1999 Volume 16 Issue 1

Post-metallocene, New Late Transition Metal and Nonmetallocene Catalysts for Olefin Polymerization
Jin Guoxin , Zhou Guangyuan , Liu Changkun , Huang Baotong
1999, 16(1): 1-5
[Abstract](831) [FullText HTML] [PDF 202KB](20)
Abstract:
A new family of homogeneous, late transition metal catalysts based on iron(Ⅱ), cobalt(Ⅱ), nickel(Ⅱ)and palladium (Ⅱ) complexes of substituted salicylaldimine ligands and non-metallocene catalysts for the olefin polymerization has been review ed with 33 references.
Photoelectrochemical Study of PbS/RuL2(NCS)2 Sensitized Cd(Ⅱ)Doped Nanoporous TiO2 Film Electdode
Li Weihua , Hao Yanzhong , Wang Yanqin , Qiao Xuebin , Gao Enqin , Yu Cheng , Yang Maizhi , Cai Shengmin
1999, 16(1): 6-10
[Abstract](337) [FullText HTML] [PDF 211KB](2)
Abstract:
5%Cd (Ⅱ)doped nanoporous TiO2 film electrode was prepared.The photoelectrochemical behavior of the electrodes sensitized by PbS, RuL2(NCS)2(L=2, 2'-bipy ridine-4, 4-dicarboxy lic acid)and composite PbS /RuL2(NCS)2 respectively have been investigated.The results showed that the photocurrent generations of the sensitized Cd (Ⅱ)doped TiO2 film electrodes ex tended to visible and infrared regions and the electrode sensitized by composite PbS/RuL2 (NCS)2 was much better than others in solar energy conversion.
Hydrogenation Activities of Palladium Catalysts Supported on Guanidoethyl-, Aminoethyl-and N, N-Dicyanoethylaminoethyl-Zirconium Phosphonate
Luo Zhongjie , Ma Xuebing , Gong Chengbin , Fu Xiangkai
1999, 16(1): 11-15
[Abstract](263) [FullText HTML] [PDF 203KB](2)
Abstract:
Three amorphous zirconium mixed phosphate phosphonate supports Zr(HPO4)2-x· (O3P(CH2)2NRR1)x·H2O (R=H or (CH2)2CN;R1=H,-C(=NH)NH2 or (CH2)2CN) and palladium catalysts supported on them were prepared from 2-guanidoethylphosphonic acid, 2-aminoethylphosphonic acid, and N, N-(biscyanoethyl) aminoethylphosphonic acid with zirconium oxychloride and phosphoric acid, respectively. All the supports with their palladium catalysts have been characterized by IR, TG, DTA and XPS measurements. Factors influencing the hydrogenation activities under atmospheric pressure over the catalysts have been examined in comparison with Pd/C catalyst. The supported catalysts showed very high hydrogenation activity and selectivity for some vinyl compounds and nitrobenzene. They can be used repeatedly.
Ni-Pd-P Film Electrodeposited on Semiconductor Silicon and Its Structure
Liu Bing , Yao Suwei , Guo Hetong , Yuan Huatang , Zhang Yunshi
1999, 16(1): 16-20
[Abstract](486) [FullText HTML] [PDF 370KB](1)
Abstract:
Ni-Pd-P film was formed on semiconductor silicon by potential controlled electrodeposition technique. Results showed that addition of H3PO3 improved the deposition of Ni and P. With increase of pH of the plating solution, the content of Ni was increased and the Pd and P contents were decreased. The composition of P had a great effect on the inter stress of the film. Many cracks were found on the surface of the film containing 1.49% P, but they disappeared entirely when the P content was 3.50%. Deposit containing lower than 2% P was a solid solution with fcc structure. The structure changed from crystal to amorphous when P content was higher than 4%.
Synthesis, Characterization and Bioactivity of Rare Earth Binary Complexes Containing Indole-3-Propionic Acid
Song Zhigang , Chen Zhonglin , Wang Liufang
1999, 16(1): 21-25
[Abstract](309) [FullText HTML] [PDF 202KB](1)
Abstract:
Fifteen binary rare-earth complexes with indole-3-propionic acid were prepared in general formula of RE(IPA)nH2O(RE=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, n=1; RE=Dy, Ho, Er, Tm, Yb, Lu, Y, n=0;IPA=indole-3-propionic acid).The compositions and structures of the complexes have been investigated by IR, TG, XRD and 1H NMR techniques. Their effects on the growth of wheat seedling has been examined briefly.
Cocatalytic Role of CeO2 in Combination with Pd/γ-Al2O3 Catalyst
Jiang Xiaoyuan , Zhou Renxian , Mao Jianxin , Zheng Xiaoming
1999, 16(1): 26-29
[Abstract](418) [FullText HTML] [PDF 198KB](1)
Abstract:
The TPR, SEM, TPD-MS techniques and CO oxidation activity measurement have been used to study CeO2-Pd/γ-Al2O3 catalyst under oxygen-enriched and oxygen-deficient conditions. Results showed that interaction between CeO2 and Pd caused the peak of the CeO2-Pd/γ-Al2O3 catalyst in TPR curve to shift to lower temperature, promoted surface oxygen desorption of Pd/γ-Al2O3, favored the Pd distribution, improving the oxidation activity of the catalyst.
Influence of Solvents on the Metal Hydride Electrode Binded by SBS Elastomer
L Guojin , Lei Cuiyue , Shan Zhong qiang , Han Zuoqing , Yang Lansheng , Zhang Yingping , Guan Yunlin
1999, 16(1): 30-33
[Abstract](451) [FullText HTML] [PDF 242KB](1)
Abstract:
Styrene-butadine-styrene elastomer (SBS) has been found to be a better binder than PTFE and H PMC in preparation of metal hydride electrode. On binding with SBS, three solvents have been tested:toluene, turpentine oil and butyl acetate, among them the turpentine oil appeared most favorable. In the last case the electrode had the highest dischargeability in high current, discharge capacity and the least inner resistence.The optimum shaping temperature for electrode preparation was 80℃.
Oxidative Dehydrogenation of Propane on Supported V2O5/Zr3(PO4)4 Catalysts
Zhang Weide , Sha Kaiqing , Yu Lajia , Wan Huilin , Tsai Khirui
1999, 16(1): 34-37
[Abstract](357) [FullText HTML] [PDF 167KB](1)
Abstract:
0.6%~6.0%V2O5 were supported on the amorphous Zr3(PO4)4 by a impregnation method. The supported catalysts were effective in the oxidative dehydrogenation of propane, e.g. on a 3.0%V2O5/Zr3(PO4)4 catalyst propene had selectivity of 53.8% at a propane conversion of 17.0% and the yield of propene was 9.1%. XRD, IR and Raman results showed that the vanadium oxide was distributed on the support in form of VOx species. ESR results indicated there are V4+ species in the catalysts, implying that the oxidation couple of V5+/V4+ could be responsible for the redox reaction in propane oxidative dehydrogenation.
Synthesis, and Thirdorder Nonlinear Optical Property of Some Transition Metal Dithiocomplexes
Wu Jieying , Tian Yupeng , Xie Fuxin , Ni Shisheng
1999, 16(1): 38-41
[Abstract](527) [FullText HTML] [PDF 179KB](1)
Abstract:
4-Aminophenyl ammonium dithiocarbam ate and their Ni(Ⅱ), Pd (Ⅱ)and Pt (Ⅱ) complexes have been synthesized and characterized. The complexes formed metall (Ⅱ) dithiocarbimates with tetrabutyl ammonium bromide in alcoholic NaOH solution. The spectral results indicated that both dithiocarbamate and dithiocarbimate complexes are bidentate ligand and have square planar configuration. The third-order nonlinear optical response results obtained by degenerate four-wave mixing technique showed that the dithiocarbim ate complexes have higher third-order nonlinear optical response due to high delocalization of the system.
Deactivation of Commercial Sulfur-resisting WGSR Catalyst Mo-Co-Mg/γ-Al2O3
Li Yumin , Wang Hainan , Wang Rijie , Zhang Jiyan , Zhang Liu
1999, 16(1): 42-45
[Abstract](321) [FullText HTML] [PDF 171KB](1)
Abstract:
The deactivation of commercial catalyst for water gas shift reaction (WGSR) has been studied through activity evaluation, temperature program med technique, XRD, porosity and sulfur content measurements. It is found that the deactivation of a long-run catalyst is the results of sintering, formation of the inactive phases of MoS2, CoS2, CoSO4 and MgAl2O4, and irreversible conversion of the active sulfur component into inactive ones. Temperature and steam advance the deactivation.
Effect of Cu(Ⅱ)on the Interaction Between Amino Acids and Solid Particles
Cheng Fengyun , Zhang Zhengbin
1999, 16(1): 46-49
[Abstract](327) [FullText HTML] [PDF 176KB](1)
Abstract:
The interactions between copperion, amino acids and solid particles have been investigated.The ion exchange percentageE(%)-pH curves for tryptophane absorbed on amorphous Fe(OH)3 are peaked, while the E(%)-pH curves for tyrosine adsorbed on δ-MnO2 have a complex form of both "S-shaped" and "reverse S-shaped" curves, indicating the formation of type Ⅰ ternary surface complexes.
Structure and Reductive Characteristics of Ag-Fe Complex Oxide Catalysts
Chen Min , Luo Mengfei , Zheng Xiaoming
1999, 16(1): 50-53
[Abstract](311) [FullText HTML] [PDF 165KB](2)
Abstract:
Ag-Fe complex oxide catalysts were prepared by a coprecipitation method. The structure of the catalysts has been investigated by XRD technique and the effect of thermal treatment on the reducibility of the catalysts by TPR technique. The results show ed that there is a relationship between the reducibilities and Ag contents of the catalysts and the oxidation activities of the catalysts lie in the σ-AgFeO2 species dispersed on the surface of the catalysts.
Effect of Al in Mm(NiCoMnAl)5 on the Performance of the Sealed MH/Ni Cell
Wang Xianyou , Liu Bing , Yuan Huatang , Zhang Yunshi
1999, 16(1): 54-57
[Abstract](438) [FullText HTML] [PDF 167KB](1)
Abstract:
XRD results showed that in sealed MH/Ni cell Al can be dissolved in alkaline solution and precipited on the surface of Ni(OH)2, forming Ni1-xAlx(OH)2. Surface pretreatment of the hydrogen storage alloy powder of Mm(NiCoMnAl)5(Mm=mixed rare earth metal) could avoid the Al being released into the sealed MH/Ni cell.
Selective Hydrogenation of Maleic Anhydride to Succinic Anhydride on PdCl2/PPh3
Liu Pu , Liu Ye , Yin Yuanqi
1999, 16(1): 58-61
[Abstract](449) [FullText HTML] [PDF 163KB](1)
Abstract:
A noval preparation method of succinic anhydride with high selectivity and conversion by homogeneous hydrogenation of maleic anhydirde has been successfully developed. Results show that among catalysts and ligands studied PdCl2 is the best catalyst and PPh3 is the most suitable ligand. The effects of n(PPh3)/n (Pd), reaction temperature, hydorgen pressure, catalyst concentration and maleic concentration have been investigated. Under the typical reaction conditions: PdCl2=1.25×10-3 mol/L, n(MA)/n(Pd)=2000, n(PPh3)/n(Pd)=4 in 8 mL ethylene glycoldimethyl ether at 373~393 K and hydrogen pressure of 2.5 MPa for 1 hour more, the conversion of meleic anhydride is 90% and the selectivity of succinic anhydride is 100%.
Synthesis of Liquid Crystals Containing Sulfonate Unit
Li Zhiping , Ren Guodu
1999, 16(1): 62-64
[Abstract](861) [FullText HTML] [PDF 134KB](1)
Abstract:
Sodium 4-(4"-octyloxydiphenyl-4'-carbonyloxy) benzenesulfonate is synthesized via esterification of 4'-octyloxybiphenyl-4-carboxylic acid with sodium hydroxybenzene sulfonate using dicyclohexylcarbodiimide and 4-dimethy lamino-pyridine as catalysts. Its sulfonyl chloride on reaction with alcohols gives nine liquid crystals with sulfonate unit in molecules.The products have been characterized to be liquid crystals by IR, MS as well as DSC and polarizing optical microscopy techniques.
Microstructure and Physical Property of Chemically Deposited NiPAl2O3 and NiP-SiC Composites
Wu Yucheng , Zhang Lide , Li Guanghai , Huang Xinmin , Shi Huazhong , Liu Famin , Zhang Ye , Yao Baodian
1999, 16(1): 65-67
[Abstract](346) [FullText HTML] [PDF 136KB](1)
Abstract:
The title composites were obtained by chemical deposition method. It is found that the components are mechanically incorporated and the crystalization tendency of the composite coatings increases with increase of codeposited components and decrease of phosphorus content in alloy. Ni3P was observed in composite at higher aging temperatures.The composites have higher hardness and lower wear volume than the original alloy.
Synthesis of Tetra(4-nitrophenyl) porphyrin and Tetra(4-aminophenyl) porphyrin
Zhu Baoku , Xu Zhikang , Xu Youyi
1999, 16(1): 68-70
[Abstract](896) [FullText HTML] [PDF 127KB](1)
Abstract:
An improved method for synthesis of tetra (4-nitrophenyl) porphyrin (TNPP) and tetra (4-aminophenyl) porphyrin (TAPP) is reported. 4-Nitrobenzaldehyde was cyclized with pyrrole in refluxing nitrobenzene using a lactic acid catalyst and then precipited by methanol giving TNPP of 22.3% yield in high purity. Reduction of TNPP with SnCl2·2H2O in concentrated HCl gave high purity TAPP in yield of 81.5%.
Partial Oxidation of Methane to Syngas by Self-exothermic Reaction
Bi Xianjun , Wang Zhen , Hong Pinjie , Dai Shushan
1999, 16(1): 71-73
[Abstract](319) [FullText HTML] [PDF 127KB](1)
Abstract:
The partial oxidation of methane to syngas by self-exothermic reaction has been studied over Ni/ZrO2 catalyst. It is found that the Ni content in catalyst had little effect on the activity and selectivity of the catalyst and increase of space velocity and reaction temperature improved the methane conversion and the selectivity of CO and H2.
Photoluminescence in Copolymers of Two Alkoxyl Substituted Polyphenylene
Wang Haiqiao , Zeng Fandi , Huang Dexiu
1999, 16(1): 74-76
[Abstract](398) [FullText HTML] [PDF 136KB](1)
Abstract:
The photoluminescence behaviour of two polymers:poly (2, 5-dibutoxyphenylene) (DBO-PPP)and poly(2, 5-didodecyloxyphenylene) (DDO-PPP)either in blend or in copolymer forms were found to be almost identical with each other. Their emission intensities were both increased with increase of DDO-PPP content.
Coordination of Chitosan with Zn(Ⅱ)and IR spectra
Wang Aiqin , Li Hongqi , Yu Xianda
1999, 16(1): 77-79
[Abstract](305) [FullText HTML] [PDF 127KB](1)
Abstract:
A series of chitosan-Zn(Ⅱ)complexes with n (chitosan):n(Zn(Ⅱ))=1:0.05~1:1.0 were synthesized in aqueous acidic solution. The results indicated that the Zn(Ⅱ) content of the complexes prepared in dilute formic acid solution was higher than in other acid solutions: acetic, propionic, benzoic and hydrochloric acids.IR spectrum results showed that Zn(Ⅱ)are coordinated to-NH2,-NHCO-and-OH groups of chitosan molecnle and the final complexes have no definite chemical composition.
Laser Induced Electroless Deposition of Nickel on Semiconductor Silicon
Liu Bing , Gong Zhenglie , Yao Suwei , Guo Hetong , Yuan Huatang , Zhang Yunshi
1999, 16(1): 80-82
[Abstract](280) [FullText HTML] [PDF 133KB](1)
Abstract:
Laser induced electroless deposition of nickel on the semiconductor silicon after Pd impregnation has been carried out by using YAG laser and investigated by XPS combined with Ar+ sputtering technique. The results indicated the existence of interdiffusion between Ni, Pd and Si at room temperature and formation of different silicide compounds.
Syntheses of Antiviral Precursors:Trihydroxy Nucleosides
Liu Li , Chen Zuxing , Wang Shimin , Yang Guichun
1999, 16(1): 83-85
[Abstract](288) [FullText HTML] [PDF 129KB](1)
Abstract:
Title compounds were obtained by treating nucleosides with two antagonistic polymeric reagents, P-IO4- and P-BH4- in one-pot process.The method has the advantages of simple operation, mild reaction condition and unnecessary isolation of the intermediates with high yield.
Cotton Stalk Cellulose Modification Ⅲ. Preparation and Adsorption Property of Cotton Stalk Cellulose Modified by Poly (ethyleneamine)
Hu Ling , Meng Ling zhi , Li Qingyun , He Yongbing
1999, 16(1): 86-88
[Abstract](474) [FullText HTML] [PDF 133KB](1)
Abstract:
Two modified cotton stalk cellulose derivatives (CEN-1, CEN-2) were prepared by reaction of epoxy-activated cotton stalk cellulose powder with diethylenetriamine or triethylene-tetramine, respectively.The effects of pH value of the solution on the adsorption properties of CEN-1 and CEN-2 to Pb2+, Hg2+, Cr3+ ions are discussed.
Synthesis of Inverse Suspending Agents for Acrylate Polymerization
Lu Jianmei , Zhu Xiulin , Wan Dechun , Jiang Qisong , Li Yi
1999, 16(1): 89-91
[Abstract](480) [FullText HTML] [PDF 131KB](1)
Abstract:
Two copolymers(S-1, S-2) were prepared from styrene with N-vinylpyrrolidone and N, N-diethylacrylamide respectively. The partly neutralized acrylate (sodium) was polymerized in cyclohexane by using the copolymers as an inverse suspending agent. When S-1 meeted 8%< F2W< 20% and 1.2 ×104< M< 7.5 ×104 the polyacrylate obtained had a particle size of 0.3~2.6mm and a high water absorption ability. Using S-2 as suspending agent the particle size of polyacrylate was ca.1 mm. The copolymers have the advantages of improving the particle size of polyarylate and a little adhesion to reactor.
Polyaniline/Poly (butyl acrylate-styrene-hydroxyethyl acrylate) Conductive Complex
Chen Yichi , Zuo Lei , Yan Tingjuan , Yin Wusheng , Wu Jinping , Gu Tiren
1999, 16(1): 92-94
[Abstract](380) [FullText HTML] [PDF 134KB](1)
Abstract:
Aniline was polymerized within the poly (butyl acrylate-styrene-hydroxyethyl arylate) [P(BSH)] copolymeric matrix, forming directly a flexible conductive composite film. The conductivity of the films was increased with the amount of aniline, and again increased firstly and then decreased with the increase amount of the oxidant. When the weight ratio of aniline to [P(BSH)] was 0.2, the conductivity of the film was up to 8 S/m.
Determination of Nucleotide Molecules by Matrixassisted Laser Desorption/Ionization Mass Spectrometry
Deng Huimin , Li Jun , Lai Zhihui , Zhao Shankai
1999, 16(1): 95-97
[Abstract](303) [FullText HTML] [PDF 138KB](1)
Abstract:
Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry has been used to determine the molecular weights of DNA oligomers d(T)6 and d(C)10.The results showed that 3-hydroxypicolinic acid was effective matrix in comparision with the mixture of 3-hydroxy picolinic acid and picolinic acid, 2, 5-dihydroxybenzoic acid, α-cyano-4-hydroxycinnamic acid, 2, 5-dihydroxyacetophenone and 2, 4, 6-trihydroxyacetophenone.NH4+ ion exchane resin and diammonium hydrogen citrate were used successfully to eliminate the influences of Na+, K+, Ca2+, Mg2+ ions.
Adsorption property of Schiff-base Type and Secondary Amine Type Chitosan-Crownethers
Tan Shuying , Wang Yuting , Peng Changhong , Tang Yurong , Luan Zhaokun
1999, 16(1): 98-100
[Abstract](480) [FullText HTML] [PDF 140KB](1)
Abstract:
Two N-Schiff base type chitosan-crownethers (S15-CTS and S18-CTS) were synthesized by reaction of 4'-formylbenzo-15-crown-5 and 4'-formylbenzo-18-crown-6 with chitosan respectively. N-secondary amine type chitosan-crownethers (Z15-CTS and Z18-CTS) were also prepared by reaction of N-Schiff base type chitosan-crow nethers with sodium borohydride.Their static adsorption properties for metal ions (Pd2+, Cu2+ and Hg2+) had been studied. The results showed that four chitosan-crow nethers had good adsorption character and adsorption selectivity for Pd2+ in the presence of Cu2+ or Hg2+.
Oscillation of Cyclic Voltammogram of Ethanol Oxidized at Platinized Platinum Electrode
Wang Jundong , Wang Zhenrong , Chen Xu , Yang Xiaoli , Yu Haitao , Fu Honggang , Xu Shanpeng , Huang Juying
1999, 16(1): 101-103
[Abstract](381) [FullText HTML] [PDF 126KB](1)
Abstract:
Ethanol oxidized at a platinized platinum electrode in alkaline solution containing Na2MoO4 gave periodic and aperiodic oscillation in cyclic voltammogram. It is considered as a result of oxidation of ethanol coupled with oxidation and reduction of Mo at the electrode surface.
Surface Phosphating of Amorphous Fe-W Deposit and Its Corrosion Behavior in NaCl Solution
Wang Hongzhi , Yao Suwei , Zhang Weiguo
1999, 16(1): 104-106
[Abstract](262) [FullText HTML] [PDF 134KB](1)
Abstract:
A fine phosphate coating was fo rmed on the surface of amorphous Fe-W deposit after phosphating in zincous phosphating solution. The anodic polarization curves show ed that the pitting potential of Fe-W deposit moves about 1.4 V tow ard noble after phosphating. The immersion test showed that the corrosion resistance of Fe-W deposit against Cl- after phosphating has increased and its corrosion rate is about one fifth of that of the original FeW deposit.
Solvent Extraction of Ethanol by Chemical Complexation with Iron Caproate
Qi Jiang , Dai Youyuan
1999, 16(1): 107-109
[Abstract](470) [FullText HTML] [PDF 125KB](1)
Abstract:
Solvent extraction of ethanol has been carried out by caproic acid, caproic acid containing iron caproate and toluene containing iron caproate based on the HSAB principle. Experiments showed that caproic acid containing iron caproate could give higher distribution ratio than single caproic acid, indicating that there is a strong interaction between iron caproate and ethanol. Distribution ratio of ethanol was greatly affected by the concentration of iron caproate, but slightly by initial concentration of ethanol. The mechanism of extraction is discussed.
Asymmetric Synthesis of (1'S, 4R, 5R)-2-(1'-Bromoethyl)-2-(5-bromo-6-methoxy-2-naphthyl)-1, 3-dioxolane-4, 5-dicarboxylic Acid
Hu Aixi , Fan Guozhi , Zhao Haitao , Wang Guiying
1999, 16(1): 110-112
[Abstract](363) [FullText HTML] [PDF 136KB](2)
Abstract:
Title compound was synthesized with total yield of 80% by acetalization, asymmetric bromination, hydrolysis of 6-methoxy-2-propionylnaphthalene, using (2R, 3R)-dimethyl tartrate as a chiral auxiliary.
The Tribological Property of CePO4 Nanoparticle
Liang Qi , Zhang Zhijun , Xue Qunji , Liu Weimin
1999, 16(1): 113-114
[Abstract](659) [FullText HTML] [PDF 98KB](1)
Abstract:
CePO4 nanoparticles surface-modified by alkylphosphate can be well dispersed in chloroform, benzene and liquid parrafin with lower friction factor, high antiwear and load-carrying ability.
Synthesis and Reduction of Deuterated Acetophenone-d8
Zhang Lin , Xie Rugang
1999, 16(1): 115-116
[Abstract](370) [FullText HTML] [PDF 92KB](2)
Abstract:
Deuterated acetophenone-d8(C6D5-COCD3) was prepared from perdeutero-benzene (C6D6)and perdeutero-acetic acid in high yield and high deuterium isotopic content(about 86% and 99.3% respectively). C6D5-COCD3 was then reduced with nickel-aluminum (Ni-Al) alloy in 12%~18% NaOD-D2O solution to give corresponding deuterated α-phenylethanol-d10(C6D5-CDODCD3), the yield and deuterium isotopic content were 85.2% and 99.2%.
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