1998 Volume 15 Issue 6

Constitution and Structure of the Colored Passive Films of W-S Cluster Compounds on Steel Surface
Li Daohua , Ye Xiangrong , Zhou Yiming , Xin Xinquan
1998, 15(6): 1-5
[Abstract](654) [FullText HTML] [PDF 209KB](0)
Abstract:
Colored W-S cluster compound films as decorative and anticonosive layers were coated on strrl surface by immevsing in W S42- solution. The results of FT-IR, F-IR, FT-Ra-man, APS and AES analyses showed the existence of W-S-Fe, terminal W-S and terminal W-O bonds in the cluster films. The films were composed of the elements W, S, Fe and O. The valences of these elements are found to be +6, +6 (+4), +3, -2 in the surface, and +6 (+4), -2, +2, -2 in the internal layer of the films, respectively. A multimolecular layer structure of the films has been verified. The relative atomic percent contents and the thickness of the films were calculated at the constant elemental composition section on the AES profile curves. The longer the reaction time, the thicker the films. On heating at 250 ℃ in air for 2 hours the structure and distribution of the elements changed, while the composition and valence state of the elements in the films remained unchanged.
Effect of Adsorption of Surfactants and Polyvinylpyrrolidone on the Stability of ZrO2 Suspension
Zhao Zhenguo , Qian Cheng , Wang Qing , Liu Yingqing
1998, 15(6): 6-10
[Abstract](495) [FullText HTML] [PDF 209KB](0)
Abstract:
The adsorption of sodium dodecylbenzene sulfonate(SDBS), tetradecyl pyridine bromide(TPB) and polyvinyl pyrrolidone(PVP) onto the ZrO2 particles in aqueous solutions and the effect of the adsorption on the stability of ZrO2 suspension have been studied. The results show that the isotherms are of LS type for SDBS at pH2.4 and of S type for TPB at pH 7.0, respectively. The adsorption isotherms for both surfactants are roughly identical with potential changecurves of ZrO2 particles:at maximum adsorption ZrO2 has greater potential value and the adsorbed surfactant ions form surface micells with more parts of their hydrophilic groups being towards water phase, increasing the stability of ZrO2 suspension. The amount of PVP adsorbed on the positively charged ZrO2 is greater than that on the negatively charged ZrO2. In concentrated PVP solution the ZrO2 suspension has higher stability.
Regeneration of Spent Industrial NiMo/γ-Al2O3 Catalysts for HDS
Su Jixin , Xiao Tiancun , Wang Haitao , Lu Yuli , Zhou Changli , Li Shuben , Zhang Kongyuan
1998, 15(6): 11-15
[Abstract](494) [FullText HTML] [PDF 206KB](0)
Abstract:
The hydrodesulfurization(HDS) catalytic activity of spent industrial catalyst Ni-Mo/V-Al2O3 can be regenerated through oxidation below 723 K, calcination in air at 753 K for 3 h, and reduction at 673 K in H2 for 2 h and oxidation at 723 K in air for 4 h successively. The activity for HDS of some regenerated samples can even be higher than that of the fresh catalyst sample.
Phase Behaviour of Core-Shell Type Polyacrylate- Polyurethane Microemulsion Cast Films
Dong Anjie , Feng Shiyou , Wan Tong , Sun Duoxian
1998, 15(6): 16-20
[Abstract](384) [FullText HTML] [PDF 197KB](0)
Abstract:
The phase separation of the core-shell type polyacrylate-polyurethane cast films has been studied by mechanodynamic test, IR and DSC methods. The results indicated that the existence of hydrogen bondings between acetone C=O in the core and - NH in the shell improves the phase separation of the soft and hard segments in the shell, and also improves the compatibility of the core and shell, breaking the short range order of the hard segments.
Inhibition Mechanism of Imidazoline Amide in CO2 Solution
Zhang Xueyuan , Ma Limin , Du Yuanlong , Cao Dianzhen
1998, 15(6): 21-24
[Abstract](436) [FullText HTML] [PDF 167KB](0)
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The inhibition mechanism of imidazoline amide(IM) in CO2 solution has been studied by electrochemical techniques including electrochemical impedance spectrum and polarization result measurements. It is shown that the inhibition of IM is due to the negative catalytic effect on the iron. Its adsorption obeyed the Langmuir isotherm. The positive shift over to adsorption potential is the main reason of desorption of IM on the anode, which increases the interface capacity and decreases the transmission resistance.
Application of Functional Electropolymerized m-Phenylene Diamine Membrane in Immunosensor Analysis
Chen Ruichuan , Lu Fang , Li Donghui , Zhang Changgong , Wan Zhen
1998, 15(6): 25-28
[Abstract](426) [FullText HTML] [PDF 167KB](0)
Abstract:
An electropolymerization method of m-Phenylene diamine membrane, polyphenylene diamine(PMPD) on the surface of graphite electrode is described. To identify the quality of the membrane, a rapid and sensitive method has been established based on the reaction of a horseradish peroxidase(HRP) labeled PMPD with orthophenylene diamine. An antiHBsAg and an anti-MIgG immunoelectrodes were prepared for detecting hepatitis B surface antigen(HBsAg) and mouse immunoglobin G(MIgG). The optimum membrane preparation conditions are polymerization:0.12 mol/L MPD solution in 1.2 mol/L H2SO4 for 20 min under 2.5 V, activation:with 3% glutiraldehyde for 4 h. The prepared HRP labeled electrode and immunoelectrodes possessed good repetition. Catibration graphs were linear for HBsAg in ranges from 0.1~3.2μg/mL and 0.1~2.0μg/mL for MIgG/mL.
Synthesis and Insecticidal Activity of Silicon- containing Asymmetric Thiophosphates and Their Carbon Analogues
He Zhengjie , Li Zhengming , Wang Youming , Yang Zhiqiang , Qian Baoying
1998, 15(6): 29-32
[Abstract](413) [FullText HTML] [PDF 163KB](0)
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Two series of silicon-containing asymmetric thiophosphates have been synthesized to investigate their insecticidal activity. The carbon analogues of one series of the silicon compounds have also been prepared. Their 1H, 31P NM R spectra and insecticidal activities are discussed.
Water-Soluble and Amphiphilic Polymers 22.Influence of Acrylic Acid/Vinyl Acetate Copolymer on the Morphology of CaSO4 Precipitate
Liu Jingyu , Jiang Shichun , Wang Zhigang , Han Ping , Xu Suxian , Fang Tianru
1998, 15(6): 33-36
[Abstract](374) [FullText HTML] [PDF 179KB](0)
Abstract:
Presence of title copolymer in the aqueous solution of Na2SO4 and CaCl2 not only decreases the amount and crystallization rate of CaSO4 precipitate, but also markedly reduces its particle size and changes its morphology and crystal form.
Effects of Dopped Phosphorus on Carbon Anodes Property
Wu Yuping , Fang Shibi , Jiang Yingyan , Wan Chunrong
1998, 15(6): 37-40
[Abstract](593) [FullText HTML] [PDF 166KB](2)
Abstract:
The effects of incorporation of phosphoric acid on the carbonaceous materials have been investigated. Results of elemental analysis, XPS and XRD measurements show that phosphorus is in bond with carbon and oxygen atoms. At 600 ℃, the incorporated phosphoric acid favors the cyclization, dehydrogenation and carbonization processes and both the nitrogen content and graphene nitrogens relative contents are increased. The bondage state of phosphorus leads the interlayer distance d002 of carbon material to increase and the reversible capacity below and above 0.9 V increase with the amount of added phosphoric acid with the total value being up to 524 mAh/g. At 1000 ℃, the carbonization degree is not much changed and the reversible capacity at about 1.0 V increases as a result of the incorporation of phosphorus atoms.
Effect of In2O3 Doping on the Gas Sensitivity of ZnFe2O4
Chu Xiangfeng , Liu Xingqin , Meng Guangyao
1998, 15(6): 41-44
[Abstract](440) [FullText HTML] [PDF 168KB](0)
Abstract:
In2O3 has been doped in ZnFe2O4 by a chemical coprecipitation method. XRD results showed that in doped system there is no new phase formed and only a little change in lattice constants. Doping of In2O3 decreased the conductivity of ZnFe2O4 sensor, changed its conduction mechanism and increased its response to C2H5OH.
Chiral Recognition of D/L-Tyrosine by β-Cyclodextrin and Synthesis of Supramolecular Inclusion Compound
Zhang Youming , Wei Taibao
1998, 15(6): 45-48
[Abstract](370) [FullText HTML] [PDF 163KB](1)
Abstract:
The chiral recognition action of U-cyclodextrin(U-CD) to D/L-tyrosine(D/L-tyr) have been studied by circular dichroism measurement. The solid supramolecular inclusion compound of U-CD with L-tyr has been prepared and characterized by elemental analysis, thermal analysis, thin-layer chromatography and X-ray diffraction analysis. The inclusion equilibrium constants were obtained approximately by fluorescence spectrophotometry. The results indicated that U-CD showed a higher affinity for L-tyr than for D-tyr and it formed a 11 host-guest compound with L-tyr of constitution L-tyr/U-CD° 12H2O. The formation constant is calculated to be 5.13 × 103 mol-1° L. The inclusion compound had a more or less greater thermal stability than tyrosine and U-CD.
Study of Pd-Cu/MoO3-SiO2 Catalyst for Partial Oxidation of Ethane to Ethene by CO2
Li Qing , Zhong Shunhe , Shao Yu
1998, 15(6): 49-52
[Abstract](448) [FullText HTML] [PDF 168KB](0)
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Chemisorption combined with IR spectrometry and TPD and microreactor techniques have been used to investigate the adsorption activation and partial oxidation reactivity of CO2 and CO2H6 on title catalyst. It is found that CO2H6 is chemisorbed on the surface of the catalyst through H of its C-H bond and terminal O of Mo=O bond. For the adsorption of CO2 on the catalyst besides the linear type and the scissors type there appears another horizo-ntal type. The lattice oxygen of the catalyst is found to play an important role in partial oxidation. A mechanism of partial oxidation is proposed.
Synthesis of Di(Tri) benzyltin Unsaturated Alkylphosphates
Yin Handong , Zhang Rufen , Ma Chunlin
1998, 15(6): 53-56
[Abstract](421) [FullText HTML] [PDF 162KB](0)
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Ten noval di (tri) benzyltin unsaturated alkylphosphates with general formula[(PhCH2)n Sn]n-1 O2 P(O)R(n=2,3; R=-C≡CPh, -C≡CC5H11-n, -C≡CCH2OCH3, -C≡CC H2O C2H5, CH=CClPh) were synthesized and characterized by elemental analysis, IR, 1H NMR and TG-DTA measurements. Some of the compounds exhibited better miticidal and fungicidal activities.
Cyclization Modification in Course of Cis-polymerization of Butadiene Initiated by Rare Earth Catalyst
Wang Chaoyang , Yang Jihua , Dong Weimin , Pang Shufen
1998, 15(6): 57-60
[Abstract](375) [FullText HTML] [PDF 161KB](0)
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Butadiene was polymerized to some extent in the presence of binary catalyst system NdCl3° 3i-PrO H-AlEt3 in toluene and the allylchloride was then added to the solution in order to cyclize the formed polybutadiene and cyclopolymerize the unreacted butadiene monomers. Influ-ences of the amount of rare earth catalyst, molar ratio of allylchloride to AlEt3, cyclization reaction time and temperature, and concentration of the monomers on the cyclization reaction have been investi-gated. The microstructures of the end polymers have been characterized by IR and 1H NMR measurements.
Synthesis of Perhalogenated Pyrene by Plasma Reaction
Xie Suyuan , Zhang Qiang , Huang Rongbin , Zheng Lansun
1998, 15(6): 61-64
[Abstract](435) [FullText HTML] [PDF 163KB](1)
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A series of perhalogenated aromatic compounds were synthesized by arc-discharging of solid polytetrafluoroethylene and glow-discharge of chloroform vapor, respectively. Among the products, perchloropyrene(C16Cl10) and perfluoropyrene (C16F10) were separated and charac-terized. The features of the plasma reaction and product formation mechanism have been discussed. The products of the plasma reaction are normally a series of compounds with similar structure. Their formation appeared not to be affected by the compositions or structures of the reagents, as well as the discharge conditions.
Synthesis and Characterization of Diazoresin with 2-Diazo-1-naphthaquinone-5-sulfonic Anion as Counterion
Cao Weixiao , Yang Lei
1998, 15(6): 65-67
[Abstract](524) [FullText HTML] [PDF 126KB](1)
Abstract:
The title diazoresin has been synthesized which involves two kinds of photosensitive groups:diazonium and 2-diazo-naphthaquinone. The photochemical and thermal properties of the resin has been investigated preliminarily. The results show that the resin possesses photosensitivity as well as high thermal stability. The resin film undergoes structural conversion from linear to crosslinking under UV irradiation.
Synthesis and Spectral Analysis of Ruthenium Complexes with Phenathroline Derivatives
Shi Jianjun , Lü Weixing , Wang Huaibing , Gao Jianfeng
1998, 15(6): 68-70
[Abstract](423) [FullText HTML] [PDF 128KB](0)
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The synthesis and spectral characteristics of the title coordination compounds are reported and discussed.
The Photosensitivity and Nonlinear Optical Properties of a Charge-Transfer Salt Based on Tungstosilicic Acid
Niu Jingyang , Wang Jingping , Dang Dongbin , Bo Yan
1998, 15(6): 71-73
[Abstract](396) [FullText HTML] [PDF 129KB](0)
Abstract:
A charge-transfer salt exhibiting photosensitivity and nonlinear optical property has been synthesized from tungstosilicic acid and N-methylpyrolidone and characterized by elemental analysis and IR spectrometry. The photosensitivity of the compound has been studied by diffuse reflectance electronic spectrometry and ESR measurement. The nonlinear optical property of the compound is determined by powder method. The results show that electron can be transfered between organic species and the anion under light irradiation. The compound exhibits the second- and third- order nonlinear optical properties. The third-harmonic generation intensity and the third-order susceptibility of the compound measured by second-harmonic generation technique relative to a KDP crystal were estimated to be I=0.85 I KDP and i(3)=36 × 10-12 esu, respectively.
Preparation of Oxygen Evolution Electrode from Spinel NiCo2O4 by Composite-Plating Technique
Cai Naicai , Zhang Keli , Yuan Jibing , Liu Yong , Sun Jutang
1998, 15(6): 74-76
[Abstract](488) [FullText HTML] [PDF 132KB](0)
Abstract:
The Ni-NiCo2O4 composite electrodes for oxygen evolution were prepared by composite electroplating technique. In the course of plating the particles of spinel NiCo2O4/(ca. 4μm) were easily co-deposited on the nickel deposited electrode forming a high rough Ni-NiCo2O4 composite plating layer. The Ni-NiCo2O4 composite electrodes exhibited low oxygen overvoltage and good stability and had two Tafel slopes smaller than that of pure Ni plating electrode.
On the Crystallinity of Syndiotactic Polypropylene
Yu Yingning , Zhang Hongfang , Mo Zhishen , Chen Wei , Sun Chunyan
1998, 15(6): 77-79
[Abstract](500) [FullText HTML] [PDF 130KB](0)
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A formula for calculating the crystallinity of syndiotactic polypropylene samples synthesized by metallocene catalyst with constant syndiotacticity has been derived on the basis of W AXD intensity and the graphic resolution method. The calculated by this formula values have been compared with those obtained by DSC and density measurements. They all give a maximum value at Tc(95℃) of the polymer, while the calculated values are more or less higher.
Crystallization and Melting Behavior of Polycaprolactam/poly(ether sulfone) Blends
Zhang Zhimin , Chen Guifen , Wang Guibin , Jiang Zhenhua , Ma Rongtang
1998, 15(6): 80-82
[Abstract](353) [FullText HTML] [PDF 129KB](0)
Abstract:
A series of polycaprolactam(PA6)/poly(ether sulfone)(PES) blends were prepared in a Brabenderlike apparatus and the effect of PES on crystallization and melting behavior of PA6 has been investigated by DSC technique. The melting temperature and nonisothermal crystallization temperature of PA6 decreased with increase of weight fraction of PES in blends. Three melting peaks were found in DSC isothermogram. The Avrami exponents varied between 3.2 and 3.7, almost irrespertive of Tc and composition, and the rate of crystallization decresed with increase of temperature and PES content.
Stability of High Water Content Emulsion Membrane
Xu Guocai
1998, 15(6): 83-85
[Abstract](461) [FullText HTML] [PDF 140KB](0)
Abstract:
Emulsive plastes were prepared with high NH4NO3 aqueous solution as dispersion phase and polyisobutylene succinimide emulsifying agene as continuous phase. The stability of oil membrane of the plastes has been examined in organic dispersing agents and moving water, respectively. The oil membrane was found to be more stable in cyclohexane, paraffin oil and acidic moving water than in alkaline moving water.
On the Degradation of Starch/Polyethylene Blends
Yu Jiugao , Li Hansheng , Gao Jianping , Lin Tong
1998, 15(6): 86-88
[Abstract](535) [FullText HTML] [PDF 135KB](1)
Abstract:
The influences of environmental temperature, humidity and oxygen concentration on the mechanical properties, viscosityaverage molecular weight, hydroperoxide concentration and micrograph of starch/polyethylene blends have been investigated. The results revealed an acceleration effect of starch on the degradation of polyethylene.
Fluorescence Spectrometric Study on the Suppression of Ge-132 on Maillard Reaction of Phenylalanine
Chen Ji , Ma Genxiang , Li Xiaojing , Zhang Shugong , Li Deqian
1998, 15(6): 89-91
[Abstract](528) [FullText HTML] [PDF 132KB](0)
Abstract:
It has been observed that λem of phenylalanine and glycosylated phenylalanine in fluoresce spectra are 281.0 nm and 440 nm, respectively, that permits to investigate the suppression of Ge-132 on the Maillard reaction of phenylalanine without any interference. The result shows that the fluorescence intensity(FI) of glycosylated phenylalanine increases continuously with the decrease of FI of phenylalanine, and Ge-132 exhibits a suppression on the Maillard reaction of phenylalanine up to 42.3%.
Preparation of Nanocrystalline SnO2
He Yunpu , Li Yadong , Li Longquan , Yu Juan , Qian Yitai
1998, 15(6): 92-93
[Abstract](428) [FullText HTML] [PDF 102KB](0)
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Nanocrystalline SnO2 was prepared by hydrothermal hydrolysis of SnCl4 in NH3° H2O/polyglycol mixture at 150℃. IR, Raman spectrometry, XRD and TEM were used for their characterization. The results showed that a nonagglomerated and well dispersed SnO2 in average size of 3 nm was obtained.
Synthesis and Characterization of Poly(ether ether ketone ether ketone)
Qiu Zhaobin , Mo Zhishen , Yu Yingning , Zhang Hongfang
1998, 15(6): 94-95
[Abstract](562) [FullText HTML] [PDF 99KB](1)
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4,4'-Bis(fluorobenzoyl)diphenyl ether was prepared and polycondensed with hydroquinone to give a PEEKEK. The polymer has been characterized by IR, DSC, TGA and WAXD methods. It has the same crystal structure as PEEK and also a good thermal stability. The Tg, Tm and thermal decomposition temperatures(weight loss=5%) were found to be 134℃, 315℃ and 510℃, respectively.
Characterization of a Heterocyclic Containing Poly(aryletherketone) Copolymer
Liu Yanjun , Chen Lianzhou , Jian Xigao , Zhu Xiuling
1998, 15(6): 96-97
[Abstract](390) [FullText HTML] [PDF 98KB](0)
Abstract:
A novel poly(aryletherketone) copolymer containing phthalazinone moiety was prepared by nucleophilic substitution reaction of 4-(4-hydroxyphenyl)(2H) phthalazin-1-one with bis-1,4-(4-chlorobenzoyl) benzene(BCBB) and 4,4'-difluorobenzophenone(DFPK). The copolymer has been studied by FTIR, DSC, TGA and X-ray diffractometry. It is an amorphous plastics with Tg=245~254℃ and good thermal stability, and the Tgs of the copolymer were increased with decreasing of molar ratio of BCBB to DFPK. The copolymer is soluble in aprotic dipolar solvents.
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