2002 Volume 13 Issue 4

Insertion of Selenium into Zinc Carbon Bond and Application in Synthesis of Arylselenoester
Xin Hua XU , Wen Qi LIU
2002, 13(4): 283-284
[Abstract](519) [FullText HTML] [PDF 652KB](1)
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Selenium was inserted into the zinc carbon bond of aryl zinc halides to form corresponding zinc selenoates.They reacted in THF-HMPA with acylhalides to afford the selenoesters in high yields.
One-Pot Reaction of Aldehydes,α-Haloketones and (Phenylsulfonyl)acetonitrile Promoted by SmI3
Xue Sen FAN , Yong Min ZHANG
2002, 13(4): 285-286
[Abstract](502) [FullText HTML] [PDF 639KB](3)
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One-pot reaction of aldehydes,α-haloketones and (phenylsulfonyl)acetonitrile promoted by SmI3 proceeded smoothly to give 1-cyano-1-phenylsulfonyl-2-aryl-3-aroyl-propane derivatives in moderate to good yields.
The Rearrangement of 2-Benzothiazolylthioacetyl Hydrazide in Synthesis of s-Triazolo[3,4-b]benzothiazole-3-thiol
Yan ZHANG , Ren Zhong QIAO , Chao Feng DAI , Peng Fei XU , Zi Yi ZHANG
2002, 13(4): 287-289
[Abstract](510) [FullText HTML] [PDF 1061KB](2)
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The rearrangement reaction of 2-benzothiazolylthioacetyl hydrazide 1 with potassium hydroxide and carbon disulfide in ethanol to produce s-triazolo[3,4-b]benzothiazole-3-thiol 3 was described.3 also can be obtained from 2-benzothiazolylhydazine 2 and the two methods for getting 3 were compared.Mannich reaction of compounds 3 was reported too.
Synthesis of 6(E)-Geranylgeraniol-19-oic Acid
Shu Hua LI , Wei Dong LI , Yu Lin LI
2002, 13(4): 290-291
[Abstract](575) [FullText HTML] [PDF 670KB](1)
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Facile synthesis of 6(E)-geranylgeraniol-19-oic acid 1,a naturally occurring alicyclic diterpene acid,by a Horner-Wadsworth-Emmons olefination of two readily available fragments 2 and 3,is described.
Synthesis of 5-Deoxy-5-Acyloxyiminoavermectin B1 Derivatives
Xi Guang LIU , Jing Ping WU , Xiao Mei LIANG , Dao Quan WANG
2002, 13(4): 292-293
[Abstract](493) [FullText HTML] [PDF 669KB](1)
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Four 5-deoxy-5-acyloxyiminoavermectin B1 derivatives 4a~d were synthesized via three steps from avermectin B1 and their biological activities were tested against Heliothis armigera,Laphygma exigua and Musca domestica.
Synthesis of a Novel Type of Glycophosphate Mimics
Qiang XIAO , Yong JU , Yu Fen ZHAO
2002, 13(4): 294-295
[Abstract](648) [FullText HTML] [PDF 674KB](0)
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A series of novel type of glycophosphate mimics are synthesized by Todd reaction and their structure were determined on the basis of NMR,ESI-MS.
A Convenient Synthesis of the Substituted 2,3-Diarylindole the Potent Selective COX-2 Inhibitors
Wen Hui HU , Zon Ru GUO , Ai Ping BAI , Zhi Bin XU
2002, 13(4): 296-298
[Abstract](609) [FullText HTML] [PDF 1120KB](7)
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Phenyl sulfone-containing 2,3-diarylindole derivatives were designed and identified to be selective COX-2 inhibitors.A convenient synthetic route was also developed for the synthesis of the novel inhibitors.
DNA Modification with Photochromic Spiro Compounds
Peng ZHANG , Ji Ben MENG , Teruo Matsuura , Yong Mei WANG
2002, 13(4): 299-302
[Abstract](574) [FullText HTML] [PDF 1349KB](4)
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The photochromic spiropyrans and spirooxazine having a succinimidyl ester or isothiocyanate pendant group can form covalent products with transaminated DNA. The absorption spectra and solid reflection spectra of modified DNA with these photochromic spiro compounds were investigated.
The Purification of Glucose Type Glycosyl Nitrate and the Synthesis of Spacer-armed N-Acetyllactosamines and Their Dimers
Qing LI , Hui LI , Bin SU , Xiang Bao MENG , Meng Shen CAI , Zhong Jun LI
2002, 13(4): 303-305
[Abstract](502) [FullText HTML] [PDF 1135KB](0)
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3,6-di-O-acetyl-4-O-(2,3,4,6-tetra-O-acetyl-β-D-galactopyranosyl)-2-azido-2-deoxy-β-D-glucoppyranosyl nitrate could be separated from its mannose type isomer by glycosylation according to the reactivity difference of these two compounds.The pure glucose type nitrate can be converted to corresponding trichloroacemidate,which reacted with spacer arms in solution of CH2Cl2 with BF3·Et2O as promoters to give desired glycosides and dimers.
Electrochemical Synthesis of Polythiophene in an Ionic Liquid
Jia Hua SHI , Xun SUN , Chun He YANG , Qing Yu GAO , Yong Fang LI
2002, 13(4): 306-307
[Abstract](501) [FullText HTML] [PDF 772KB](0)
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Polythiophene (PTh) was prepared by the direct electrochemical synthesis in an ionic liquid ([BMIM]PF6 containing 0.1 mol/L thiophene by cyclic voltammetry,constant potential and constant current techniques.It is found that smooth and blue-green PTh films can be obtained at a potential of ca.+1.75 V (vs.Ag/AgCl) or a current of ca.1.5 mA cm-2 in the ionic liquid.
Preparation of p-1,1,3,3-Tetramethylbutylphenol by Using Nafion-H Catalyst
Li Qin YOU , Guo Rong ZHENG , Ping LU
2002, 13(4): 308-310
[Abstract](579) [FullText HTML] [PDF 1043KB](1)
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p-1,1,3,3-Tetramethylbutylphenol was prepared by the alkylation of the phenol with Nafion catalyst in extremely high yield.Various reaction conditions were investigated,including the reaction temperature,reaction time,ratio of the starting material,amount of the Nafion catalyst and the recycle times of the catalyst.
Vapor-phase Nitration of Benzene to Nitrobenzene over Supported Sulfuric Acid Catalyst
Jing Lin CHEN , Wei Guo CHENG , Hong Feng LIU , Qing Song LIN , Lian Hai LU
2002, 13(4): 311-314
[Abstract](600) [FullText HTML] [PDF 1513KB](7)
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Vapor-phase nitration of benzene over solid acid catalyst is expected to be a clean process with no sulfuric acid waste.We investigated this process over solid acidic catalysts utilizing diluted nitric acid (60-70%) as nitrating agent,and found that supported sulfuric acid catalyst exhibited a very high catalytic activity.Under the conditions of reaction temperature 160-170℃,space velocity (SV) 1200 h-1,the yield and the space-time yield (STY) of nitrobenzene (NB) based on HNO3 were more than 98% and 0.75 kg·kgcat-1·h-1 over 10% H2SO4/SiO2 (by weight) catalyst respectively.
Asymmetric Polymerization of Menthyl Methacrylate by Anionic Catalysts
Yong An XU , Hong XUE , Lian Xun GAO , Meng Xian DING
2002, 13(4): 315-316
[Abstract](470) [FullText HTML] [PDF 673KB](0)
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In this paper,(-)menthyl methacrylate((-)MnMA) was polymerized at-78℃ in toluene with three types of anionic catalysts,which were complexes of fluorenyllithium with (-)sparteine-((-)-Sp) ,(S,S)-(+)-2,3-dimethoxy-1,4-bis(dimethylamino)butane((+)DDB) and N,N,N',N'-tetra-methylethylenediamine(TMEDA),and the chiral optical property of the obtained polymer was studied.The circular dichroism (CD) spectrum of the polymer showed negative Cotton effect
Preparation and Cyclic Voltammetry Characterization Of Cu-dipyridyl Imprinted Polymer
Yi Ning ZENG , Ning ZHENG , Peter G. OSBORNE , Yuan Zong LI , Wen Bao CHANG , Zong Mu WANG
2002, 13(4): 317-320
[Abstract](496) [FullText HTML] [PDF 1708KB](0)
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Polymer capable of specific binding to Cu-dipyridyl complex was prepared by molecular imprinting technology.The binding specificity of the polymer to the template (Cu-dipyridyl complex) was investigated by cyclic voltametric scanning using the carbon paste electrode modified by polymer particles in phosphate buffer solution.Factors that influence rebinding of the imprinted polymer were explored.The result demonstrated that the cyclic voltammetry was an efficient approach to explore interactions between template and imprinted polymers.
A Novel Oligosaccharide from the Mucus of the Loach
Chuan Guang QIN , Kai Xun HUANG , Hui Bi XU
2002, 13(4): 321-324
[Abstract](534) [FullText HTML] [PDF 1718KB](1)
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A novel oligosaccharide was isolated and purified from the mucus of the loach,Misgurnus anguillicaudatus.It was identified by several qualitative tests and characterized by elementary analysis,UV and IR spectrum.Its average molecular weight (Mw=1539.4) was determined by gel permeation chromatography.The major structural monomers of Misgurnus anguillicaudatus oligosaccharide were identified to be D-galactose and L-fucose by paper chromatography and gas chromatography.
A New Ceramide from the Ascomycete Tuber indicum
Jin Ming GAO , An Ling ZHANG , Chen Ying WANG , Xiang Hua WANG , Ji Kai LIU
2002, 13(4): 325-326
[Abstract](538) [FullText HTML] [PDF 701KB](5)
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A new C-18 phytosphingosine derivative (1) was isolated from the fruiting bodies of Tuber indicum. Its structure was established as (2S, 3S, 4R, 2'R)-2-N-(2/-hydroxytricosano-yl)-octadecan-l, 3,4-triol by spectral and chemical methods.
A New Polyphenolic Compound from Rubus aleaefolius and Its Inhibitory Activity on Mammalian Cell Cycle at G0/G1 Phase
Cheng Bin CUI , Qing Chun ZHAO , Bing CAI , Xin Sheng YAO , Hiroyouki OSADA
2002, 13(4): 327-330
[Abstract](510) [FullText HTML] [PDF 1434KB](1)
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Rubuphenol (1),a new polyphenolic compound,was isolated together with the known ellagic acid (2) as new cell cycle inhibitors from Rubus aleaefolius Poir.through a bioassay-guided separation procedure and the structure of 1 was elucidated by spectroscopic method.Compounds 1 and 2 inhibited the cell cycle of tsFT210 cells at the G0/G1 phase respectively with the MIC values of 14.6μM and 10.3μM.
Huperzine W,a Novel 14 Carbons Lycopodium Alkaloid from Huperzia serrata
Chang Heng TAN , Xiao Qiang MA , Guo Fu CHEN , Shan Hao JIANG , Da Yuan ZHU
2002, 13(4): 331-332
[Abstract](727) [FullText HTML] [PDF 587KB](2)
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Huperzine W,a novel 14 carbons Lycopodium alkaloid,was isolated from the whole plant of Huperzia serrata,and its stucture was determined by spectroscopic analysis.
Saluenolide A,A Novel Eremophilanolide from Senecio saluenensis
Yu ZHAO , Peng WANG , Simon PARSONS , David W. H. RANKIN , FranÇise GUÉITTE , Thierry SEVÉET , Hong YU , Yi Neng HE , Xiao Jiang HAO
2002, 13(4): 333-334
[Abstract](572) [FullText HTML] [PDF 638KB](1)
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From Senecio saluenensis,a novel eremophilanolide Saluenolide A was isolated.Its structure was elucidated by 2D-NMR technique and X-ray diffraction.
Two New Xanthone Glycosides from Polygala tenuifolia
Yong JIANG , Peng Fei TU
2002, 13(4): 335-336
[Abstract](560) [FullText HTML] [PDF 835KB](4)
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Two new xanthone glycosides,polygalaxanthone Ⅳ and Ⅴ were isolated from the roots of Polygala tenuifolia Willd.Their structures were established as 6-O-[(α-L-rhamnopyranosyl-(1→2)-β-D-glucopyranosyl]-1-hydroxy-3,7-dimethoxyxanthone (polygalaxanthone IV),and 6-O-[α-L-rhamnopyranosyl-(1→2)-β-D-glucopyranosyl]-1,3-dihydroxy-7-methoxyxanthone (polyga-laxanthone Ⅴ),respectively,on the basis of chemical and spectral evidence.
Two New C-glucoside Flavonoids from Leaves of Crataegus pinnatifida Bge.var.major N.E.Br.
Pei Cheng ZHANG , Sui Xu XU
2002, 13(4): 337-340
[Abstract](555) [FullText HTML] [PDF 1213KB](1)
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Two new C-glucoside flavonoids,namely 8-C-β-D-(2"-O-acetyl) glucofuranosyl apigenin and 3"-O-acetylvitexin,were isolated from leaves of Crataegus pinnatifida Bge.var.major N.E.Br..Their structures were elucidated by the spectroscopic means and chemical evidence.
A New Limonoid from the seed of Aphanamixis polystachya
Hua Ping ZHANG , Shao Hua WU , Xiao Dong LUO , Yun Bao MA , Da Gang WU
2002, 13(4): 341-342
[Abstract](519) [FullText HTML] [PDF 673KB](2)
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A new limonoid named rohituka-15 1,with a known limonoid dregeana-1 2,was isolated from the seed of Aphanamixis polystachya (Meliaceae).The 13C NMR data assignment of dregeana-1 2 and the structural elucidation of the new compound 1 were based on spectral analysis including 1H-1H COSY,HMQC and HMBC experiments.
Sesquiterpene Lactones from Elephantopus scaber
Qiao Li LIANG , Zhi Da MIN
2002, 13(4): 343-344
[Abstract](522) [FullText HTML] [PDF 681KB](0)
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A new germacranolide sesquiterpene lactone,isoscabertopin,was isolated from Elephantopus scaber together with the known scabertopin.Their structures were determined by spectroscopic methods.
Two New Pentacyclic Triterpenes from Sabia parviflora
Jin CHEN , Bin CHEN , Jun TIAN , Feng E WU
2002, 13(4): 345-348
[Abstract](502) [FullText HTML] [PDF 1096KB](0)
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Two new pentacyclic triterpene acids,1α,3β-dihydroxyl-olean-12-en-28-oic acid and 1α,2α,3β-trihydroxyl-olean-12-en-28-oic acid,were isolated from the arial parts of Sabia parviflora.
Liquid-liquid Extraction System Based on Non-ionic Surfactant-salt-H2O and Mechanism of Drug Extraction
Lei LI , Feng LIU , Xiang Xu KONG , Shun SU , Ke An LI
2002, 13(4): 349-350
[Abstract](510) [FullText HTML] [PDF 769KB](1)
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Extraction behavior of chlorpromazine hydrochloride (CPZ) and procaine hydro-chloride (PCN) in the system described in the title was studied.Research shows that the extraction efficiency of CPZ can amount to 96% by twice extraction,while that of PCN is 77%.This system produces the distribution coefficients (KD) of 12.3 and 2.6 respectively for CPZ and PCN.Extraction mechanism is deduced according to ultraviolet and molecular fluorescence spectra variation of the drugs in the system studied.
Impedance Characterization of Adsorption Process of Calmodulin on Au Substrate and its Combination with Ca2+
Ke Qiang DING , Zhen Bin JIA , Qing Fei WANG , Juan BAI , Ru Ting TONG , Xin Kui WANG , Hui Bo SHAO
2002, 13(4): 351-354
[Abstract](504) [FullText HTML] [PDF 1421KB](0)
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In this paper,the adsorption process of calmodulin (CaM) on Au substrate was first investigated with electrochemical impedance spectroscopy (EIS) method.The result reveals that the adsorption of the protein-calmodulin contains two steps,i.e.,one short quick step followed by a slow one.The complexation of calmodulin with Ca2+ was also first probed using EIS technique,in which the complexation of CaM with Ca2+ could be reflected by the change of apparent membrane capacitance(Capp) clearly.In all above measurements,a redox couple Fe(CN)63-/ Fe(CN)64- was used as probing-pin to reflect all the changes occurring in the above process.Our work suggests that some biological processes of CaM could be studied using EIS method conveniently.
A Method of Determining Selectivity Coefficients Based on the Practical Slope of Ion Selective Electrodes
Hai Xia WANG , Min PU
2002, 13(4): 355-358
[Abstract](590) [FullText HTML] [PDF 1426KB](9)
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It is a problem to be solved that the experimental selectivity coefficients of ion selective electrodes (ISEs) depend on the activity.This paper studied the new method of determining selectivity coefficients.A mixed ion response equation,which was similar to Nicolsky-Eisenman (N-E) equation recommended by IUPAC,was proposed.The equation includes the practical response slope of ISEs to the primary ion and the interfering ion.The selectivity coefficient was defined by the equation instead of the N-E equation.The experimental part of the method is similar to that based on the N-E equation.The values of selectivity coefficients obtained with this method do not depend on the activity whether the electrodes exhibit the Nernst response or non-Nernst response.The feasibility of the new method is illustrated experimentally.
Density Functional Studies of the Reaction of Ytterbium Monocation with Fluoromethane: C-F Bond Activation and Electron-Transfer Reactivity
Dong Ju ZHANG , Cheng Bu LIU
2002, 13(4): 359-362
[Abstract](627) [FullText HTML] [PDF 1474KB](0)
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The potential energy surface and reaction mechanism corresponding to the reaction of ytterbium monocation with fluoromethane,which represents a prototype of the activation of C-F bond in fluorohydrocarbons by bare lanthanide cations,have been investigated for the first time by using density functional theory.A direct fluorine abstraction mechanism was revealed,and the related thermochemistry data were determined.The electron-transfer reactivity of the reaction was analyzed using the two-state model,and a strongly avoided crossing behavior on the transition state region was shown.The present results support the reaction mechanism inferred from early experimental data and the related thermochemistry data can provide a guide for further experimental researches.
Quantitative Structure-Property Relationship on Prediction of Surface Tension of Nonionic Surfactants
Zheng Wu WANG , Gan Zuo LI , Jian Hai MU , Xiao Yi ZHANG , An Jing LOU
2002, 13(4): 363-366
[Abstract](577) [FullText HTML] [PDF 1442KB](10)
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A quantitative structure-property relationship (QSPR) study has been made for the prediction of the surface tension of nonionic surfactants in aqueous solution.The regressed model includes a topological descriptor,the Kier & Hall index of zero order (KH0) of the hydrophobic segment of surfactant and a quantum chemical one,the heat of formation (ΔHf) of surfactant molecules.The established general QSPR between the surface tension and the descriptors produces a correlation coefficient of multiple determination,r2=0.9877,for 30 studied nonionic surfactants.
Bonding and Mössbauer Isomer Shifts in (Tl,Pb)-1223 Cuprate
Fa Ming GAO , Dong Chun LI , Yan Zhi WANG , Yong Jun TIAN , Min Zi CHEN , Si Yuan ZHANG
2002, 13(4): 367-370
[Abstract](505) [FullText HTML] [PDF 1322KB](0)
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By using the chemical bond theory of dielectric description,the chemical bond parameters of (Tl,Pb)-1223 was calculated.The results show that the Sr-O,Tl-O,and Ca-O types of bond have higher ionic character and the Cu-O types of bond have more covalent character.Mössbauer isomer shifts of 57Fe and 119Sn doped in (Tl,Pb)-1223 were calculated by using the chemical environmental factor,he,defined by covalency and electronic polarizability.Four valence state tin and three valence iron sites were identified in 57Fe,and 119Sn doped (Tl,Pb)-1223 superconductor.We conclude that all of the Fe atoms substitute the Cu at square planar Cu (1) site,whereas Sn prefers to substitute the square pyramidal Cu (2) site.
Semidifferential Electroanalysis of Aqueous Triton X-100/Toluene/H2O Microemulsion
Chun Sheng MO , Zhen Zhong HUANG , Ming Hua ZHONG
2002, 13(4): 371-374
[Abstract](508) [FullText HTML] [PDF 1524KB](1)
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Semidifferential electroanalysis is used as an effective method for investigating microstructure and structural transition of Triton X-100 microemulsions.
Synergetic Effects of UV/Fe3+ Combined with Electrocatalysis for p-Nitrophenol Degradation
Ming Hua ZHOU , Zu Cheng WU , Da Hui WANG
2002, 13(4): 375-378
[Abstract](519) [FullText HTML] [PDF 1634KB](2)
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Synergetic effects for p-nitrophenol degradation were observed in the combination of two-advanced oxidation processes,UV/Fe3+ and electrocatalysis.The enhancement of removal rate for p-nitrophenol and COD was around 123% and 278%,respectively.The possible contributions for the synergetic effects were the electrochemically regeneration of ferric ion and the role of the oxygen that formed on the anode.
Highly Efficient Photosensitization of Mesoporous TiO2 Electrode with a Cyanine Dye
Yan Jie REN , Fan Shun MENG , He TIAN , Sheng Min CAI
2002, 13(4): 379-380
[Abstract](536) [FullText HTML] [PDF 736KB](1)
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A low cost cyanine dye,1,1-dimethyl-3-ethyl-2-[3-(1,3-dihydro-3,3-dimethyl-1-ethyl-5-carboxyl-2H-indol-2-ylidene)-1-propenyl]-1H-benz[e] indolium iodide (1) was synthesized and applied to sensitize mesoporous TiO2 electrode.Photoresponse of the electrode was extended to the visible and remarkably high incident photon-to-current conversion efficiency (IPCE) over 70% was achieved from 500 nm to 600 nm.
Carbon Nanotubes Grown on Sepiolite as Catalyst Carrier
Ji Peng CHENG , Jiang Ping TU , Ying YE , Yan Lin SUN , Fu LIU , Yue Sheng NING , Fan Zhi KONG , Huan Ming LU , Xiao Bin ZHANG
2002, 13(4): 381-384
[Abstract](571) [FullText HTML] [PDF 1192KB](0)
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Multi-walled carbon nanotubes were synthesized by the catalytic decomposition of acetylene at 750℃ over sepiolite powder,which was treated with aqueous cobalt nitrate.It is expected that the composite with high specific area will have high capacity of hydrogen storage.
Synthesis of Nanosized NaY Zeolite by Confined Space Method
Bo WANG , Hong Zhu MA , Qi Zhen SHI
2002, 13(4): 385-388
[Abstract](1723) [FullText HTML] [PDF 1476KB](8)
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Nanosized NaY crystals have been prepared from metakaolin and sodium silicate by confined space synthesis with starch additive.It is found that the product has a narrow crystal size distribution (50-100 nm),high Si/Al ratio (Si/Al=4.6-6.1),high surface area (1090 m2/g) and the average diameter of nanosized NaY (75 nm) synthesized is 30 nm,it is smaller than that of without starch additive.
Synthesis of NiFe2O4 Powders Well Defined in Size and Morphologies
Yu Ting ZHAO , De Hong CHEN , Dai Rong CHEN , Xiu Ling JIAO
2002, 13(4): 389-392
[Abstract](500) [FullText HTML] [PDF 1207KB](0)
Abstract:
The uniform NiFe2O4 powders with different particle size and morphologies (octahedral,cubic and spherical) have been prepared from different precursors via hydrothermal process.The nanocrystallines derived from precursor B in the weak alkali solution (pH≤10) are superparamagnetic.
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