• Volume 29,Issue 3,2012 Table of Contents
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    • >Functional materials
    • Study on Preparation of Porous Ceramic Separation Membrane Supports

      2012, 29(3).

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      Abstract:The porous ceramic separation membrane supports are prepared using alumina fine as main raw materials, and the TG/DSC curves of raw materials powder are analyzed. The effects of supports’ sintering temperature on the shrinkage are studied. The effects of different the sintering temperature, holding time and materials powder particle size on pore structure and size of supports are studied. The effect of the pore former dosage on porosity are studied. The results show that sintering temperature 1200℃, holding time 6h, porous agent more than 20%, prepared the uniform pore size distribution, porosity, accord with more than 50% of porous ceramics waterproof demand separation membrane supports.

    • Synthesis and Spectral and Electrochemical Properties of Novel Triphenylamine Derivatives

      2012, 29(3).

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      Abstract:With triphenylamine and fluorenone as raw materials, three novel triphenylamine derivatives: (4-fluorenylidene hydrazo methylenephenyl)diphenylamine, bis-(4-fluorenylidene hydrazo methylenephenyl)phenylamine and tris-(4-fluorenylidene hydrazo methylenephenyl)amine(a~c) were synthesized via Nucleophilic Addition. The structures of the three target compounds were characterized by means of FTIR, 1HNMR and elemental analysis. Their UV-Vis spectra, fluorescence spectra, electrochemical behavior and thermal stability were studied respectively. The results show that the thin films of three compounds(a~c) emit red fluorescence. They all obviously have the performance of Aggregation-Induced Emission (AIE). Their ionization potential energy levels (5.62~ 5.65 eV) are matched with work function (4.8 eV) of positive electrode(ITO), so the barrier of hole transporting can be effectively reduced and in favor of hole-transport. The results of TG curves show that their thermal decomposition temperatures (Td) are 317,292 and 303 ℃ and they all have good thermal stability.

    • Synthesis and characterization of Li1.3Al0.3Ti1.7(PO4)3 thin films heated by different annealing techniques

      2012, 29(3).

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      Abstract:Li1.3Al0.3Ti1.7(PO4)3 thin films were prepared by rapid thermal annealing (RTA) and conventional furnace annealing (CFA). The phase and surface morphology of the prepared films were characterized by X-ray diffraction and scanning electron microscope. The electrochemical window, ionic condutivity and activation energy were conducted by cyclic voltammetry, and A.C. impedance spectroscopy. The results show that the films prepared by RTA and CFA are homogenous and crack-free. However, the film prepared by RTA shows smaller grains and is denser than the one prepared by CFA. The electrochemical windows of the two films are beyond 2.4V. The ionic conductivity of the films prepared by RTA and CFA are 2.7?10-6 S.cm-1 and 1.4?10-6 S.cm-1, respectively. The activation energy of the film prepared by RTA is slightly smaller than the one prepared by CFA.

    • Study of Preparation and Properties of LnBaCo2O5 δ-La10Si6O27 Composite Cathode for Solid Oxide Fuel Cells

      2012, 29(3).

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      Abstract:A novel LnBaCo2O5 δ-La10Si6O27 composite cathode, with continuous ion transportation from the cathode to the electrolyte, was prepared by wet impregnation method. The phase composition and microstructure of the cathode were investigated by XRD and SEM. The composite cathode showed an excellent electrocatalytic activity, which was determined by ac impedance spectroscopy, and is a potential cathode material for the intermediate temperature solid oxide fuel cell.

    • Research in CuCoMnOx spectrally selective paint coatings

      2012, 29(3).

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      Abstract:Spectrally selective paint coatings were prepared by spraying method using polyurethane modified by acrylic resin as binder and CuCoMnOx semiconductive compound oxide as pigment. The effect of P/B (pigment/binder) ratio, milling time, temperature, substrates and film thickness on the optical properties of the coatings was investigated. The results show that the solar absorptance (αs) and thermal emittance (εT) of the coatings are 0.936 and 0.312 , the αs/εT ratio is 3.0 when the P/B ratio is 3:1, the milling time is 9~12h, the substrate is Al and the thickness is 1.9μm. The coating also has favorable mechanical behavior, corrosion resistance and weatherability.

    • Synthesis and Biological Activities of Fluorinated 1,3,4-Thiadiazolylureas

      2012, 29(3).

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      Abstract:Six fluorinated 1,3,4-thiadiazolylureas were synthesized by reaction of fluorine-containing benzoyl azides with 2-amino-5-(fluorine-containing styryl)-1,3,4-thiadiazoles, which were prepared in one step through the condensation-cyclization of fluorine-containing cinnamic acid and thiosemicarbazide with POCl3 as dehydrating agent, in the yield of 68%, 69%, 66%, 67%, 71% and 73% respectively. The structures of the products were confirmed by IR, 1H NMR, MS and elemental analysis. The preliminary bioassay showed that target compounds IIIc and IIId exhibit good cytokinin activity at the concentration of 10 mg/L, and the promoting rates of them are 53.5% and 55.1%, respectively.

    • The status and development of water treatment chemicals industry in China

      2012, 29(3):0-0.

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      Abstract:Described and analysed the water treatment chemicals problems from development, situation, marketing, features in the wide field of vision had been in this article. The article also offered a wide range data from production and marketing, and had been given the suggestion for adjustment water treatment chemicals marketing strategy. Key words:Water treatment agent; Water treatment chemicals; Scale inhibitor; Corrosion inhibitor; Biocides

    • >Surfactants
    • Synthesis And Properties Of Di-linear Alkylated

      2012, 29(3).

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      Abstract:Di-linear alkylated diphenylmethane sulfonate(DSDM) is a series of new-style anionic gemini surfactants, they have been synthesized from lauric acid, myristic acid , cetylic acid and chlorosulfonic acid as raw materials,and been separated and purificated by silica gel chromatography.The structures of them were characterized by 1H-NMR and MS. The surface tension and oil-water interfacial tension have been measured. The results indicated that the cmc and γcmc is 1.452 mmol?L-1和38.49 mN?m-1 at 25℃ ; The interfacial tension of C14-DSDM、C16-DSDM are affected by temperature and hardness of the water. The interfacial tension of C14-DSDM is not affected by salinity,but the interfacial tension of of C16-DSDM is affected seriously by salinity. themixed surfactant exhibits and ultra-low interfacial tension of 9.44?0-3mN/m.

    • Application of polydimethyl silicone surfactant on properties of styrene-acrylate emulsion

      2012, 29(3).

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      Abstract:Through the hydrosilylation the polydimethyl silicone surfactant(PSS) was prepared,and then styrene-acrylate emulsion was synthesized by semi-continuous pre-emulsified polymerization, and the PSS was used as emulsifier.IR analysis and EDS energy were used to tested the structure of PSS. The CMC was 4.53×10-6mol•L-1and the cloud point was 61~62°C.And then the effect of PSS dosage(wt%,1%~5%) on the properties of styrene-acrylate emulsion was studied. The results show that the more PSS was used, the conversion rate of monomer could be 98.65%, the gelation rate could be 0.87%, the stability of emulsion became higher firstly and then were stable, and the water absorption rate of the styrene-acrylate emulsion with the polydimethyl silicone as emulsifier was decreased to 9.51%, and defoaming times was 18s,has lower surface tension, shorter defoaming time, lower water absorption and better water resistance than the styrene-acrylate emulsion with emulsifier without polydimethyl silicone(Alkyl phenolic epoxy vinyl ether,OP-10).

    • >Biological engineering
    • Effects of Levofloxacin on the production and the structure of rhamnolipids produced by pseudomonas aeruginosa NY3

      2012, 29(3).

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      Abstract:Two mutagenesis strains named NY3-1 and NY3-2 were obtained through pseudomonas aeruginosa NY3 inducing with levofloxacin. By comparing the physical and chemical properties of rhamnolipids produced by them, some conclusions were reached as follows: Production, composition and structure characteristics of rhamnolipids produced by mutagenesis strains and wild strains were quite different. Compared with the wild strains,yield of rhamnolipids produced by NY3-1 was improved by 19.57%, while for NY3-2 the yield was decreased by 17.60%. the ratios of amounts of disaccharide and monosaccharide in rhamnolipids produced by NY3、NY3-1、NY3-2 strains were 0.969,0.677 and 1.316 respectively. The infra-red spectrums demonstrated that no C=C unsaturated bond was found in the rhamnolipids produced by NY3 strains, while those produced by NY3-1 and NY3-2 strains contained C=C bond. The results from electrospray ionization mass spectrometry (ESI-MS) analysis showed that all the rhannolipids produced by the three stains contained Rh-C10,while only that produced by two induced strains have high content of Rha-Rha-C10:1 which contain C=C unsaturated bond.

    • Resolution of (R,S)-2-hydroxy-4-Ethyl benzene by Immobilized Serratia sp. Lipase

      2012, 29(3).

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      Abstract:Optical resolution of (R,S)-2-hydroxy-4-Ethyl benzene [(R,S)-HPBE] by calcium alginate-glutaraldehyde cross-linking Serratia sp. lipase was developed, and the activity and many factors affecting the resolution were investigated. The optimum reaction conditions were temperature 50℃, pH=7.0, concentration of (R,S)-HPBE 40 mmol/L and ρ(lipase amount)=200 g/L. After 10 h of resolution by immobilized lipase, the conversion rate of (R)-HPBE is 93.4% and e.e. is 96.2%. After twelve times repeated batch operation, the conversion rate of product by immobilized lipase is more than 80%.

    • >Modernization technology of traditional Chinese medicines
    • Comparative analysis of volatile constituents in herbal pair Flos Farfarae –Tatarian Aster Root and its signal herb by GC-MS

      2012, 29(3).

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      Abstract:In this paper, the constituents of essential oils which extracted with hydrodistillation from the herbal pair Flos Farfarae –Tatarian Aster Root (FF-TAR) and its signal herbs were analyzed by capillary GC-MS and elucidated based on the standard mass spectral data. 52, 44 and 45 kinds of volatile components were identified respectively. Relative mass fractions of the constituents were determined by area normalization method. The identified relative contents of essential oils were 96.48%, 88.47% and 91.61%, respectively. Four new volatile compounds in herbal pair Flos Farfarae –Tatarian Aster Root are produced because of the chemical reactions and physical changes occurred in the process of decocting two single herbs.

    • >Catalysis,separation and purification technology
    • L-phenylalanine preparation of Chiral Stationary Phase

      2012, 29(3).

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      Abstract:Abstract:L-phenylalanine CSP was prepared by L-phenylalanine and stearoyl chloride via esterification, amidation, saponification and acid chloride reaction, The CSP had been characterized by FT-IR ,1HNMR spectra and elemental analysis. According to the mass ratio of 3:1, The CSP and silica gel were used as thin layer chromatography,V(ethanol): V(ethyl acetate): V(triethylamine)=11:5:1 as development system, duloxetine was separated on the TLC,(R-)duloxetine Rf1=0.87,(S-)duloxetine Rf2=0.75.

    • Influence of Phosphate Modification on the Structure and Catalytic Performance of Zeolite Y

      2012, 29(3).

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      Abstract:The zeolite Y synthesized by in-situ crystallization technique was modified with phosphate. The crystalline structure and surface acidity of the modified zeolite Y(named zeolite PY) were characterized by using techniques such as X-ray diffraction ( XRD) , NH3 temperature programming desorption (NH3-TPD). The results showed that the introduction of phosphorus had no effect on crystal form of the zeolite PY, and the caused impact on relative crystallinity was obscure. Moreover, the space unit shrank, the cell parameter decreased, and the molar ratio of Si/Al increased. It was found that the modified PY catalyst could effectively adjust the total acid amount and acid strength of the catalysts. The introduction of phosphorus could also decrease the total acidity, weak acidity and strong acidity, but increased the moderately strong acidity. Further evaluation that carried on a small fixed fluidized bed showed that the modified PY catalyst exhibited excellent heavy oil cracking capability an d superior selectivity to desired products.

    • The purification of m-dinitrobenzene by Triphrase Transfer catalysis

      2012, 29(3).

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      Abstract:a variety of polymeric phase transfer catalysts with quaternary ammonium active center was synthesized by means of quarterisation of tertiary amine and chloromethylated polystyrene polymer.crude m-dinitrobenzene was purified by Phase Transfer Catalyst to tansfer the p-dinitrobenzene and o-dinitrobenzene into nitrodiphenyl ether.The best process conditions and catalyst were determined on the base of reaction yield of different regents and catalysts.It was concluded that polystyrene polymer pyridine and methnol were the best catalyst and oxyalkylation reagent for this reaction.The feasible process conditions m(crude m-dinitrobenzene):m(methnol): m(sodium hydroxide):m(polystyrene polymer pyridine)was 1:0.8:0.1:0.12,tempeture and reaction time were 76-78℃ and 2h.The purity of m-dinitrobenzene was high to 99.5% to prepare the m-phenylenediamine and recycling of polystyrene polymer pyridine resin was very easy and could be used 7 times.

    • Advance in the application of hydrophobic catalyst over SDB in chemical industry

      2012, 29(3).

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      Abstract:In water-containing catalytic reactions, regarding of whether water is reagent, reaction medium or product, water has much influence on the activity and life of hydrophilic catalysts. Hydrophobic catalysts can well overcome the disadvantage of hydrophilic catalysts by avoiding the coverage of water on active components. In recent years, SDB (styrene-divinylbenzene copolymers) have got more and more attention in the field of catalyst preparation due to the distinct hydrophobicity of SDB. Advances of research and application of hydrophobic catalysts over SDB in nuclear industry and the production of saturated acid /ester and olefine acid /ester were reviewed in this paper. Based on the research, the room of research and application of the hydrophobic catalyst was prospected.

    • Preparation and Catalytic Applications of Sulfonated Amorphous Carbon Materials

      2012, 29(3).

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      Abstract:Sulfonic acid group-functionalized amorphous carbon solid acid catalyst (AC-SO3H) was prepared through vapour-phase transfer sulfonation method. The material was characterized by means of inductively coupled plasma atomic emission spectrometry (ICP-AES), Fourier-transform infrared spectrum (FT-IR), X-ray powder diffraction (XRD), scanning electronic microscopy (SEM) and thermogravimetric analysis (TGA). Elemental analysis result shows that the obtained solid acid catalyst has a —SO3H group loading of 2.03 mmol/g. Comparing with other solid acid catalysts, AC-SO3H shows enhanced activity and proves to be efficient heterogeneous catalyst for Baeyer-Villiger oxidation of ketones and Friedel-Crafts alkylation of anisole with benzyl alcohol. The catalyst shows excellent thermal and structural stability, and retains good activity over several cycles. The synthesis process is simple and the catalyst can be easily prepared in large scale.

    • >Drug and cosmetic materials
    • Synthesis and Antitumor Activity of Novel Bisamides Compounds

      2012, 29(3).

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      Abstract:Ten novel bisamides compounds containing benzothiazol unit were synthesized. Their structures were characterized by 1H NMR, 13C NMR, IR and elemental analyses. Preliminary bioassay indicated that some compounds posed antitumor activity to PC3 and BGC-823 cells in vitro by MTT method. The antiproliferation activity of compound N-(2-(6-methylbenzothiazol-2-ylcarbamoyl)4-methylphenyl)-4-chlorobenzenecarboxamide (4a) and N-(2-(4-methylbenzothiazol -2-ylcarbamoyl)-4-methylphenyl)-2-methylbenzene carboxamide (4e) to PC3 cells at the concentration of 10 μmol•L-1 was 70.8% and 68.4%. And the antiproliferation activity of compound N-(2-(benzothiazol-2-ylcarbamoyl)-4-methylphenyl)-2-methylbenzenecarboxamide(4d) to BGC-823 cells at the concentration of 10 μmol•L-1 was 65.9%.

    • Preparation of a novel chitosan /β-cyclodextrin magnetic microspheres and study on their adsorption properties

      2012, 29(3):0-0.

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      Abstract:A series of novel magnetic microspheres were prepared from chitosan and β-cyclodextrin through inverse suspension crosslinking. The obtained magnetic microspheres were characterized by optics microscopy,IR and VSM. The adsorption behavior of papain on microspheres was studied also.The results showed that the microspheres were spherical shape and good magnetic response. the adsorption of papain on microspheres was described by both the Langmuir adsorption isotherm and the Freundlich isotherm. Sodium dodecyl sulfate-polyacrylamide gel exectrophoresis(SDS-PAGE)showed that papain was desorbed form magnetic microspheres without denaturation.

    • >Electro-organic chemistry and industry
    • Effect of compound additives on Electroless Copper Plating Using Sodium Hypophosphite as Reducing Agent

      2012, 29(3).

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      Abstract:Abstract: The electroless copper plating was studied in a bath consisting of sodium hypophosphite as reducing agent, 2, 2′-dipyridyl and K4Fe(CN)6 as additives. The effect of various additives on the deposits was systematically investigated in this paper. The electrochemical analysis showed that oxide potential was increased by addition of 2, 2′-dipyridyl and K4Fe(CN)6 additives. On the contrary, the oxide potential was decreased. Furthermore, the deposits were characterized by scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and four-probe method. Compare with single additive, the compound additive (10 mg/L 2, 2′-dipyridyl and 4 mg/L) showed higher purity of deposit (w(Cu)= 96.27 %), brighter and more compact deposit surface. In addition, the surface resistivity of the deposits was as low as 0.0229 μΩ• m.

    • >Fine chemical intermediates
    • Synthesis of dithiodipropionamide derivatives and Study of their bacteriostatic and antifouling properties

      2012, 29(3).

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      Abstract:Three dithiodipropionamide derivatives , N’N-dimethoxypropyl- dithiodip- ropionamide(MPD),N’N-dibutoxypropyl-dithiodipropionamide (BPD),N’N-dinoctyl- dithiodipropionamide(OLPD)were synthesized from methyl acrylate in the aqueous phase and detected by infrared spectrometer and NNR spectrometer. The bioassay results showed that all the three compounds possessed good antibacterial activities, with MIC value of BPD to Escherichia Coli and Staphylococcus aureus reached 0.0625 mg/mL.Then the compounds were put into paintings made them antifouling paintings. The study of their antifouling properties by submerging in the ocean showed that they all have good qualities of antifouling. The BPD showed the best antifouling property.

    • Study on One-step Synthesis of Benzaldehyde from Styrene

      2012, 29(3).

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      Abstract:Carbonyl oxides(zwitterion) are the most reactive intermediates in ozonolysis reaction. This paper describes the trapping carbonyl oxides by amines or H2O. The direct ozonolytic conversion of styrene to benzaldehyde without the intermediacy of 1,2,4-trioxolanes(ozonides) and traditional reduction decomposition. The effect of the type of solvent, amount of solvent, reaction temperature, the flow of ozone and the kind of additive were investigated. The results show that H2O gives better reactivity than amines, different amines reactivity decreased in the order:Et3N>Bu3N>(C8H7)3N, tertiary amine>secondary amine. The appropriate reaction conditions are as follows (based on 0.05 mol styrene): 25.0 mL acetone as solvent, reaction temperature 0~5℃, the flow of ozone 200 mL•min-1, n(H2O):n(styrene)=3:1. Under above conditions, the average yield of benzaldehyde is about 96.5%.

    • >Other
    • Ultrasonic–Assisted Synthesis of N-(2- Hydroxyl ethyl)-3- methyl imidazole terafluoroborate ionic liquid and Applied for Aqueous Two-phase System

      2012, 29(3).

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      Abstract:The N-(2- Hydroxyl ethyl)-3- methyl imidazole terafluoroborate ([C2OHmim]BF4) were synthesized under the conditions of ultrasound intermittent operation.The yield was 57.69%. Compared with conventional synthesis, the reaction time was drastically reduced and the higher yield was obtained. Then [C2OHmim]BF4 was used for aqueous two-phase system (ATPS). The result shows that salt kind and its concentration had important influence on ATPS. The thermal stable ATPS can be formed as follows: 2mL [C2OHmim]BF4 , 3mL water , 0.7500g (NH4)2SO4 and 25 degree. The phase volume ratio of system was 2.4∶2.6 about PH 6~9. [C2OHmim]BF4can be reused for extraction.