2001 Volume 18 Issue 6

Synthesis and Biological Activity of 1-Sulfonyl-3, 5-diamino-1H-Pyrazole Derivatives
ZHAO Wei-Guang , CAO Yi-Bing , LI Zheng-Ming , GAO Fa-Wang , WANG Su-Hua , WANG Jian-Guo
2001, 18(6): 423-427
[Abstract](225) [FullText HTML] [PDF 219KB](1)
Abstract:
1-sulfonyl-3,5-diamino-1H-pyrazole-4-nitriles (3) were synthesized by the reaction of sulfonylation of 3,5-diamino-1H-pyrazole-4-nitriles (2), which were prepared from 2-cyano-3,3-dimethylthio acrylonitrile as starting material with arylamines. All the novel compounds were confirmed by 1H NMR and elemental analysis, and some by IR and MS. Some of the target compounds show excellent herbicidal activities.
Sol-gel Synthesis and Properties of Ce1-xCaxO2-x Solid Solutions
PENG Cheng , JIANG Kai , LI Wu-Ju , WANG Lin , WANG Hong-Yan , LIANG Hong-Wei , MENG Jian
2001, 18(6): 428-431
[Abstract](367) [FullText HTML] [PDF 190KB](1)
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A series of solid electrolytes, Ce1-xCaxO2-x(x=0~0.35), were prepared by sol-gel method. The relation of the crystal structure with the content of CaO was systematically investigated. XRD spectra showed that a pure fluorite phase was formed at 160℃. No phase was observed from room temperature to 800℃. The synthesis temperature in sol-gel method was significantly lower than in the traditional ceramic method and also lower than in the hydrothermal synthesis method. The purity of the product prepared by the sol-gel method is higher with the grain size uniformly smaller. They were easily sintered into highly dense ceramic pellets at 1300℃. XPS showed that the oxygen vacancy increased obviously by doping CaO, resulting in the increase of the oxygen ionic transport number and conductivity. Therefore, the performance of ceria-based solid electrolyte was improved.
In-situ FTIR Spectroscopic Study of Electrocatalytic Oxidation of CH3CH2OH on Sb Modified nm-Pt/GC Electrode
CHEN Guo-Liang , SUN Shi-Gang , CHEN Sheng-Pei , ZHOU Zhi-You
2001, 18(6): 432-435
[Abstract](262) [FullText HTML] [PDF 188KB](1)
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The electrochemical behavior of irreversibly adsorbed antimony on nm-Pt/GC have been studied by cyclic voltammetry and in-situ FTIR spectrometry. The results showed that the adatoms of Sb were stable on the surface of nm-Pt/GC when the scanning potentials were below 0.50 V(SCE). In comparison with the unmodified nm-Pt/GC electrode, the Sbad/nm-Pt/GC electrode manifested significant increase in catalytic activity for oxidation of ethanol, and the maximum activity was found when the coverage of Sbad was 0.137. The oxidation peak potential in this case negatively shifted to about 150 mV with peak current being double increased.
Stability and Rheological Property of Mg-Al-CO3 Dispersions
LI Lei , SUN Peng , DUAN Xue
2001, 18(6): 436-439
[Abstract](469) [FullText HTML] [PDF 196KB](1)
Abstract:
The stability and rheological property of the aqueous nanosized Mg-Al-CO3 LDH(n(Mg)/n(Al)=3) dispersions have been studied. It is found that the stability of the dispersions containing nano Mg-Al-CO3 LDH depends on both the solid content and the structure of the LDH and the stable aqueous LDH dispersion can be obtained without use of any dispersants. The rheological property of the aqueous LDH is in close relation with the layered structrue of the LDH. The shear-thinning of aqueous LDH dispersions is reversible and depends on the shearing time. The XRD analysis and SEM, TEM observations showed the existence of rod-shaped aggregates in the stable aqueous LDH dispersions.
Isolation of Anisole from Volatile Oil of Foemiculum Vulgare Mill by Crystalline Inclusion Method
CHANG Huai-Chun , YANG Chang-Chun , WANG Xiu-Mei , WANG Hong-Bo , TONG Jian , SU Chang-An , GUO Wen-Sheng , CAI Yun-Ping , MA Ming-Yang , CHENG Guang-Rong , LÜ Yang
2001, 18(6): 440-443
[Abstract](592) [FullText HTML] [PDF 187KB](1)
Abstract:
The chemical components of volatile oil from Foemiculum Vulgare Mill were determined by GC-MS, amomg them 82.65% were anisole. A selective isolation of anisole from the volatile oil from mentioned seed has been carried out by an inclusion method. 1,1,6,6-Tetraphenyl-hexa-2,4-diyne-1,6-diol(abbrv. DD) was used as a host molecule with anisole being as a guest molecule. The structure of the inclusion complex was characterized by IR, XRD, 1H NMR techniques and the host-guest molar ratio in complex was found to be 3:1. The anisole was isolated from inclusion complex by using Kugelrohr vacuum distillation technique and the isolated compound was characterized to be trans-anisole.
Effects of the Heat-Treatment of Carbon on Performance of the Oxygen Electrode for PEMFC
HUANG Cheng-De , TIAN Jian-Hua , SHI Jing-Shi , HAN Zuo-Qing , CHEN Yan-Xi
2001, 18(6): 444-446
[Abstract](262) [FullText HTML] [PDF 159KB](1)
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The effects of heat-treatment of carbon on the oxygen electrode for PEMFC were investigated. The particle size of Pt and the structure of carbon in the catalyst were measured by TEM and XRD. The results showed that the performance of the oxygen electrode was improved after heat-treatment of carbon. The reasons were attributed to the reduction in Pt size and conductivity of the carbon black.
Thermal Stability and Decomposition Kinetics of Some Metalloporphyrins
XU Hai , YU Dao-Yong , WANG Zong-Xian , Que Guo-He
2001, 18(6): 447-449
[Abstract](532) [FullText HTML] [PDF 141KB](1)
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The thermal stability and thermal decomposition kinetics of four metalloporphyrins: Ni-OEP, VO-OEP, Ni-TPP, VO-TPP(OEP:2,3,7,8,12,13,17,18-octaethyl-21H,23H-porphine; TPP:5,10,15,20-tetraphenyl-21H,23H-porphine) have been investigated. The thermal stability order of the four metalloporphyrins in N2 is found to be: VO-TPP≈Ni-TPP> VO-OEP> Ni-OEP. The thermal decom position kinetics parameters of metalloporphyr ins are evaluated.
Synthesis of Antimony Tris(Thioethyl Carboxylates) as Thermal Stabilizers for Poly(vinyl chloride)
LIU You-Nian , SHU Wan-Gen , WANG Chun-Jiang , ZENG Dong-Ming , CHEN Qi-Yuan
2001, 18(6): 450-453
[Abstract](513) [FullText HTML] [PDF 170KB](1)
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A kind of thermal stabilizers for PVC antimony tris (thioethyl carboxylate) (Sb(SCH2CH2OOCR)3, (R:CnH2n+1, n=7,11,17), was synthesized from carboxylic acid, antimony trioxide and 2-mercapto ethanol in two steps using tetra-n-butyl titanate as catalyst and xylene as azeotropic solvent. The thermal stab ility time was about 8~40 min (at 200℃) when they were blended in 2% mass ratio in PVC. The thermal stability of tris (thioethyl stearate) was better than that of Ca-Zn complex stabilizers and lead complex stabilizers. It can match dibutyltin dilaurate. The stabilization mechanism of the stabilizers for PVC was disscussed briefly.
Separation and Analysis DHA from Isochrysis Galbana
LI Run , ZHANG Wan-Kuan , NI Hang-Sheng , DAI Jun-Biao , WANG Hong , ZHOU Chun-Yu
2001, 18(6): 454-456
[Abstract](917) [FullText HTML] [PDF 143KB](1)
Abstract:
Isochrysis galbana is used as a new source of DHA (docosahexaenoic acid). The fatty acid of Isochrysis galbana was extracted by a mixture of CH3Cl, CH3OH and H2O(1:2:0.8 in volume) and esterified by a mixture of BF3 and C2H5OH(1:3 in volume), respectively. The esterification degree was detected with silica gel thin films. The quantitative analysis for DHA was carried out by GC and GC/MS techniques using ethyl ester of C19 fatty acid as an internal standard. DHA in yield of 2.2% was obtained from algae isochrysis galbana.
Study on Supramolecular System of the Host CP66 with Naphthalene Derivatives
YIN Wei , ZHANG Xiu-Lian , ZHANG Mai-Sheng
2001, 18(6): 457-461
[Abstract](266) [FullText HTML] [PDF 217KB](1)
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The supramolecular systems of the host 1,8,22,29-tetra [8.1.8.1]-paracyclophane (CP66) with T-naphthol, U-naphthol, 2, 6-dihydroxyl naphthalene and 6,7-dihydroxyl naphthalen-2-sulfonic acid as guests have been studied by UV spectrometry, fluorescence probe and synchronous fluorimetry. The CP66 formed 1:1 stoichiometric supramolecular system for all naphthalene compounds. The complex formation reactions of CP66 with T-naphthol, 2,6-dihydroxyl naphthalene were enthalpy promoted, while the reactions of CP66 with U-naphthol and 6,7-dihydroxyl naphthalen-2-sulfonic acid were entropy promoted. The unchanged values of the constant Ks shows that the main contribution to the formation of supromolecular systems of the CP66 with 6,7-dihydroxyl naphthalene-sulfonic acid arises from the electrostatic attraction. The host CP66 is found to recognize the isomer of naphthol by using a fluorescence probe.
Electrochemical Redox Behavior of Ni Nanowire Electrode and Its Application to Catalysis of Electrooxidation of Ethanol
KONG Jing-Lin , XUE Kuan-Hong , HE Chun-Jian , SHAO Ying , CHEN Qiao-Ling , YAO Jian-Lin , XIE Yong , TIAN Zhong-Qun
2001, 18(6): 462-465
[Abstract](472) [FullText HTML] [PDF 194KB](1)
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The Ni nanowire electrodes were fabricated by using porous alumina as a template. The electrodes possess high redox current density, high discharge capacity and good redox reversibility in 1 mol/L KOH solution, showing its potential application as an excellent battery electrode. Experimental results also revealed its good catalytic activities for electrooxidation of ethanol in an alkaline medium.
Influence of Reactive Extruding Conditions on the Grafting Degree, Grafting Efficiency and Melt Flow Rate of PP-g-GMA
WANG Yong , YAO Zhan-Hai , SONG Yong-Xian , YIN Jing-Hua
2001, 18(6): 466-468
[Abstract](335) [FullText HTML] [PDF 144KB](1)
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The functionalization of polypropylene grafted with glycidyl methacrylate (GMA) through reactive extrusion is reported. The influences of the concentration of GMA and initiator dicumyl peroxide (DCP), reaction temperature and residence time of materials in the extruder on the grafting degree (Gd), grafting efficiency (Ge) and melt flow rate (MFR) were investigated. The results showed that the Gd of PP-g-GMA was in direct proportion to the loading level of GMA. And there was a very limited effect of the concentration of the initiator on the grafting degree. The proper processing temperature window of the reative extrusion was 195~230℃. When the residence time of materials in the extruder was over one minute the grafting degree kept constant. The MFR of PP-g-GMA was proportional to the concentration of initiator and inversely proportional to the loading level of monomer. There were very limited effects of both the residence time and extruding temperature on the MFR of PP-g-GMA and no obvious influence of the concentration of monomer and initiator, extruding temperature and residence time of material in the extruder on the grafting efficiency of PP-g-GMA.
Study on Diethylenetriamine Cured Epoxy Resin/Montmorillonite Nanocomposite
XU Wei-Bing , BAO Su-Ping , NIE Kang-Ming , HE Ping-Sheng
2001, 18(6): 469-472
[Abstract](457) [FullText HTML] [PDF 183KB](1)
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The organophilic montmorillonites with increased interlayer spacings were prepared from hydrophilic clay by cation exchange with trimethylcetyl ammonium bromide. The epoxy resin/diethylenetriamine/montmorillonite nanocomposites were prepared by casting and curing processes and the intercalation behavior of epoxy resin in the organophilic montmorillonite was investigated by XRD and DMTA methods. It is found that the nanocomposites obtained were intercalated upon curing with diethylenetriamine and the intercalation was independent of the curing conditions. The glass transition temperature from DMTA analysis revealed the glass transition temperature of the extragallery cured epoxy resin and was in relation to the curing temperatures. Addition of organophilic montmorillonite led to the disappearance of the T' peak of loss tangent of the nanocomposites.
Synthesis and Antiseptic Property of E-and Z-2'-(1-Imidazolyl)-O-(α-methyl-dichlorobenzyl)-2, 4-dichloroacetophenoxime Nitrate
LI Zai-Feng , LUO Fu-Ying
2001, 18(6): 473-476
[Abstract](340) [FullText HTML] [PDF 184KB](1)
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E-and Z-2'-(1-imidazolyl)-2,4-dichloroacetophenoxime isomers have been prepared starting from m-dichlorobenzene chloroacetyl chloride?imidazole by different feeding order in oximation and introduction of imidazolyl groups. T-Chloro-dichloroethlybenzene (ⅡA~Ⅱc) were synthesized from m-, p- and o-dichlorobenzene. And six E-and Z-target compounds were synthesized in yield 57.5%~64.5% by reactions of Ⅰ and Ⅱ, respectively. Their structures were characterizated by elemental analysis, IR and 1H NMR. The preliminary tests showed that the Z isomers of the title compounds had more or less higher antiseptic effect on the roting of rice roots.
Preparation of Cross-linking Cationic Starch and Its Decolorization Performance
JU Ben-Zhi , ZHANG Shu-Fen , YANG Jin-Zong
2001, 18(6): 477-480
[Abstract](255) [FullText HTML] [PDF 179KB](1)
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In the presence of lithium hydroxide solution (6%), the cross-linking cationic starch bearing quaternary amino groups was prepared via reaction of starch with glycidyl trimethyl ammonium chloride (GTA) by dry process. The effects of lithium hydroxide catalyst solution (6%), reaction temperature, reaction time, amount of water on reaction efficiency were studied and discussed briefly. Under conditions: starch 5.8 g,GTA 3 g, lithium hydroxide solution (6%) 2 g, reaction time 4 h, reaction temperature 70℃ and amount of water 24.6%, the product with 0.5 degree of substitution was obtained. The reaction efficiency was 83.3%. The results showed that the cross-linking cationic starch was an excellent decolorant for reactive dyes. When the dosage was 105 mg/L,the decolorization efficency on synthetic wastewater containing reactive red X-3B、reactive blue X-BR、reactive yellow KN-6G 100 mg/L was 99.1%、88.0%、95.5% respectively.
Effect of Element Electronegativity in Supporters on the Selectivity of Supported Rare Earth Catalysts
SHAN Cheng-Ji , ZHANG Cheng-Lin
2001, 18(6): 481-483
[Abstract](365) [FullText HTML] [PDF 140KB](1)
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Supported rare earth catalysts were made from Nd(O-i-Pr)3 and the halides, especially chlorides of the ⅠA and ⅡA groups, used as catalyst supporters, for studying the relationship between the composition of supporters and the selectivity of supported rare earth catalysts. It was found that the electronegativity of the ⅠA or ⅡA elements showed an obvious effect on the selectivity of the supported catalysts, i.e. the selectivity of the supported catalyst was increased with the increase in their electronegativity, as in the case of supported Ti-catalyst.This rule was also held as the supporters are magnesium halides.
Catalytic Synthesis of Acetals and Ketals over Dealuminated USY Catalysts
ZHANG Min , JIANG Xiao-Ping , WANG Qiong
2001, 18(6): 484-486
[Abstract](332) [FullText HTML] [PDF 146KB](1)
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The acetalization and ketalization of various aldehydes and ketones with alcohols by using dealuminated USY(ultrastable Y-type zeolite) as catalyst were studied. The influences of silica/alumina ratio in the catalyst, catalyst amount and reaction time on the reaction were investigated. It is showed that the dealuminated USY is a high active catalyst for acetalization and ketaliz ation and its high activity can be readily returned to original by heating at 500℃ for 5 hours.
Structure and Biological Activities of Alkaline Soluble Polysaccharide from Marasmius Androsaceus FR
BAI Ri-Xia
2001, 18(6): 487-489
[Abstract](668) [FullText HTML] [PDF 140KB](1)
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An alkaline soluble polysaccharide R-1 has been obtained by extraction with 2% NaOH from marasmius androsaceus FR. and purified by chromatography on Sepharose CL-4B and HPLC. The GC-MS analysis showed it appeared constructed from glucan. Through periodate oxidation, Smith degradation, methylated analysis and 13C NMR it revealed that R-1 has 1→3 Glc as main chain and 1→6 Glc as side chain. The inhibition percentage against S-180 tumor of R-2, which was obtained by elemination of its side chains, was 92.8%.
Microwave-promoted Extraction of Pt and Pd from Aqueous Biphase System of Polyethyleneglyol/(NH4)2 SO4 and the Non-isothermal Kinetics of Reaction
GAO Yun-Tao , WU Li-Sheng , WANG Wei
2001, 18(6): 490-492
[Abstract](314) [FullText HTML] [PDF 146KB](1)
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Microwave irradiation technique was used to promote the extraction processes of bromide complex anions of Pt(Ⅱ) and Pd(Ⅱ) from aqueous biphase system of polyethyleneglyol/(NH4)2SO4. The results showed that under microwave irradiation the distribution ratio of metals, extraction capacity and extraction ratio increased significantly as compared with conventional extraction technique. Under microwave irradiation the extraction ratio of Pt or Pd achieved 100.0% and 99.6%, respectively. The non-isothermal kinetics on the extraction reaction also approved the enhanced extraction rate.
Modification of TiO2 Nanoparticles by An Organic Dye PDS in Reverse Micelle System
FENG Lin , CHU Ying , LIU Jing-Lin , CHEN Yue , XU Li-Ping
2001, 18(6): 493-495
[Abstract](278) [FullText HTML] [PDF 135KB](1)
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The TiO2 nanoparticles were modified by phthalocyanine dinuclear sulphate (PDS). The results showed that a, the adsorption intensity of PDS in UV-Vis spectrum increased with increase in water content in [H2O]/[Surft.] ratio; b, in AOT/isooctane reverse micelle system the UV-Vis spectral peak intensity for PDS decreased, broadened and redshifted with increase in concentration of TiO2 in TiCl4 solution, and the fluorescence spectral intensity for PDS decreased and then gradually to quenching also with increase in TiO2 concentration.
Preparation of Insoluble Quaternary Ammonium Bactericides Based on Silica Gels
LI Feng-Yan , WANG Xie-Qing , CHEN Yong-Jun , LI Ben-Gao
2001, 18(6): 496-497
[Abstract](261) [FullText HTML] [PDF 99KB](1)
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The insoluble quaternary ammonium bactericide was synthesized in two steps using silica gel as a carrier. The silica gels first reacted with 3-chloropropyltrimethoxysilane to give an intermediate, the chloropropyl groups on which then reacted with dimethyl tetradceylamine to give the quaternary ammonium bactericides. The bactericidal rate of the product against heterotrophic bacteria was 99% as tested in vitro.
Synthesis and Characterization of Aminoglucose Complexes with Zinc(Ⅱ)、Iron(Ⅱ) and Copper(Ⅱ)
GUO Zhen-Chu , PENG Bin , HAN Liang , LIU Wu-Yang , YUAN Han-Zhen
2001, 18(6): 498-500
[Abstract](769) [FullText HTML] [PDF 147KB](1)
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The complexes of aminoglucose with zinc(Ⅱ)、 iron(Ⅱ) and copper(Ⅱ) were synthesized. Their compositions and structures were characterized by elemental analyses, IR, UV and 1H NMR spectra. Some physical properties and optical activities were measured. The coordination number of all complexes were found to be 4.
A Novel Method for Bromination of α-H in Alkylbenzenes
YI Bing , CHEN Hong-Biao , LIN Yuan-Bin , ZHAO Hong-Bin
2001, 18(6): 501-503
[Abstract](336) [FullText HTML] [PDF 136KB](1)
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A novel bromination method for T-H in alkylbenzenes using KBrO3/NaHSO3 as bromination agent and under an incandescent light illumination is reported. The method has advantages of mild reaction condition, simple operation, high utilization of bromine and avoidance of the erosive HBr gas. For some alkylbenzenes, especially some alkylbenzenes with a second substituent in benzene ring, the method provides brominated products of high yield and purity only at temperature usually of 50~55℃ under light illumination.
Property and Structure of a Single-component Anionic Polyurethane Emulsion
LUO Qiang , CHENG Ying-Hua , XIU Yu-Ying
2001, 18(6): 504-506
[Abstract](279) [FullText HTML] [PDF 142KB](1)
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A single-component anionic polyurethane emulsion has been prepared from polyepoxyglycol, tolylene diisocyanate, dimethoxypropionic acid and ethylene diamine via prepolymeration route. The effects of the molecular weight of polyether polyol, the ratio of isocyanate group to hydroxy group and the amount of dimethylolpropionic acid on the property of the PU film and its physical property have been investigated.
Synthesis of Nefedipine by Wicrowave Treatment
TU Shu-Jiang , MA Heng-Jun , DENG Xu , YAO Chang-Sheng
2001, 18(6): 507-508
[Abstract](317) [FullText HTML] [PDF 99KB](1)
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The Nefedipine has been synthesized by reaction of m-nitrobenzaldehyde, ethyl acetoactate and ammomiun acetate under microwave irradiation without solvent. The reaction is completed in 4 min with 82% yield.
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