2001 Volume 18 Issue 1

Studies on Synthesis,Magnetic Resonance and Biological Activity of Lanthanide Complexes with Noncyclic Polyether-Histidine Schiff Base
LU Gui , YAO Ke-Min , ZHANG Zhao-Ying , SHEN Lian-Fang
2001, 18(1): 1-4
[Abstract](298) [FullText HTML] [PDF 138KB](1)
Abstract:
Five lanthanide complexes with tetraglycol aldehyde bis-histidine Schiff base were synthesized and characterized by elemental analysis, IR spectrometry, TG-DTA and magnetic susceptibility as Ln3(H2L)2(NO3)9(Ln=La,Nd,Gd,Er,Yb; L=C20H26N6O7). The obtained complexes were investigated in detail by high resolution solid state(HRSS) 13C NMR using cross polarization,magic angle spinning(CP/MAS)and total suppression of sidebands(TOSS) techniques. Some new information about the splitting peaks of 13C-for-COO- group are given. On the basis of them,the coordination of imidazole group was discussed. The crystal field strength of the Gd(Ⅲ) complex was investigated by EPR spectrometry. The experimental results show that Er3+ complex has some biological activities and could dispose of O2·-.
Study on the Substitution and Moisture-Retention Capacity of Carboxymethyl Chitosan
CHEN Ling-Yun , DU Yu-Min , XIAO Ling , QIN Cai-Qin
2001, 18(1): 5-8
[Abstract](851) [FullText HTML] [PDF 141KB](1)
Abstract:
A series of N,O-carboxymethylchitosan(CM-chitosan) were prepared. The position and degree of substitution were determined by potentiometric titration, IR and 13C NMR. The results indicated that the degree of substitution of the compounds increased significantly with decrease of molecular weight of chitosan and the carboxymethylation reactivity decreased in the order OH-6 >OH-3 >NH2. The moisture-absorption and moisture retentio-properties of CM-chitosans and moisture-retention properties of CM-chitosans were found quite similar to those of hyaluronic acid. The moisture absorbability increased with increasing in molecular weight and moisture retention capacity of CM-chitosas with the degree of substitution. The CM-chitosans with molecular weight from 0.56×104 to 8.6×104 and degree of substitution greater than 1.0 had better moisture-absorption moisture retention capacity than hyaluronic acid.
Study on the Polymerization with Organic/Inorganic Hybrid-Supported Titanium Catalysts Ⅱ.Styrene Polymerizaton
ZHU Ning , TANG Tao , CHEN Hui , YU Guang-Qian , FENG Zhi-Liu , HUANG Bao-Tong
2001, 18(1): 9-11
[Abstract](372) [FullText HTML] [PDF 111KB](1)
Abstract:
The use of organic/inorganic hybrid materials poly(styrene-co-maleic anhydride)/SiO2 as the support for titanium catalysts in styrene polymerization was studied. Results indicated that at 70℃ the activity of the inorganic/organic hybrid supported catalysts would reached a maximum; 1.49×106 g/(mol·h). With increase in reaction temperature, the molecular weight of polymer decreased, and the polydispersity was much wider. DSC and FTIR measurements showed that the product was syndiotatic polystyrene.
Study on the Free Radical Graft Copolymerization of Maleic Anhydride onto Poly(β-hydroxybutyrate)
CHEN Cheng , PENG Shu-Wen , FEI Bin , AN Yu-Xian , ZHUANG Yu-Gang , DONG Li-Song , FENG Zhi-Liu
2001, 18(1): 12-15
[Abstract](394) [FullText HTML] [PDF 145KB](1)
Abstract:
The graft copolymerization of maleic anhydride(MA) onto poly(U-hydro-xybutyrate) (PHB) using benzoyl peroxide as initiator was studied. The effects of polymerization conditions on graft degree,including solvents, monomer and initiator concentrations, reaction temperature and time,were investigated. The best reaction conditions were described. The results showed that graft degree of MA onto PHB could be controlled in the range from 0.3% to 0.85%. The grafted PHB was characterized by 13C NMR and chemical titration of MA group.
Laser Stimulated Selective Oxidation of i-Butane to Methacrylic Acid over Mo4V6O24
TAO Yue-Wu , ZHONG Shun-He
2001, 18(1): 16-20
[Abstract](196) [FullText HTML] [PDF 200KB](1)
Abstract:
A Mo/V complex oxide was prepared from (NH4)6Mo7O26·4H2O and NH4VO3 by a coprecipitation method. The surface composition, structure, chemsorption and behavior of laser stimulated selective oxidation of isobutane have been investigated by XRD, IR, TPD and microreactor. The results showed that the main phase of the complex oxide is Mo4V6O24, which has a storeyed structure composed of MoO3 and V2O4. There are both Lewis base sites, O2- in the surface Mo=O or Mo-O-V bonds, and Lewis acid site, V4+ appeared on the surface of complex oxide. Two methyl hydrogens in isobutane molecule can be chemisorbed on the terminal oxygen of the neibouring Mo=O bonds on the surface of the complex oxide. Under the conditions of 0 1 MPa, 200℃ and 1000 times of laser excitation with 972 cm-1 on the Mo=O bonds, about 6.5% isobutane were converted to isobutene, methyl propenal and methacrylic aicd, among them 78% were the latter. A mechanism is proposed for isobutane selective oxidation.
Electrochemical Properties and Catalytic Activity of Undecatungstomaganosilicate Isomers
MA Rong-Hua , LUI Chun-Tao , WANG Shou-Guo , QU Lun-Yu
2001, 18(1): 21-24
[Abstract](430) [FullText HTML] [PDF 135KB](1)
Abstract:
Synthetic method and electrochemical properties of undecatungstomanganosilicate isomers T-and,Ui-Kn H6-n[SiW11Mn(H2O)O39xH2O (Ui=U1,U2,U3) are reported. The effect of structure on the redox has been investigated. The order of polarographic half-wave potential E1/2 of heteropoly anions as follows: U2 >U1 >U3 >To in epoxidation of maleic acid with H2O2 is U3(87.86%) >U1(82.50%) >T(64.20%) >U2(56.10%).
The XPS and TPR Characterization of Sulfur-resisted Catalysts for Water Gas Shift Promoted by K2CO3
LIN Ren-Cun , YANG Yi-Quan , YUAN You-Zhu , WEI Guang , WANG Qi , FAN Jin-Hong , DAI Shen-Jun
2001, 18(1): 25-28
[Abstract](387) [FullText HTML] [PDF 146KB](1)
Abstract:
The XPS, TPR techniques were used to study the promotion effect of K2CO3 to the supported catalyst Co-Mo-K-O/V-Al2O3 for water gas shift. The XPS results show that the amount of low valence molybdenum and S2- increases with increase of the content of K in sulfured catalyst, and (S-S)2- is suppressed. It is found that keeping the ratio (Mo4++Mo5+)/Mo6+ at 0.8~1 level and remaining more S2- species on the catalyst are in favor of the improvement of the catalytic activity at low temperature. Two hydrogen adsorped peaks of TPR, namely T and U peaks, which can be ascribed to Mo6+→Mo5+ and Mo5+→Mon+(n=4,3,2) reduction processes respectively, appear both at sulfured state and functioning state. The experiment results indicate that there is a close relation between the altitude of the peaks and the activity of the catalyst at low temperature.
Preparation of 2-Hydroxyl-1,4-naphthoquinone by Catalytic Oxidation of Naphthol over Iron Porphyrin
YAN Yan , ZHENG Guo-Dong , CHEN Yu-Qin , ZHEN Kai-Ji , FANG Chi-Guang , WANG Ao , LI Qing , CHANG Xin
2001, 18(1): 29-31
[Abstract](317) [FullText HTML] [PDF 107KB](1)
Abstract:
The 2-hydroxyl-1, 4-naphthoquinone(HNQ) was prepeared by catalytic oxidation of 1-naphthol and/or 2-naphthol in NaOH methanol solution with H2O2 over 5,10,15,20 tetra(4-methoxyl)phenyl porphyrin iron chloride in yield of 57% and purity of 95%. The UV-Vis, IR, NMR, MS, mp determination and elemental analysis were used for characterization. A spectro photometric method was proposed for quantitative analysis of HNQ using λmax=452 nm.
Preparation of TiO2/SnO2 and Photocatalytic Degradation of Dichlorvos over It
LI Xiao-Hong , YAN Yiu-Ru , ZHANG Yue-Ping , HUO Ming-Liang , GUO Wei-Wei
2001, 18(1): 32-35
[Abstract](487) [FullText HTML] [PDF 155KB](1)
Abstract:
Nanoparticles of SnO2 coated with TiO2 have been prepared from Ti(OC4H9)4 and SnCl4·5H2O as precursors by an activated surface method. Their morphology and structures were investigated by IR, XRD, TEM and BET. The results indicated the nanometer TiO2/SnO2 was composed of anatase TiO2 and rutile SnO2. The TiO2/SnO2 showed a better catalytic activity than SnO2 and TiO2 alone in photocatalytic degradation of dichlorvos.
Preparation of TiO2/glass Film by Sol-gel Method and There with Photocatalytic Degradation of Rhodamine B
ANG Ya-Juan , LI in , WEi Pei-Hai , ZHANG Yan-Chang , FENG Xu-Sheng , YANG Kong-Zhang
2001, 18(1): 36-39
[Abstract](521) [FullText HTML] [PDF 144KB](2)
Abstract:
TiO2/glass films have been prepared by a sol-gel method with titanium tetrabutoxide as precursor. XRD and XPS results indicate the film is composed of anatase phase and with TiO2 size of about 15~25 nm. Triboloyical study indicates the TiO2 film has a long antiwearing life. The TiO2/glass film shows a high catalytic activity in photodegradation of rhodamine B in aqueous solution. The photodegradation follows first order kinetics and its reaction rate can be expressed by Langmuir Hinshewood equation.
Study on the Structure of Fluoropolymer Hybrid Electrolytes
WANG Guo-Jie , PAN Hui-Ming , HUANG Jing
2001, 18(1): 40-43
[Abstract](449) [FullText HTML] [PDF 165KB](1)
Abstract:
Hybrid polymer electrolytes were prepared from poly(vinylidene fluoride-co-hexafluoropropylene) and LiClO4 by two methods:melting-rolling method and solution casting impregnation method. Both two thus prepared hybrid polymeric electrolytes with the same electrolyte solution content, 72.5%(mass fraction) of 1 mol/L LiClO4 in ethylene carbonate/propylene carbonate (1:1 volume ratio), exhibited high ionic conductivity 1×10-3 S/cm at room temperature. The XRD, SEM, DSC and TGA demonstrated that the first method gave homogeneous structure of polymeric electrolyte, in which the liquid electrolyte has great interaction with polymer matrix and the samples obtained by 2nd method are microporous, where liquid electrolyte solution shows less influence on the matrix structure. Samples prepared by the 1st method have better solution retention property than samples from 2nd method.
Dynamic Mechanical Property of Styrene-Butadiene Rubber/Natural Rubber Composite
XU Wen-Zong , HAO Wen-Tao , MA De-Zhu , LIANG Li
2001, 18(1): 44-47
[Abstract](439) [FullText HTML] [PDF 133KB](1)
Abstract:
The dynamic mechanical properties of blends of natural rubber respectively with three kinds of styrene butadiene rubbers, two solution polymerized styrene-butadiene rubbers:SSBR(B), SSBR(C) and an emulsion polymerized styrene-butadiene rubber:ESSA have been investigated. The results showed that SSBR(B) had characteristic chain structure and the SSBR/NR composite showed a good compatibility and low heat generation under pressure.
Application of FTIR in Study of Thermo-oxidative Degradation of PE/Starch Blends
YU Jiu-Gao , WANG Xiao-Dong
2001, 18(1): 48-51
[Abstract](311) [FullText HTML] [PDF 134KB](1)
Abstract:
The crystalline parameters of PE/starch blends have been evaluated by FTIR as a function of thermo-oxidative aging time. It is found that the relative error is not more than 10% in comparison with that obtained from XRD measurement. FTIR technique is also tested to estimate the mass change of starch in degradation.
Ionic Conductive Property of Polyurethane/Oligo-polyether Sulfate Complexes
YANG Bing , HE Yin , WANG Lei , TANG Xiao-Zhen
2001, 18(1): 52-55
[Abstract](378) [FullText HTML] [PDF 144KB](1)
Abstract:
An oligo-polyether sulfate(SPEO) was prepared from polyethylene oxide and HClSO3 and a series of solid polymer electorlytes, complex of oligo-polyether sulfate with polyether-polyurethane, were prepared using polydioxolane as a plasticizer. FT IR, 1H NMR and complex impedance analysis were used to characterize the samples. The effects of temperature, salt concentration and plasticizer on the ionic conductivity of the complexes were investigated. The ionic conductivity was not of Arrhenius type in relation with temperature and it increased with increase of oligo polyether sulfate. At the same molar ratio of ether unit to Na+ the ionic conductivity of PU/SPEO600 was higher than that of PU/SPEO400. The highest ionic conductivity of the complexes was 10-5 S/cm at 60℃. The plasticizer polydioxolane had great effect on the ionic conductivity.
Synthesis of Biologically Active Dipeptide in a Multiphase Enzyme Membrane Reactor
JIANG Zhong-Yi , JIA Qi-Peng , LIU Jia-Qi , CHEN Hong-Fang
2001, 18(1): 56-58
[Abstract](267) [FullText HTML] [PDF 105KB](1)
Abstract:
A multiphase enzyme membrane reactor using aqueous-organic biphase instead of water phase alone as the reaction medium was employed to investigate the lipase-catalyzed synthesis of bioactive dipeptides. The medium effect on dipeptide yield was first studied. When N-acetyl-L-phenylalanine ethyl ester(APEE) was used as a carboxyl component, the reactivity order of amino acid amides was found to be L-Leu-NH2 >L-Val-NH2 >L-Ala-NH2 >L-Gly-NH2. The didpetide, N-Ac-L-Phe-L-Leu NH2, could be synthesized in the multiphase enzyme membrane reactor in a high yield and purity due to the simultaneous separation and reaction.
Fourier Transform Infrared Photoacoustic Spectra of Transition Metal Complexes of Meso-tetra-(4-lauroyloxyphenyl)porphyrin
LIU Wei , SHI Tong-Shun
2001, 18(1): 59-61
[Abstract](306) [FullText HTML] [PDF 105KB](1)
Abstract:
The fourier transform infrared photoacoustic spectra of meso-tetra-(4-lauroyloxyphenyl)porphyrin(TLPPH2) and its complexes with Mn (Ⅲ)、Fe (Ⅲ)、Co (Ⅱ)、Ni (Ⅱ)、Cu (Ⅱ) and Zn (Ⅱ) in the range of 3600~190 cm-1 were measured and investigated. The bands at 3318 and 968 cm-1 of TLPPH2 are due to the N-H stretching and in-plane and out of plane bending vibration of the pyrrole groups. All these bands disappear upon complex formation. The vibration coupling between the M-N stretching and the porphyrin ring deformation appears at 250 cm-1. Metal sensitive bands were found at 1354、1018、983、796、736、632、231 cm-1.
Synthesis of Aminoiminomethanesulfonic Acid
PAN Zhi-Xin
2001, 18(1): 62-63
[Abstract](389) [FullText HTML] [PDF 74KB](1)
Abstract:
The title compound in monohydrate was prepared from aminoiminomethanesulfinic aicd by H2O2 oxidation in aqueous sulfuric acid solution. The compound is unstable in moisture, especially in acid atmosphere.
Synthesis and Thickening Efficiency of Acrylamide-Octadecyl Acrylate Copolymer
HUANG Xue-Hong , XU Guo-Qiang , XU Chen
2001, 18(1): 64-66
[Abstract](433) [FullText HTML] [PDF 105KB](1)
Abstract:
The radical copolymerization of acrylamide(AM) with octadecyl acrylate(OA) has been carried out in DMF at 80℃ using benzoyl peroxide as initiator. The copolymers were characterized by DMTA and Kjeidahl nitrogen determination. The effects of copolymer composition, amount of initiator, reaction temperature on the thickening efficiency of copolymer towards emulsion based on styre nebutyl acrylate-acrylic acid polymer have been investigated. The results showed that the molecular weight of poly(AM-co-OA) obtained was big enough for hydrophobic associative thickening agent.
Synthesis and β-Hydrogen Elimination of Alkoxo Complexes of Tungsten
REN Jian-Guo , WANG Zi-Wei , ZHANG Zhi-Min , LIU Dian-Sheng , Minato Makoto , Ito Takashi
2001, 18(1): 67-69
[Abstract](343) [FullText HTML] [PDF 106KB](1)
Abstract:
Four alkoxo tungsten complexes[Cp2W(PMe3)OR]+ OTs-(R=Me,Et, n-Pr, i-Pr) and monohydrido tungsten complex[Cp2W(H)(PMe3)]+ OTs- were synthesized and characterized by IR, 1H NMR and elemental analysis. The U-elimination of these complexes in dimethyl sulfoxide solvent yields monohydrido tungsten complex[Cp2W(H)(PMe3)OR]+ OTs- and a ketone or aldehyde.
Synthesis of Hydrotalcite by Hydrothermal Method
XIE Hui , JIAO Qing-Ze , DUAN Xue
2001, 18(1): 70-72
[Abstract](714) [FullText HTML] [PDF 123KB](1)
Abstract:
The double-layered hydroxide with hydrotalcite structure was prepared by a hydrothermal method from two mixtures:MgSO4·7H2O with Al2(SO4)3·18H2O and NaOH with Na2CO3. It is found that increasing the ageing temperature and ageing time of the hydrothermal process was favorable for the formation of hydrotalcite structure, and the crystal size of the products could be controlled by varying ageing temperature and time.
Poisoning and Oxygen Adsorption of CuO/Al2O3 Catalyst
FENG Ru-Bin , YAO Hong-Wei
2001, 18(1): 73-75
[Abstract](384) [FullText HTML] [PDF 113KB](2)
Abstract:
The effect of CuSO4 on the property of catalyst CuO/Al2O3 has been investigated. The TPD-MS results showed that the amount of oxygen adsorbed on the surface of CuSO4-CuO/Al2O3 increased with CuSO4 content in the catalyst and the oxygen desorbed only at temperature above 900 K. TPSR results showed three adsorption sites of NO on the surface of CuO/Al2O3, respectively at 398, 643 and 683 K. The active site at 683 K was for NO decomposition and it was poisoned seriously when there was CuSO4 in the CuO/Al2O3. For CuSO4-CuO/Al2O3 the amount of N2O formed from NO decomposition reduced probably due to the increase of oxygen species in the catalyst.
Preparation of β-NiOOH and Its Charge/Discharge Performance
XIA Xi , PAN Ren
2001, 18(1): 76-78
[Abstract](328) [FullText HTML] [PDF 109KB](1)
Abstract:
U-NiOOH was prepared by chemical oxidation of U-Ni(OH)2. The physical characteristics and the chemical composition of the product were characterized by XRD, TG/DTA and ICP measurements. U-NiOOH and the mixed samples of U-NiOOH with V-MnO2 in different ratios were charged/discharged in constant current, the results show that the addition of V-MnO2 improves the discharge voltage plateau of nickel electrode and the optimum ratio of V-MnO2 in the electrode is 25%. The cut off voltage of nickel electrode should be above 0V(vs.Hg/HgO).
Determination of Multinuclear Aromatic Hydrocarbons in Coke Oven Smoke
SHANG Qing-Kun , XIANG Qian , ZHU Hong , YAN Ji-Chang , ZHU Dong-Xia
2001, 18(1): 79-80
[Abstract](304) [FullText HTML] [PDF 80KB](1)
Abstract:
The smoke sample from the Angang Iron-Steel Company's coke oven has been analysed by GC/MS. Thirty-two multinuclear aromatic hydrocarbon compounds have been detected and twenty of them are world accepted as focal poisonous.
Fe1/2Al1/2PO4 Catalyst for Preparation of Propylene Oxide from 1,2-Dichloropropane
ZHONG Shun-He , GU Xiu-Jun , LI Xing-Bo , XIAO Xiu-Fen
2001, 18(1): 81-83
[Abstract](329) [FullText HTML] [PDF 123KB](1)
Abstract:
The title catalyst was prepared by the sol-gel method. The surface composite, structure, specific area and catalytic behavior have been investigated by IR, BET, XRD, TEM techniques. The results showed that the catalyst is an amorphous composed of FePO4 and AlPO4 with specific area about 238 m2/g and average granule size less than 10 nm. Under proper reaction conditions the conversion of 1,2-dichloropropane was more than 64% and the selectivity to propylene oxide was more than 79%.
Synthesis of Novel 3-Anilinemethylene-5,6-dihydro-6-phenyl-2H-pyran-2,4-diones
JIA Qiang , LI Zheng-Ming , JIANG Lin , ZHAO Wei-Guang , WANG Su-Hua
2001, 18(1): 84-86
[Abstract](287) [FullText HTML] [PDF 108KB](1)
Abstract:
We have previously reported the preliminary fungicidal activity of 3-anilinemethylene-5,6-dihydro-6-phenyl-2H-pyran-2,4-diones and their 3D-QSAR study. In this paper, sixteen novel compounds of this series are obtained in satisfactory yields (87%~97%) by using a new "one pot" synthetic method. The Z/E isomer relation of compounds (2) is discussed briefly.
Address:Zhongguancun North First Street 2,100190 Beijing, PR China Tel: +86-010-82449177-888
Powered By info@rhhz.net