1989 Volume 6 Issue 3

SYNTHESES OF POLYSILOXANE-SUPPORTED PHOSPHDINEPLATINUM, PHOSPHINE-RHODIUM COMPLEXES AND THEIR CATALYTIC BEHAVIOR FOR HYDROSILYLATION OF OLEFINES
Chen Yuanyin , Lu Xueran , Wang Zhongyu , Yang Yezhi
1989, 6(3): 1-5
[Abstract](317) [FullText HTML] [PDF 330KB](0)
Abstract:
Poly-γ-(p-diphenyl phosphinophenyl)propyl siloxane platinum and rhodium complexes have been synthesized from γ-(p-chlorophenyl)-propyltrimethoxysilane via phosphatization with potassium diphenylphosphide,immobilization and hydrolysis on fumed silica,followed by reaction with potassium chloroplatinite or rhodium chloride. They exhibited high catalytic activity for the hydrosilylation of decene,dodecene, ω-chloroundecene, allyl benzene, phenyl allyl ethe, and allyl glycidyl ether with triethoxysilane from 80 to 100℃ and could be reused several times without loss of activity.
DYNAMIC MECHANICAL PROPERTIES OF THE CROSSLINKED COPOLYMER BASED ON CASTOR OIL POLYURETHANE/VINYL POLYMERS
Liu Wenzhong , Liu JingJiang , Yang Huiming , Han Xiaozu , Hou Chunrong
1989, 6(3): 6-9
[Abstract](246) [FullText HTML] [PDF 511KB](0)
Abstract:
The dynamic mechanical properties of the copolymer networks,AB-crosslinked polymers (ABCP), from a castor oil polyurethane(COPU)and poly(butyl methactylate) (PBMA) were quite different from that of IPN which have the similar composition to ABCP.In the case of COPU/PBMA ABCP,the damping peaks of the two components shift inward and overlap each other,which reveals that the polymer system is partially compatible.However, the damping peak of COPU/PBMA 1PN is a wide plateau.The electron micrographs show the larger domain sizes in IPN than in ABCP.The iesults indicates that the effect of chemical crosslinking on the compatibility is more notable than the physical entanglement. ABCP's from COPU/PST and COPU/PMMA are partially compatible like that of COPU/PBMA,while COPU/PMA and COPU/PBA aro completely compatible.
SYNTHESIS, CHARACTERIZATION AND ANTITUMORIGENIC ACTIVITY OF CARBOPLATIN ANALOGUES
Feng Juncai , Huang Zheyuan , Ni Yaping , Dong Yanhong , Tang Wenxia , Ji Xiujuan , Liu Xiaomei , Wang Longgui
1989, 6(3): 10-14
[Abstract](406) [FullText HTML] [PDF 332KB](0)
Abstract:
Eighteen new complexes PtA2X A=NH3,CH3NH2, 1/2 en(ethylenediamine) and 1/2 dmbn 2, 3-dimethy1-2, 3-butanediamine); X=CPrDCA (cyclopropane-1, 1-dicarboxylic acid), 2-M-CPrDCA (2-methyl-cyclopropane-1, 1-dicarboxylic acid), 2-M -CBDCA (2-methyl-cyclobutane-1,1 -dicarboxylic acid),CPDCA (cyclopentane-1, 1-dicarboxylic acid) and CHDCA(cyclohexane-11-dicarboxylic acid))have been synthesized and characterized. It is found that the activities of complexes[Pt(NH3)2X] against W-256 in rats are in following order:CPrDCA >2-M-CPrDCA >CPDCA >CBDCA(carboplatin) ≥2-M-CBDCA.
REDUCTION OF ACYL DERIVATIVES OF 2, 2-BIS-FERROCENYLALKANES
Yuan Yaofeng , Li Fengze
1989, 6(3): 15-20
[Abstract](331) [FullText HTML] [PDF 421KB](0)
Abstract:
A series of acyl derivatives of 2,2-bis-ferrocenylalkanes have been prepared from 2,2-bis-lerrocenylakanes (i.e. bisferrocenyl methane, 2, 2-bisferrocenylpropane, 2, 2-bis-ferrocenylbutane and 2, 2-bisferrocenylpentane) and acid anhydrides (i.e.acetic-propionic-,n-butyric anhydride) by Friedel-Crafts acylation. The ketones were reduced to the corresponding α-hydroxyalkyl derivatives of 2, 2-bisferrocenylalkanes with LiAlH4·Eighteen α-hydroxyalkyl and di-(α-hydroxyalkyl)derivatives have been synthesized. The synthesis and characteristies of IR and 1HNMR spectra of the compounds have been discussed.
13C-NMR STUDY ON CONFORMATION OF LANTHANIDE COMPLEXES WITH METHIONINE
Ren Jimin , Pei Fengkui , Wang Wenyun
1989, 6(3): 21-25
[Abstract](256) [FullText HTML] [PDF 338KB](0)
Abstract:
Lanthanide-induced shifts have been measured for 13C nuclei of methionine in the presence of seven lanthanide cations (La, P_1, Nd, Dy, Ho,Er, Tm) in aqueous solution.The simulation for conformation of lanthanide complexes with methionine shows that the ligand is coordinated to lanthanide ion through oxygen atoms of carboxyl group and the bend length of Ln-O is 2.7Å. In the complexes,methionine is in extended state,the favorable conformation of Cο-Cα-Cβ-Cγ-S and Cα-Cβ-Cγ-S is in trans, while that of Cβ-Cγ-S-Cδ in gauche. The conformation established for methionine complex by lanthanide-induced shift method is in agreement with the results of vicinyl proton coupling constants and 13C paramagnetic relaxation rate determinations.
STUDY ON PRODUCTION OF SODIUM CARBONATE FROM AMMONIUM BICARBONATE AND SODIUM CHLORIDE
Liao Xiaoyuan , Liu Fang , Huang Jianhan
1989, 6(3): 26-30
[Abstract](860) [FullText HTML] [PDF 314KB](0)
Abstract:
The raw material NH4HCO3 and NaCl in the production of sodium carbonate accordingto the double decomposition NH4HCO3+NaCl→NaHCO3+NH4Cl (2) are plentiful in China. The main difficulty of the process technologically is the separating NH4Cl from the mother solotion I. In this paper the method of adding a middle salt,NH4NO3 or (NH4)2SO4, has been studied. The middle salts can not change the place of the saturated pointes of the reciprocal system in the dry-salt diagram evidently,but can prolong the waiting time for crystallization of NaHCO3 in the mother solution Ⅱ. The effect of NH4NO3 is much better than that of (NH4)2SO4. In adding NH4NO3, the waiting time is prolonged enough to separate tbe crystalline of NH4Cl and the process of the fomula (2) become practicable.
STRUCTURE OF BLENDS OF EPOXY RESIN/POLY (ETHYLENE OXIDE) AND THEIR COMPLEXES WITH SODIUM THIOCYANATE
Zhang Hongfang , Mo Zhishen , Peng Xinsheng , Wang Fosong
1989, 6(3): 31-36
[Abstract](382) [FullText HTML] [PDF 837KB](0)
Abstract:
The crosslinked blends of epoxy resin(ER) and poly(ethylene oxide) (PEO) in various component ratio with different molecular weight were investigated by WAXD, SAXS, DSC and SEM methods. It is found that the crystalline blends of ER/PEO were gradually changed into amorphous and the coherent lengthes were also reduced when ER content was increased The crystal of ER/PEO blend belongs to monoclinic, that of ER/PEO-NaSCN triclinic.The crystallinity of ER/PEO-NaSCN reduces,but its long period increases in comparison with uncomplexed ER/PEO. Increasing ER content results in the increase of noncrystalline zone and long period, as well as the reduction of crystalline lamella.
SYTHESES OF CYCLOPENTANYL(OR ALLYL)CYCLOPENTA-DIENYL LATHANOID DIOHLORIDE TETRAHYDROFURANATE COMPLEXES
Wang Yuling , Chen Wenqi , Zhang Bin
1989, 6(3): 37-41
[Abstract](264) [FullText HTML] [PDF 342KB](0)
Abstract:
In this paper the syntheses of cyclopentanyl (ora llyl) cyclopentadienyl lanthanoid dichloride tetrahydrofuranate complexes are first reported. The complexes of C5H9C5H4·LnCl2-nTHF and C3H5C5H4LnCl2·nTHF (C3H9C5H4=cyclopentanyl cyclopentadienyl; C3H5C5H4=allylcyclopentadienyl; Ln=Nd, Sm, Gd; n=0, 1, 2, 3) are identified by elemental analysis, thermal analysis, IR, MS and NMR measurements. The crysal structure of the reaction intermediate C5H9C5H4Na·THF was determined by the x-ray diffraction method.
SYNTHESIS OF O-ALKOXY-PHENOLS BY PHASE-TRANSFER-CATALYSIS AND THE PROPERTIES OF THEIR LiTHIUM COMPOUNDS
Yuan Qun , Shen Xieqiang , Xu Ying
1989, 6(3): 42-45
[Abstract](317) [FullText HTML] [PDF 264KB](0)
Abstract:
In this paper seven o-alkoxy phenols and their corresponding isotope lithium compounds of 7Li and 6Li have been Frepared through the selective monoalkylating reaction of pyrocatechol and alkylhalides by phase transter catalyst. Li-O absorption frequencies in the IR spectra were found in the range of 500±100cm-1, which obeyed the tetrahedron rule of inorganic lithium compounds. The isotope effect by 6Li and 7Li was also observed.The strong double peak in the range of 1400-1350cm-1 presented in the IR spectra of o-alkoxy phenol parent compounds disappeared in the spectra of their correspounding lithium compounds demonstrating the deformation vibration of OH in the alcohols and phenols. The lithium compounds gave two kinds of aggregate ion peaks in mass spectra namely[LinRn]+ and [LinRn-1]+.
ISOTOPIC FRACTIONATION OF SULFUR IN GYPSUM CRYSTALS
Jiang Jianzhuang , Zhang Qinglian
1989, 6(3): 46-47
[Abstract](359) [FullText HTML] [PDF 140KB](0)
Abstract:
Altogether 45 samples were taken from different parts of three large gypsum crystals collected in China. The mass spectrometric analysis indicated an overall isotopic fractionation factor for 34S, α=1.003±0.001.
STUDY ON PROPERTIES OF THE CELL COMPOSED OF n-TYPE POLYACETYLENE-CARBON FIBRE COMPOSITE FILM
Zhao Jinbao , Sun Qiang , Wei Yuezhen , Zhao Xiaojiang , Wang Fosong
1989, 6(3): 48-50
[Abstract](264) [FullText HTML] [PDF 202KB](1)
Abstract:
The discharge properties of the cell consisted of Li/1mol/dm3 LiClO4+THF/PA/carbon fibre composite film have been investigated by galvanostatic method.When it was discharged at a small constant current the cell showed energy density and capacity up to 726Wh/kg and 624Ah/kg respectively. Increasing PA content in the composite can increase the capacity of the cell, but deteriorate other properties. The rate of self-discharge in a year was below 6%.
STUDY OF FERRITE-TYPE CO SHIFT CATALYST
Wang Yufu , Wang Lijie , Li Wenxia , Wu Yue
1989, 6(3): 51-53
[Abstract](789) [FullText HTML] [PDF 187KB](0)
Abstract:
The ferrite-type catalyst was found to have good activitty. The X-ray diffraction and Mossbauer spectroscopy measurements show that the active structure of the catalyst is non-stoichiometric magnetite:FeA3+[Fe1-3δ2+)Fe1+2δ3+δ]BO4 The structure formed after substituting Cr3+ for Fe3+ seems to be an iron-chromium spinellike mixed oxide:FeA3+[Fe1-x3+Fe2+Crx3+]BO4
DIRECT DETERMINATION OF LIFETOMES OF SINGLET OXYGEN IN VARIOUS SOLVENTS
Wang Wenyun , Tang Youwen , Yu Yingning
1989, 6(3): 54-56
[Abstract](613) [FullText HTML] [PDF 204KB](0)
Abstract:
A Nd:YAG pulsed laser was used to excite photosensitizers to induce the generation of singlet molecular oxygen in sclution. The lifetimes of O2 (1g) in various solvents were determined by monitoring the phosphorescence at 1270 nm. Experimental results reveal that the phosphorescence lifetime of singlet oxygen in solution depends mainly on the property of solvents used.
A NEW METHOD FOR SYNTHESIS OF β, γ-UNSATURATED AMIDES
Li Chaojun , Li Jisheng , Chen Deheng
1989, 6(3): 57-58
[Abstract](317) [FullText HTML] [PDF 122KB](0)
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Reaction of vinylalanate obtained from the readily available. dialkylvinylalane and n-butyl lithium with α-halo-amides produced the corresponding 6, γ-unsaturated amides, withclean retention of the configuration. The yields were 35% to 70%.
THE STUDY OF THIN LAYER SPECTROELECTRO-CHEMISTRY OF [Co(H2O)4(NCS)3](18-C-6)COMPLEX
Yu Zhangyu , Li Haiying , Li Chunying , Gu Dengping
1989, 6(3): 59-61
[Abstract](322) [FullText HTML] [PDF 191KB](0)
Abstract:
The reduction of the title complex on a micro golden grid electrode using thin layer cyclic voltammetry and spectrcelectrochemistry techniques was studied. The results showed that the transfer number of the first step reduction of Co(Ⅱ) was 1, and E0=-0.583V(vs SCE). A mechanisum was Proposed.
THE CRYSTAL STRUCTURE OF DIMETHYLETHANOL-AMMONIUM BIS(O-DIPHENOL)ANTIMONATE
Lu Yunjin , Gu Da
1989, 6(3): 62-64
[Abstract](262) [FullText HTML] [PDF 222KB](0)
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The crystals of the title compound (C16H20O5NSb) are monoclinic with space group P21/n and a=19.055(4)Å, b=8.867(2)Å, c=20.329(5)A; β=102.64(7)° for Z=8. The intensity data are collected on the fourcicle diffratometer of model CAD4-11/44. The structure was refined to R=0.034 for 5603 reflections.
ON THE THERMAL STABILITY OF CHLORINATED POLYVINYL CHLORIDE Ⅰ. INFLUENCE OF CHLOkINE-CONTENT ON THE THERMAL STABILITY
Ma Wenguang , Zhang Zhengbai
1989, 6(3): 65-67
[Abstract](307) [FullText HTML] [PDF 191KB](0)
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The thermal stabilities of chlorinated polyvinylchloride(CPVC) and polyvinyl chloride (PVC) were compared through their infrared spectra and conductivity data. CPVC showed a much higher thermalstability than PVC. The influence of chlorine content in polymers on the stability. has been discussed.
CRYSTAL STRUCTURE OF SmCl3(DME)·2THF
Jin Zhongsheng , Nie Guojun , Hu Ninghai , Chen Wenqi
1989, 6(3): 68-70
[Abstract](718) [FullText HTML] [PDF 185KB](0)
Abstract:
The crystal structure of the title compound in which DME=Dimethoxyethane was determined using x-ray diffractometer. The complex crystallizes in monoclinic space group P21/a with Z=4. Lattice parameters are: a=13.547(8), b=8.607(4), c=16.029(9)Å,β=90.35(5)°. The crystal structure was determined by Patterson and Fourier techniques and refined by least-squares to a final value R=0.0443. The samarium(Ⅲ) ion is 7-coordinate,being bonded to three chlorine atoms, two oxygen atoms of two THF and two oxygen atems of DME. The Sm-Cl distances are in the range 2.647-2.674Å. The Sm-O distances are in the range 2.465-2.504Å.
1H NMR STUDY oF WATER IN H2O-CHCl3-CCl4 SYSTEM
Chen Zi , Wu Xiongwu , Teng Teug , Ning Yongcheng
1989, 6(3): 71-74
[Abstract](288) [FullText HTML] [PDF 239KB](0)
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The behaviour of water in H2O-CHCl3-CCl4 system is studied.by 1H NMR method.Water is thought to exist in the form of H2O, H2O·CHCl3, (H2O)2 and (H2O)2·CHCl3 in the system.The formation constants for the species of H2O·CHCl3, (H2O)2 and (H2O)2·CHCl3 evaluated from NMR data are 1.56, 15.3 and 18.5 (mole fraction) respectively.
γ-IRRADIATION ON THE CHLOROSULFONATED POLYETHYLENE
Li Shuzhong , He Zhongda , Yang Jinrong , Zhang Jie
1989, 6(3): 75-77
[Abstract](298) [FullText HTML] [PDF 205KB](0)
Abstract:
The effect of radiation dose on the gel content of chlorosulfonated polyethylene (CSM) has been investigated. The results indicated that with the same radiation dose the more the chlorine content in CSM, the easier was the CSM to be crosslinked. IR spectra study showed the importance of CCl group in CSM in radiation crosslinking.The presence of the antioxidants depressed the oxidation of CSM during irradiation. The tensile strength. and the elongation of the polymer increased with increasing radiation dose when the latter was low. A maximum value of the tensile strength appeared at about 110 kGy. It is also found that γ-irradiation in dose of 60-300 kGy showed no effect on the glass transition temperature and dielectric property of CSM.
SILICA GEL SUPPORTED POLYETHYLENE GLYCOLS FOR PHASE TRANSFER CATALYSIS
Kang Ruhong , Fan Fengge , He Yanzhang , Zhang Lanping
1989, 6(3): 78-80
[Abstract](358) [FullText HTML] [PDF 200KB](0)
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Polyethylene glycols with different mean molecular weight (200-1000) were immobilizedon to silica gels. They all exhibited a certain catalytic activity in esterification and some nucleophilic substitution reactions. The influence of the chain length of polyethylene glycol,the dosage of catalyst used and the polarity of the solvents on the catalytic activity were studied. The catalysts could be used repeatedely seven times with little loss of its activity.
DERIVATIVE OSCILLOGRAPHIC POTENTIOMETRIC TITRATION Ⅱ. TITRATION OF Cu2+ BY DPTC- ON PLATINUM ELECTRODE
Liu Xiaohua , Zhang Wenbin , Gao Hong
1989, 6(3): 81-83
[Abstract](463) [FullText HTML] [PDF 174KB](0)
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The results of determination of cupric ion in synthetic and superconductor samples by DDTC- on platinum electrodes using derivative oscillographic potentiometric technique proves the simplicity and rapidity of the method proposed by the authors.
FACTOR ANALYSIS AND FOURIER TRANSFORM INFRARED SPECTRA OF BLEND OF POLY(n-OCTADECANYL METHACRYLATE) AND POLY(VINYL ACETATE)
Shi Mingxiao , Lin Xianfu , Liu Min , Huang Aihua , Jin Gang , Chen Yaozu
1989, 6(3): 84-86
[Abstract](271) [FullText HTML] [PDF 211KB](0)
Abstract:
The number of components in the blend of poly(n-octudecanyl methacrylate)(P n-OMA) and poly(vinyl acetate) (PVA) was determined by factor analysis and FTIR spectrophotometry. The results indicated that it is a compatible system.Three peaks between 1600cm-1 and 1800cm-1 in the (P n-OMA)/PVA system,which correspond to carbonyl group of (P n-OMA) PVA and the interaction of (P n-OMA) with PVA respectively, were revealed by leastsquare curve-fitting (peak resolving) method.The interaction spectrum was used to analyze the blend system for the magnitude of the interaction as a function of composition.The maximum interacticn was at 60wt% of (P n-OMA).
EFFECT OF SOLVENTS ON THE SYNTHESIS OF POLYACETYLENE FILM
Wang Daike , Zhao Xiaojiang , Wang Fosong
1989, 6(3): 87-89
[Abstract](276) [FullText HTML] [PDF 321KB](8)
Abstract:
Acetylene polymerized by a heat aged mixture of Ti(OBu)4-AlEt3 in various solvents (alkane and aromatic hydrocarbon)yields a high performance polyacetylene film (HPPA).Being doped with iodine, the films showed an electrical conductivity of 103 S/cm at room temperature. The value was over 104 S/cm after stretching of the film. The HPPA films were high compact and stable in air and composed of relatively ordered piling up of fibrils.Its apparent density and permeability of N2 were 0.80g/cm3 and 3.2×1011 Jcm3(STP)/cm2·s·cmHg,respectively. The results of IR, TEM and X-ray diffraction indicated that the films were high crystalline and had 65-85% of cis-PA and 20-100 nm of fibre diameter.
ON THE WATER SOLUBILITY OF PARTLY N-ACYLATED CHITOSANS
Chen Tian , Yan Jun , Xu Rongnan , Xia Yan
1989, 6(3): 90-92
[Abstract](345) [FullText HTML] [PDF 193KB](0)
Abstract:
A series of partly N-acylated chitosans was prepared and their solubility and water sorption were studied. It was found that N-acetyl, N-propionylchitosan (degree of acylation 55%), N-butyrylchitosan (degree of acylation 50%) dissolve fairly in water. The X-raydiffraction intensity curve of the water-soluble N-acetylchitosan showed that it was almost amorphous.
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