• Volume 33,Issue 2,2016 Table of Contents
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    • >Functional materials
    • Synthesis, Characterization and Properties of Sulfonic /Carboxylic Type High Solid Waterborne Polyurethane

      2016, 33(2).

      Abstract (923) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A series of sulfonic acid / carboxylic acid type high solid content of waterborne polyurethane (ZW1~ZW4) was synthesized with dimethylol propionic acid (DMPA), A95 (amino sulfonate content 50%) as two hydrophilic chain expanding agent. The structures of the products were characterized by FTIR and X-ray diffractometer, the results showed that the reaction was carried out in accordance with the expected route. With the increase of the amount of sulfonic acid group, the emulsion solid content increased, particle size decreased and the distribution became wider. The Zeta potential was from -44.5 mV to -62.7 mV, but the stability of the acid was decreased. The results of film performance showed that, with the increase of the amount of sulfonic acid group, the elongation at break increased to 2800 % from 2100 %, the tensile strength decreased to 14 Mpa from 28 Mpa, and the crystallinity increased. In addition, heat resistance and water resistance decreased.

    • >Biological engineering
    • Synthesis of L-tryptophan with Escherichia coli Whole Cells Expressing Tryptophanase from Enterobacter aerogenes

      2016, 33(2).

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      Abstract:To achieve the purpose of efficient, low cost catalytic synthesis of L- tryptophan, tryptophanase from Enterobacter aerogenes was recombinant expressed in Escherichia coli BL21(DE3) using plasmid pET30a as vector. The enzymatic properties of the recombinant tryptophanase were studied, and several influencing factors of the enzyme reaction, such as temperature, initial pH, mass concentration of pyruvic acid, n (indole) / n (pyruvic acid) were investigated with pyruvic acid, indole and ammonium as substrates. Then, pyruvate fermentation broth, indole and ammonium were transformed to L-tryptophan by the recombinant tryptophanase. The results indicated that the recombinant tryptophanase was successfully expressed, and the optimal conditions for the enzymatic conversion were 35 oC, initial pH=9.0, c (pyruvic acid) =0.17 mol/L, and n (indole) : n (pyruvic acid) = 0.6:1. In 100 mL reaction mixture which contained 0.57 mol/L of pyruvic acid, after 28 h, the concentration of L-tryptophan synthesized by tryptophanase whole cell was 0.25 mol/L, by adding 6.5 mL 4.27 mol/L of indole alcohol solution. And, the mole conversion rate of indole was up to 91.8%. This study increases the catalytic activity of tryptophanase, provides a low-cost pyruvate substrate source, and provides a useful reference for industrial production of L- tryptophan.

    • >Modernization technology of traditional Chinese medicines
    • Ultrasonic-assisted Ethanol Extraction of Flavonoids from Hawthorn Seed and Their Antioxidant Activity

      2016, 33(2).

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      Abstract:Abstract: Flavonoids were extracted from Hawthorn seed under ultrasonic assistance, with ethanol as extraction solvent. The technical conditions were investigated based on single factor and orthogonal tests. Meanwhile, compared with ascorbic acid and rutin, the antioxidant activity of flavonoids was evaluated by scavenging DPPH radical, hydroxyl radical and method of Fe3+. The results showed that the optimal ultrasonic-assisted extraction condition of flavonoids from Hawthorn seed were shown as follows: ethanol volume fraction of 50%, material-to-liquid ratio of 1:25 (25 mL liquid per gram materials), ultrasonic power of 250 W, ultrasonic-assisted extracting time of about 40 min and extraction temperature at 60℃. The extraction rate of flavonoids reached 7.89%. The flavonoid extraction exhibited obviously ability of scavenging DPPH free radical and OH free radical, and showed a higher reducing capacity to Fe3+. The antioxidant activity increased with the increase of the concentration of purified flavonoids, which was superior to rutin but inferior to ascorbic acid.

    • >Water treatment technology and environmental protection
    • Preparation and Adsorption Properties of Dendrimers with Graphene as Core Encapsulated Co Nanocomposites

      2016, 33(2).

      Abstract (1038) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:Polyamidoamine (PAMAM) dendrimers with graphene as core encapsulated Co nanocomposites which was prepared by chemical reduction method. The samples were characterized by means of FTIR, TG, XRD and TEM. The effect of pH value, adsorption time and temperature conditions on the third generations of PAMAM dendrimer with graphene as core nanocomposite (G3.0-PAMAM/Co) tested for Congo red adsorption performance were studied. The results showed that G3.0-PAMAM/Co was strong magnetic adsorbent for Congo red. The adsorption process of Congo red on G3.0-PAMAM/Co could be described with the Lagrangian pseudo-second-order kinetic model. The results indicated that the adsorption process was mainly chemical adsorption. The thermodynamics of Congo red adsorption on the G3.0-PAMAM/Co followed the Langmuir adsorption equation. The maximum adsorption amount was 161.49 mg/g.

    • >Functional materials
    • Synthesis and Fluorescent Properties of the Polyamidoamine- phenoxybenzaldehyde Dendrimers

      2016, 33(2).

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      Abstract:Polyamidoamine-phenoxybenzaldehyde dendrimers of G1.0 and G4.0 were prepared with ethylenediamine as center core, methyl acrylate as branch monomer and phenoxybenzaldehyde as terminated functional groups by divergent method. Molecular structure of PAMAM-PBZA dendrimers were characterized by FTIR and 1HNMR. In additional, the fluorescent properties of PAMAM-PBZA dendrimers were studied. The results showed that Ce4 、Zn2 and Cu2 were all found to enhance the fluorescence of the PAMAM-PBZA dendrimers. Furthermore, the fluorescent emission peak of the mixed solution occur blue shift with increasing metal ions concentration, which was observed distinctly for 1.0GPAMAM-PBZA. The fluorescent intensity of PAMAM-PBZA dendrimers augmented with increasing its concentration. At the same time, the fluorescent emission peak of 1.0GPAMAM-PBZA occur red shift distinctly.

    • >Water treatment technology and environmental protection
    • Study on the Flocculant and Recycle of the Leather Auxiliary Agent by Using Cationic Keratin Flocculation

      2016, 33(2).

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      Abstract:Keratin grafted with quaternary ammonium salt cationic reagent can improve the cationic degree. In the experiment, a cationic keratin protein was prepared by introducing a quaternary ammonium into the keratin molecule. The cationic keratin was used as flocculant, the flocculation performance of several common leather auxiliaries was investigated, and the flocculation performance of the flocculant was studied. The experimental results show that the effect of some kinds of leather auxiliaries is good, among them, the flocculation effect of the dye is the best, the flocculation rate can reach more than 90%.When The floc is used as leather filling material, the thickness of the leather can reach 15.12%, the tensile strength is increased from 15.81MPa to 16.40MPa, and the elongation at break of the blank is also increased from 5 to 5, 8 to 9, and the ideal filling effect is improved.

    • Application of Amino-Functionalized MCM-41 as an Adsorbent to Remove Methylene Blue from Water

      2016, 33(2).

      Abstract (1007) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:MCM-41 was modified by 3-aminopropyl trimethoxysilane, the prepared MCM-41-NH2 was characterized by small angle X-ray diffraction, nitrogen adsorption, transmission electron microscopy and infrared spectroscopy. The MCM-41-NH2 was employed to adsorb methylene blue from water. Experimental conditions, including adsorbent dosage, initial pH of sample solution, temperature and contact time were also investigated. The increase in temperature enhanced the adsorption of MB. Results showed that the adsorption behavior could well be depicted by Langmuir equations and pseudo-second-order kinetic model.

    • Research on Preparation and Degradation Methyl Orange of Supported [Bmim]3 xPMo12-xVxO40/ SiO2 Catalyst

      2016, 33(2).

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      Abstract:The H3 xPMo12-xVxO40(x=1-3) with keggin structure was prepared by Na2HPO4, NaVO3 Na2MoO4?2H2O according to the stoichiometric coefficient. Then the [Bmim]3 xPMo12-xVxO40(x=0-3) hybrid materials was prepared by the H3 xPMo12-xVxO40(x=0-3)and the 1-utyl-3-methyl imidazole bromide ionic liquid. The IR spectra and XRD characterization showed the synthetic [Bmim]3 xPMo12-xVxO40(x=0-3) hybrid materials have keggin structure. The SiO2-supported [Bmim]3 xPMo12-xVxO40(x=0-3) hybrid materials were obtained. And the prepared samples were apply to the research of the degradation of organic dye methyl orange. The optimal reaction conditions were determined: when [Bmim]5PMo10V2O40/SiO2 loading was 50 wt.%, the temperature of reaction was 50 oC, the dosage of hydrogen peroxide was 5 mL, the catalyst was 0.5 g, the highest rate of degradation of organic dye Methyl orange reached up to 94 %. The catalyst has good regeneration performance, which can be reused at least four times. The degradation rate of Methyl orange has no significant decline.

    • >Rubber and plastics auxiliaries
    • Structural Analysis of C22-Tricarboxylic Acid Triesters though Different Reaction Conditions

      2016, 33(2).

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      Abstract:Synthesis of C22-tricarboxylic acid triesters was accomplished by methyl linoleate obtained from biodiesel and dibutyl maleate as raw meterials through different reactions. The structure and molecular weight were confirmed by FTIR、NMR and MS. Results showed that the reaction using iodine as catalyst gave the corresponding Diels-Alder adduct with cyclohexene structure. With KOH/clay catalyst, the product had a conjugated structure according to carbanion process. The radical reaction occurred without catalyst and the produced molecules also contained conjugated structures.

    • >Acrylic series chemicals
    • Al-Z-SBA-15 mesoporous molecular sieves mediated catalytic synthesis of n-butyl acrylate

      2016, 33(2).

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      Abstract:Al-Z-SBA-15 mesoporous molecular sieves were successfully synthesized by the degradation process, and the samples were analyzed by XRD, FT-IR and Py-FTIR. In this experiment, Al-Z-SBA-15 was used as a catalyst in the reaction of acrylic acid and butyl alcohol in a batch reactor. The experimental results show that with Al-Z-SBA-15 highly ordered hexagonal dielectric pore structure and surface acidity. In the esterification reaction get larger conversion rate, optimum reaction conditions of esterification: n (acrylic acid): n (n-butanol): n (hydroquinone) =1:1.4:0.4, reaction temperature and 190 ℃, the reaction time of 4 h, catalyst dosage is 6% the mass of acrylic acid. The catalyst has high catalytic activity and good reusability。

    • >Special dyes and pigments
    • Effect of Water-soluble Alcohols on the properties of Gel ink

      2016, 33(2).

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      Abstract:Water-soluble alcohol is an important part of the preparation of carbon black pigment type gel ink, the type and amount directly affect the dispersion stability of pigment paste and the performance of the gel ink. The effects of compatibility of resin dispersion SMA (styrene-maleic anhydride resins) with six kinds of water soluble alcohol on carbon black slurry dispersion stability as well as the value of thixotropic, moisturizing and writing performance of the gel ink was investigated. The results showed that, the compatibility of PEG-200, PEG-400 and glycerol was better to disperse resin SMA. PEG-400 has the best dispersion stability to the carbon black slurry. Water-soluble alcohol which compatible with the dispersion resin SMA well could have a greater impact on the value of thixotropic of the gel ink with its content changes. Added glycerol, ethylene glycol and PEG-400 in the gel ink could obtain better moisturizing effect. The gel ink prepared with glycerol, PEG-200 and PEG-400 showed stable, uniform lines and good writing properties.

    • >Surfactants
    • The Influence of Amphiphilic Alginate Derivate on the Aggregation Behavior of TiO2 Nanoparticles in Aqueous Solution

      2016, 33(2).

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      Abstract:the stability of TiO2 nanoparticles dispersion system was got by dodecyl sodium alginate (NaAlg-Dode) adsorbing on the TiO2 nanoparticles. The particles size, zeta potential and rheological properties of suspension system were measured by means of Fourier transform infrared spectrometer (FTIR), Dynamic light scattering (DLS) and Rheometer. The influence of NaAlg-Dode on the aggregation behavior of TiO2 nanoparticles in aqueous solution and rheological property were researched at various pH values. Experimental results showed that NaAlg-Dode was conducive to the stability of TiO2 nanoparticles dispersion system within the scope of pH=4~8. The average size of TiO2 particles from 2.5祄 down to around 500 nm and the surface Zeta potential of particles reduced from 0 mV to about -40mV at pH=6.3.At the same time the shear stress of TiO2 nanoparticles dispersion system increased gradually with the addition of NaAlg-Dode, which suggested that the interaction between particles enhanced. Therefore, the stable mechanism of TiO2 nanoparticles dispersion system by NaAlg-Dode improving: NaAlg-Dode molecules was able to promote particles stable disperse in aqueous solution via changing the zeta potential and space steric of TiO2 by electrostatic interactions, hydrogen bonding and hydrophobic function.

    • >Adhesives
    • Synthesis and Properties of a Novel Bis-phenylbiguanide as Latent-curing Agent for Epoxy Resin

      2016, 33(2).

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      Abstract:Dicyandiamide is commonly used as curing agent in epoxy resin. A new latent curing agent for epoxy resin was synthesized to improve the comprehensive performance of dicyandiamide curing agent. The chemical structure of curing agent was characterized by FTIR,1H NMR. The optimum ratio of epoxy resin and curing agent was 5:1 under the assistance of DSC. The optimum curing temperature and storage time in room temperature was 130 ℃ and 30 d obtained by curing activity test and gel test, respectively. Tensile strength of cured epoxy resin was 38.07 MPa, which is analyzed by tesion test. Thermal decomposition temperature of the cured epoxy was exceeded 270 ℃ with the help of TG. Comparing with dicy/epoxy resin curing system, the new agent has better compatibility with epoxy resin. Its latency performance was fine and curing temperature was decreased more than 30 ℃ and the cured epoxy has excellent mechanical properties and good thermostabilities.

    • >Fine chemical intermediates
    • Synthesis and Study on Properties of An MR/Fluorescence Imaging Molecular Probe Using LNCS As Carrier

      2016, 33(2).

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      Abstract:Abstract:Low degree of polymerization (DP) and narrow molecular weight distribution chitosan (LNCS6) (DP=6, Mw/Mn = 1.08) was prepared with the method of microwave-assisted oxidative degradation. It was used as a carrier molecular to link 7-hydroxyl-8-formylcoumarin (CA) as the fluorescence emission group, diethylenetriaminepentaacetic acid (DTPA) as complex of gadolinium ions to get the final product Gd[DTPA/CA-LNCS6] as an potential magnetic resonance (MR) /fluorescence bifunctional imaging molecular probe. The magnetic resonance imaging (MRI) efficiency and fluorescence properties were studied, and the binding constants and thermodynamic parameters between Gd[DTPA/CA-LNCS6] and bovine serum albumin (BSA) were measured by isothermal titration calorimetry (ITC). The results showed that Gd[DTPA/CA-LNCS6] exhibited higher MRI relaxation 〔r1=13.71 L/(mmol ∙ s)〕, which was well above the clinically used Magnevist 〔r1=3.63 L/(mmol ∙ s)〕; Meanwhile, the product had significant fluorescence characteristics at 438nm, and the binding constants between Gd[DTPA/CA-LNCS6] and BSA was over 104 which was suitable for blood transportation. This work has good reference for the synthesis of probes like such type of fine chemical.

    • Synthesis and Characterization of 2-alkylimidazolines by Pressure- Fractionation Method

      2016, 33(2).

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      Abstract:2-Alkylimidazolines were prepared from organic acid including n-pentanoic acid, n-hexanoic acid, lauric acid, stearic acid and 1,2-ethylanediamine by pressure-fractionation method,respectively.The target compounds’ chemical structures were characterized by 1HNMR and FT-IR.The results showed that the preferred synthetic conditions were as following: n(organic acid):n(1,2-ethylanediamine)=1:5,reaction at 185℃ and fraction at 155℃ under the pressure of 0.25MPa.The 2-alkylimidazolines were obtained with high purity and excellent yield(86%~98% based on organic acid).

    • >Modernization technology of traditional Chinese medicines
    • Sonication-assisted Extraction of Polysaccharide from Pyrus Nivalis and Its Application in Cigarette

      2016, 33(2).

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      Abstract:With fresh pyrus nivalis as raw materials, studied the effects of ultrasonic power, temperature, solid-liquid ratio, and time on the extraction efficiency of polysaccharose using sonication-assisted extraction method. On the basis of single factor experiment, the orthogonal experiments were designed to optimize the extraction process. Moreover, polysaccharide was applied to cigarettes. The results of orthogonal experiments showed that : The optimal conditions were solid-liquid ratio 1:4 (g/mL), temperature 50 ℃, time 50 min, ultrasonic power 160 W; Under this condition, the extraction yield of polysaccharide was 3.18%. The results of experiment with polysaccharide as cigarettes flavor indicated that polysaccharide extracted from pyrus nivalis can cover the offensive taste, soften smoke gas, reduce the stimulus, enrich the flavor of smoke, produce saliva and slake thirst.

    • Chemical composition, antioxidant and cytotoxic activity of the essential oil from Phellodendron amurense fruits

      2016, 33(2).

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      Abstract:The essential oil of the fruit of Phellodendron amurense was extracted with steam distillation and its constituents were analyzed by gas chromatography-mass spectrometry (GC-MS). The antioxidant activities were screened by DPPH radical-scavenging and β-carotene bleaching assays. The cytotoxic activity of the essential oil against HeLa, A-549 and BGC-823 human tumor cell lines was investigated by Sulforhodamine B (SRB) method. GC-MS analysis identified 39 components of the essential oil. The major constituents were β-pinene, β-caryophyllene oxide, 3-methylene-4-isopropenylcyclohexanol and cembrene. The essential oil showed weak antioxidant activity in the DPPH and β-carotene tests. The essential oil showed no cytotoxic activity on A-549 and BGC-823. However, it is worth to note that the essential oil showed high cytotoxicity against HeLa cancer cell lines.

    • >Catalysis,separation and purification technology
    • Preparation of monoglycerides from fatty acid methyl ester and glycerol solution catalyzed by solid base catalyst

      2016, 33(2).

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      Abstract:Monoglycerides were produced from fatty acid methyl ester and glycerol solution catalyzed by La2O3/MgO. The purification and characterization of products were carried out by thin layer chromatography (TLC), high performance liquid (HPLC), infared spectroscopy(FTIR), and nuclear magnetic resonance(1H NMR). The influence of some reaction conditions on the yield of monoglycerides was investigated. The results show that IR characteristic of monoglycerides was consistent with literature reported, and 1H NMR indicated that the product was a mixture of linoleic acid monoglyceride and palmitic acid monoglyceride. The optimum reaction conditions as follows: reaction temperature 240℃, catalyst amount 0.75% (based on the mass of fatty acid methyl ester), moral ratio of fatty acid methyl ester to glycerol 1:2 (mole ratio) and the reaction time 2.5h, and the yield can reach 70.53% under the condition.

    • >Drug and cosmetic materials
    • Synthesis of Two C2 Symmetrical Cyclic Decapeptide

      2016, 33(2).

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      Abstract:With leucine and phenylalanine as the raw material, we synthesized two C2 symmetrical cyclic decapeptide compounds Q10-1 and Q10-2 in assistance of protection and deprotection of amino acids, N-methyl and coupling, and TBTU / HATU / DEPBT working as cyclization reagents. The cyclization yield reached 31.6% and 39%. The products were isolated and purified by HPLC, which the purity of product was up to 98%. The compound structures were characterized by means of 1HNMR, 13CNMR and ESI-MS.

    • Synthesis and Antitumor Activity of N-Pyridyl-2-(4-Aryloxyphenoxy) Propionamide

      2016, 33(2).

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      Abstract:A series of novel N-pyridyl-2-(4-aryloxyphenoxy) propionamide compounds were designed and prepared from the starting materials of (R)-2-(4-hydroxyphenoxy) propanoic acid and chloropyridine, and the structures were characterized by 1HNMR, 13CNMR, LC/MS, IR and elemental analysis.The effects of reaction conditions on the steric configuration were studied. Preliminary bioassay indicates that some compounds posed antitumor activity to A549 and Hela cells in vitro by MTT method. In particular, N-(3-nitropyridin-2-yl)-2-[4-[(6-chloroquinoxalin-2-yl) oxy]phenoxy] propanamide (Ⅳf) (IC50 = 0.007 mM) was more effective against A549 than drug cisplatin (IC50 = 0.026 mM).

    • Synthesis, Crystal Structure, and Interaction with Bovine Serum Albumin of Pyrazole-3-carboxylic Acid of Cobalt Complex

      2016, 33(2).

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      Abstract:A new complex have been synthesized by solvent method using pyrazole-3-carboxylic acid as ligand reacting with CoCl2?6H2O metal salt. The complex's structures was characterized by single-crystal X-ray diffraction. The complex crystalized in monoclinic system, group is P21/c, a = 5.0994(2) ?,b = 11.3955(5) ?,c = 9.3680(4) ?, α = 90?,β = 95.925(5)?,γ = 90? Co(Ⅱ) center six-coordinated by two carboxylate O atoms, two pyrazole N atoms, and two O atoms of two water molecules, producing a octahedral coordination environment. The interaction between complex and BSA was studied by UV–Vis spectra and fluorescence spectroscopy. The results showed that the interaction between complex and BSA were exquisite. The quenching process could be described with static quenching mechanism, with quenching rate constant being 3.54?012 L?mol?1?s?1, binding constant being 7.06154?05 L?mol?1 and binding site number being 1.2595.

    • Synthesis and Biological Evaluation of 7-Hydroxyflavones

      2016, 33(2):0-0.

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      Abstract:Eight 7-hydroxyflavones were synthesized and their strcutures were confirmed by 1H NMR and ESI-MS. Their acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) inhibitory activities was determined by the Ellman method. The result showed that the synthesized compounds had potent AChE inhibitory activity at 20 umol/L, compound IIIh displayed the most potency for AChE inhibition (34.71%) which was slight better than rivastigmine. The results indicated that these 7-hydroxyflavones may provide a useful template for the development of anti-AD agents.