHESIS OF BIS(6-BROMO-N-ETHYLPHENOTHIAZINE-3-YL) TOLUENE-IODIDE
Li Duxin , Bo Gaimei
1992, 9(3): 106-109
[Abstract](291) [FullText HTML] [PDF 253KB](0)
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A novel sensitive dye bis(6-bromo-N-ethylphenothiazine-3-yl)toluene-iodide was synthesized. Its structure has been verified by IR, NMR, MS and elemental analysis. The dye. showed a high sensivity to poly-N-vinylcarbazole and gave an absorbility at 780~900 nm.
SYNTHESIS AND CHARACTERIZATION OF CYCLOPENTADIENYL (OR METHYLCYCLOPENTADIENYL)TITANIUM (Ⅳ) ZIRCONIUM(Ⅳ) TRISDITHIOCARBAMATES
Lü Zhengrong , Gao Songqi , Zhou Yaokun , Wu Shaozu
1992, 9(3): 110-113
[Abstract](388) [FullText HTML] [PDF 293KB](0)
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Thirteen new compounds of type (RCp)M(S2CNR2)3 were synthesized by reacting (RCp)2MCl2(R=H, Me;M=Ti(Ⅳ), Zr(Ⅳ)) with sodium pyrrolidine-, piperidine- and morpholine-dithiocarbamates, respectively. The IR spectra showed that the dithiocarhamic ligands behave as bidentate ligands in the complexes. The 1H-NMR spectra showed that all complexes are rigid compounds.
REACTION KINETICS OF CDDP,CBDCA WITH GUANOSINE AND L-Met
Ding Daoyuan , Hu Jiehan , Yang Zhiyong
1992, 9(3): 114-117
[Abstract](503) [FullText HTML] [PDF 257KB](0)
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The reaction kinetics of CDDP (cisplatin), CEDCA (carboplatin) with guanosine and L-Met are compared by means of HPLC.The results show that the reaction rate of CDDP with Guo is greater than that with CBDCA. However, CBDCA gave more 1:2 products with Guo than 1:1 products and its second hydrolysis rate constant k2 is much greater than its first one k1.For reactions of CDDP and CBDCA with L-Met the second rate constants are measured as 36.1×10-3 and 5.0×10-3M-1S-1, respectively. This may be one of the reasons that CBDCA shows less nephrotoxicity than CBDP.
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