• Volume 32,Issue 10,2015 Table of Contents
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    • >Functional materials
    • Chemical Coprecipitation Synthesis of Mesoporous Fe2O3 and Study of Their Adsorption Performance

      2015, 32(10).

      Abstract (837) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Mesoporous Fe2O3 nanoparticles were synthesized by a gas-liquid chemical precipitation method. The thermodynamics and the kinetics of Fe2O3 adsorption on Congo red (CR) were studied by the set of equilibrium experiment. The results showed the adsorption isotherms were modeled by Langmuir model, and the parameters indicated that the adsorption was strongly dependent on temperature and the adsorption of CR increased with increasing temperature of the system. The calculated parameters indicated the adsorption process was determined as an endothelium process and a spontaneous process. Furthermore, the adsorption process reached equilibrium in 6 hours, and the kinetics adsorption of CR can be described by pseudo-second-order rate very well.

    • Preparation of Poly(ethylenimine) Functional Fe3O4 Nanoparticles

      2015, 32(10).

      Abstract (1110) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this paper, oleic acid coated Fe3O4 nanoparticles were functionalized by 3,4-Dihydroxybenzenepropionic acid (DHCA) in tetrahydrofuran (THF). After conjugated by polyethylene (PEI) the functionalized Fe3O4 nanoparticles were well dispersed in water. The morphology, size distribution, magnetic properties and potential of the magnetic particles were characterized by TEM FT-IR, VSM, and Zeta potential, respectively. The results show that this method is simple, the PEI functionalized Fe3O4 nanoparticles have superparamagnetic properties and excellent dispersion.

    • Synthesis of Polylactide Copolymers with Controllable Structure and Self-Assembly Behavior and Their Glucose-Responsive Properties

      2015, 32(10).

      Abstract (636) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Two types of glucose-responsive copolymers poly(lactide)-block- poly(dimethylamino-2-ethyl methacrylate)-block-polyvinyl phenylboronic acid (PLA-b-PDMAEMA-b-PVBA) and poly(lactide)-block-(poly(dimethylamino-2-ethyl methacrylate)-co-polyvinyl phenylboronic acid) [PLA-b-(PDMAEMA-co-PVBA)] were synthesized by one-step and two-step Reversible Addition-Fragmentation Chain Transfer Polymerization (RAFT), respectively, via polylactic acid (PLA) macromolecular as a chain transfer agent. These chemical structures of the copolymers had been controlled. Assembly behavior studies indicate that PLA-b-(PDMAEMA-co-PVBA) could self-assemble to form micelles in selective solvents, while PLA-b-(PDMAEMA-b-PVBA) could form micelles in glucose solvent only. Both micelles showed a good glucose-responsive property, and their particle size and morphology changed with the variation of glucose concentration.

    • Study of Adsorption and Preparation of Ginsenoside Re Molecularly Imprinted Monolithic Column

      2015, 32(10).

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      Abstract:The molecularly imprinted monolithic column(MIMC) was synthesized using α-methacrylic acid as functional monomers, ethylene glycol dimethacrylate as cross-linker, the mixture of isopropanol and dodecadol as porogenic reagent and Ginsenoside Re as template molecules by in-situ polymerization. The performances of separation and adsorption of MIMC were investigated, the results of research indicated that optimal mobile phase was methanol and water (40:60, v/v), separation factor 1.769, the adsorption isotherm followed the anti-langmiur isotherm model by frontal chromatography, saturated adsorption capacity was 0.247mg/g. MIMC has special molecule recognition ability to Re. The result of scanning electron microscopy(SEM) showed that the unique porous structure was formed in the polymer, which was beneficial to the flow of mobile phase and the mass transfer of template molecules.

    • Synthesis and Characterizations of Dodecyl/phenyl Modified Polysiloxane

      2015, 32(10):0-0.

      Abstract (1215) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:According to optimization of synthesis methods, we prepare a series of different alkyl/phenyl ratio comodified silicone oil (PAPMS) with high hydrogen silicone oil (UC202), methyl phenyl hybrid ring (DMe,Ph), hexamethyldisiloxane (MM), and 1-dodecene as raw materials. The effects of synthesis methods and molecular structure of PAPMS on their thermal stability, density, viscosity (index), homogeneity with mineral oil and abrasion resistance are studied in details. The test results show that phenyl groups are beneficial to enhance thermal stability, and introducing long carbon chain alkyl groups lead to enhancement in weight residue and viscosity, and reduction in viscosity index. The PAPMS with alkyl content of 0.90 mmol/g can form homogeneous liquid with mineral oil. When it is added into mineral oil with 10 wt.%, the wear scar diameter is reduced from 0.64mm to 0.55 mm.

    • >Surfactants
    • Properties of Several Didecyl Quaternary Ammonium Salts with Novel Counterions

      2015, 32(10).

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      Abstract:Various quaternary ammonium salts with formate (DDAF), acetate (DDAA), propionate (DDAP), ethacetate (DDAE), chloridion (DDAC) and nitrate (DDAN) being counter ions were researched. The surface activities and potential application were measured. We find it is interesting to notice that DDAF, DDAA, DDAP and DDAE have the higher value of the critical micelle concentration and the minimum surface tension than traditional surfactant DDAC, and DDAN shows higher surface activities than traditional surfactant DDAC. DDAF, DDAA, DDAP and DDAE show excellent emulsifying performance and wetting power ability, while its foaming power is low. In addition DDAN has higher foaming power, emulsifying performance and wetting power than DDAC. Moreover, the bacteriostatic tests show that DDAF, DDAA, DDAP, DDAE and DDAN have greater efficacy than DDAC against E. coli and S. aureus.

    • >Biological engineering
    • A Preliminary Study on Fermentation Optimization and Biocatalytic Properties of Fungal Nitrilase

      2015, 32(10).

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      Abstract:The culture conditions of recombinant E. coli harboring fungal nitrilase were systematically investigated in the level of shake flask, including medium composition, inducers, induction condition, pH and temperature. The results showed that a modified SOC medium containing trace elements was used as the fermentation medium with glycerol as the carbon source and peptone plus yeast extract as the nitrogen sources. The preferred inoculation amount was 0.5% (v/v). The induction for nitrilase production was carried out at 25°C and pH 7.5 with 0.5 mmol/L IPTG as the inducer for 12 h. The enzyme activity of the nitrilase were substantially improved through optimization and the total activity reached up to 3.8 U/mL, which was 3-fold higher than that of the initial level (0.84 U/mL). Subsequently, the nitrilase production in a 5-L stirred tank fermentor was determined and proved to be almost the same as that of shake flask. Preliminary study on biocatalytic properties of resting cells showed that the optimum reaction temperature and pH of the fungal enzyme were 45°C and pH 7.2.

    • >Catalysis,separation and purification technology
    • Preparation and CO2 Adsorption Property of Silica-immobilized Imidazolium Ionic Liquid Polymers

      2015, 32(10).

      Abstract (1005) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The grafting polymerization of ionic liquids on silica surface was performed by the solution polymerization and surface-initiated atom transfer radical polymerization methods. The silica-immobilized ionic liquid polymers were characterized via FTIR, TG and SEM analysis. The CO2 adsorption property and the selectivity of CO2/N2 were investigated. The CO2 thermodynamic study and diffusion performance of silica-immobilized ionic liquid polymers was also discussed. The results show that loading amount of ionic liquid made by the surface initiated ATRP method is much higher than that of by the solution polymerization method. The sample prepared by solution polymerization method presents more developed porous structure, and the CO2 adsorption of them can reach 4.54 wt% at 273 K and 0.1 Mpa. The CO2/N2 selectivity of the silica-immobilized ionic liquid polymers is much better than that of the bare silica. The silica-immobilized ionic liquid polymers exhibit good CO2 sorption/desorption cycle capacity. The sorption of CO2 on silica-immobilized ionic liquid polymers is likely due to physisorption.The diffusion coefficients of CO2 adsorption on silica-immobilized ionic liquid polymers are much higher than that of the ionic liquid polymers.

    • Kinetics of Yohimbine Hydrochloride Adsorption onto Strong Acid Cation Exchange Fiber

      2015, 32(10):0-0.

      Abstract (1547) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The features of yohimbine hydrochloride absorbing on the strong acid cation exchange fiber were characterized by SEM and IR. Then the absorption kinetic data of yohimbine hydrochloride by strong acid cation exchange fiber were fitted by the pseudo-first-order kinetic model and pseudo-second-order kinetic model. The adsorption process was better described by the pseudo-second-order model,and the apparent activation energy of reaction (Ea) was 14.39 kJ•mol-1. The absorption speed controlling step was liquid film diffusion. The rate constant of Boyd film diffusion kB increased from 0.170 to 0.186 min-1 and the effective diffusion coefficient D increased from 2.755 10-11 to 3.017 10-11m2s-1 with the increase of initial yohimbine hydrochloride concentration from 100 to 300 mg/L.

    • >Drug and cosmetic materials
    • Syntheses and Antitumor Activities Evaluation of Styryl Quinoline Derivatives

      2015, 32(10).

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      Abstract:Ten styrylquinoline derivatives were prepared from anilines and aromatic aldehydes in two steps. Firstly, four 2 -methylquinolines have been synthesized from anilines and (E)-2-butenal using hydrochloric acid as catalyst. Then styrylquinolines were obtained with 64% ~ 78% yield by refluxing 2-methylquinolines and aromatic aldehydes in glacial acetic acid. The structures of all synthesized compounds were confirmed by 1HNMR, MS and IR. The antitumor activity of these compounds against A 549 and HCT 116 cell lines was evaluated by MTT assay in vitro. The results showed that compounds Ⅱc exhibited high activity against A 549 and HCT 116 cell lines with IC50 value of 9.77 and 9.66 μmol·L-1, respectively, and compounds Ⅱd exhibited high activity against HCT 116 cell lines with IC50 value of 9.80 μmol·L-1 .

    • Rheological Properties of Straw Carboxymethyl Cellulose and Application in Dyeing with Curcumin

      2015, 32(10).

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      Abstract:Ethanol nitrate method was used to extract the cellulose from waste crop stalks, different substituted ratios of carboxymethyl cellulose was prepared by etherification reaction. The rheological properties of CMC aqueous solution was studied by DHR-2 rheometer, Finally the CMC was used in dye hair with curcumin, and compared with common thickeners on the marker. The results show that CMC solution behaved like pseudoplastic fluid and had the nature of shear thinning. Its system viscosity increased with the larger mass fraction and average substitution degree. The mass fraction of CMC solutions had little influence on linear viscoelastic range which strain less than 70 percent of the area. CMC aqueous solution system had good thixotropy and its viscosity step changed with the step changes of shear rate. CMC could make curcumin easy to dye, and do not severely injure hair, the brightly dying performance, high hair strength and color fastness were obtained after dyed.

    • >Rubber and plastics auxiliaries
    • Synthesis and Application of Flame Retardant Polydimethyl Silicon Acid Terephthalic Diester

      2015, 32(10).

      Abstract (755) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A kind of polymeric silicone flame retardant charring agent, polydimethyl silicon acid terephthalic diester was synthesized from dichlorodimethylsilane and hydroquinone. The effects of reaction time and reaction temperature on the yield were investigated. The optimum reaction conditions were: n(dichlorodimethylsilane):n(hydroquinone)=1:1, dropping dichlorodimethylsilane to hydroquinone at the temperature of 40℃, keeping the reaction at 70℃ for 7h. The target products would be received after purification, its yield was 96.7%. The structure and flame retardance of the product were characterized by means of FTIR、1H-NMR、TG-DTA and limiting oxygen index technique. The results showed that the product had a good charring flame retardant effect when applied to PBT or PP. And its complex formulation with APP had good synergistic effects.

    • >Dyeing and finishing auxiliaries
    • Organic quaternary ammonium salt polymer synthesis and applications of antibacterial fabric softener

      2015, 32(10):0-0.

      Abstract (748) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A new type of organic silicon long chain organic quaternary ammonium salt fabric softener (VPEQ18) was synthesized by solution polymerization using hydroxypropyl acrylate (HPAA) and allyl polyether epoxy (APE500) and 18 tertiary amine as raw materials, andazodiisobutyronitrile (AIBN) as initiator. Using infrared spectrum to characterization, and analysis shows that VPEQ18 with expected design chemical structure. Using softness, crease elasticity tester, and automatic color difference meter to research the application performance of VPEQ18, and eventually determine the cotton size is 6cm?0cm, VPEQ18 emulsion dosage (30%) for 3 g, curing temperature is 180℃, the curing time of 90 s process conditions, fabric can reach the ideal soft, smooth, antibacterial effect.

    • Synthesis and application of softener CAPES for raw silk

      2015, 32(10):0-0.

      Abstract (1021) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract:A carboxyl-modified polyether silicone(CAPES) was prepared by using epoxy terminated siliconeoil(α,ω-ESO),amine terminated polyether and maleic anhydride(MAn) as raw materials.The self-made carboxyl polyether silicone(CAPES) was emulsified as a white translucent blue emulsion with the nonionic surfactant isomeric alcohol ethoxylates,and the emulsion used for raw silk soft finishing.The chemical struc-ture of CAPES,its emulsion and membrane configuration on silk fiber surface were characterized by means of infrared spectroscopy(IR),nanoparticle size analyzer,Zeta potential analyzer and scanning electron microscopy(SEM).The effects of CAPES Solution pH,immersion time and silicone emulsion dosage on its treatment performance toward silk fiber was also discussed,The results showed that the average particle size of the CAPES emulsion was 84.6nm,its potential was -21.5mV,and it had a good filmforming ability on silk fabric surface. The treated silk achieved satisfactory effects when CAPES Solution pH is 6,immersion time is 30min and the dosage of CAPES is about 5g/L.

    • >Oil field chemicals and petroleum additives
    • The Synthesis and Application of New Organic Amine Boron Crosslinker AB-1

      2015, 32(10).

      Abstract (1062) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Based on the raw material boric acid, n-butyl alcohol, ethylene alcohol and tetraethylenepentamine, one kind of new organic amine boron crosslinker AB-1 is prepared to specify to hydroxyl alcohols fracturing fluid system. The optimal synthesis progress of crosslinker is determined, and some influence factors of the synthesis progress are also studied. The results have proved that: the first step--esterfication reaction, the mass fraction of boron acid is 15%, ethylene alcohol is 35%, n-butyl alcohol is 25%, under 120℃ for one hour; the second step--complexation reaction, tetraethylenepentamine is 10%, pentaerythritol is 5%, sodium hydroxide is 5~10%, under 150℃ for two hours; then crosslinker AB-1 is collected. The behavior evaluation results of fracturing fluid have proved that: hydroxypropal guar gum can be crosslinked with crosslink agent AB-1 with favorable delay crosslinking behavior, shear and temperature resistance behavior, solid-carrying behavior and gel breaking behavior.

    • Preparation and Rheological Property of Fenugreek Gum Thickener Modified by cis-Butenedioic Anhydride

      2015, 32(10).

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      Abstract:The fenugreek gum modified by maleic anhydride was synthesized with fenugreek gum (FG) as material ,using maleic anhydride (MAH) as the esterification reagent and N-bromobutanimide as catalyst. The optimum reaction condition of MAFG was obtained as follows: MAH and FG in mass ratio 0.35:1, 60℃ reaction temperature, 4 hours reaction time. The structure of MAFG was characterized by means of FT-IR, XRD, meanwhile, the rheological property of the aqueous solution and the gel of MAFG were discussed. The results showed that the modification can reduce the crystallinity. Compared to FG, MAFG has better thickening property. The rheological property of the gel of MAFG was better than FG. The gel of MAFG has good temperature and shear stability properties.

    • >Special dyes and pigments
    • Study on Syntheses and Performances of Bitriphenylamine-doner Dyes

      2015, 32(10).

      Abstract (1031) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Three organic dyes include monotriphenylamine-doner dye ST-1 and bitriphenylamine-doner dyes DT-1, DT-2 were synthesized which contained cyanoacrylic acid moieties as electron acceptors,and benzene or thiophene derivatives as conjugated linker. The structures of the molecules were characterized by means of NMR,FTIR and MS.The effects of increasing the amount of donors and prolonging its conjugated linkers on the photo-physical,electrochemical and photovoltaic properties of the dyes were studied.The results indicate that DT-1 and DT-2 can effectively enhance open-circuit voltage of DSSCs due to increase the amount of triphenylamine donors. But the absorption spectrum of DT-1 is weaker in visible area, which causes a decreasing short-circuit current. However, when thiopene is replaced by bithiophene to construct the conjugated linker, the absorption spectrum of DT-2 becomes stronger in visible section, thus Short-circuit current has been improved remarkably, and exhibit highest power conversion efficiency of 3.91%.

    • >Fine chemical intermediates
    • Synthesis and Characterization of 5,15-bis-Pentafluorophenyl-10,20-di-(2-pyridyl-) Porphyrin

      2015, 32(10).

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      Abstract:A novel compound of 5,15-bis-pentafluorophenyl-10,20-di-(2-pyridyl-) porphyrin was synthesized by two steps. The effects of the dosage of catalytic agent, temperature and time on the yield of target compound were investigated. The results show that the yield of the target compound reaches 33.6% when the molar ratio of catalyst to pentafluoro-benzaldehyde is 1:15, the temperature is 145 ℃ and the reaction time is 1 h. The target product was characterized by MS, IR, UV-Vis, 1HNMR, 19FNMR and EA. Meanwhile, It displays intense fluorescence emission with maximum at 711 nm upon 470 nm excitation at room temperature, indicating that they may be candidate for luminescent material.

    • Synthesis of 3-Methylamino-1,2-Propandiol Process Conditions Use Solid Base Catalyst

      2015, 32(10).

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      Abstract:The 3-methylamino-1,2-propandiol was synthesized by solid-base carrying triethylamine as catalyst, the 3-chloro-1,2-propanediol and methylamine as the raw materials. The influence factors on this reaction were investigated by orthogonal test and single factor analysis. It was indicated that the best process conditions for this reaction were as follows: the mole ratio of 3-chloro-1,2-propanediol to methylamine (converted into 100%) was 1:8, reaction temperature was 60 ℃, reaction pressure was 0.20 MPa, the reaction time was 3.5 h. Under the optimum reaction conditions, The synthesis yield of 3-methylamino-1,2-propandiol was 91.9%. The product was characterized by elemental analysis, gas chromatography and infrared spectrum method, and the product purity was 99.5% at least.

    • One Step Synthetic Method of 2-Hydroxy-1, 4-Cineole Catalyzed by Peroxoheteropolyoxomolybdotungstate

      2015, 32(10).

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      Abstract:2-Hydroxy-1,4-cineole(Ⅱ) is the intermediate of a botanical cineole derivative herbicide Cinmethylin. It can be obtained from terpinen-4-ol(Ⅰ) via an one-step synthetic method by using peroxoheteropolyoxomolybdotungstate (Cat-PMo2W2O24) as redox–acidic bifunctional catalyst in presence of mass fraction 30 % H2O2 aqueous solution. There were obvious effect of various reaction parameters such as solvent type, catalyst dosage, and the amount of hydrogen peroxide on the phase state, acidity or acid amount of reaction system, resulting in the changes of the conversion rate ofⅠand the yield of Ⅱ. Under the optimum conditions(Ⅰ,12 mmol; chloroform as solvent,5 ml; catalyst dosage,4.20 %(mass fraction, based on the substrate);temperature,25℃; the molar ratio of H2O2 toⅠ, 0.91; reaction time, 30 min.), 96.2% conversion of Ⅰ with 70.1% yield towards Ⅱ was achieved.

    • >Other
    • Research on preparation and stability of 4-Chloromethyl styrene/ Styrene miniemulsion

      2015, 32(10).

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      Abstract:In this paper, a series of p-Chloromethyl styrene(p-CMS)/Styrene(St) miniemulsion was prepared with the ultrasonication method. Effect of amount of emulsifier, ultrasonic time, ultrasonic power, and costabilizer content on preparation of miniemulsion and effect of p-CMS/St mass ratios on its stability were investigated. The results show that a miniemulsion with an average diameter as low as 99 nm and a polydispersity index of 0.12 was achieved, under the condition that the concentration of sodium dodecyl sulfate is 10 mg/mL, ultrasonic time is 24min, ultrasonic power is 400W and the mass ratio of hexadecane to monomer is 5%. The stability of the miniemulsion decrease with incerase the mass ratio of p-CMS/St, and Ostwald ripening may be the prime reason for the instability of p-CMS/St miniemulsion. ratio of p-CMS/St, and Ostwald ripening may be the prime reason for the instability of p-CMS/St miniemulsion.