• Volume 33,Issue 12,2016 Table of Contents
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    • >Fine chemical intermediates
    • Synthesis, Characterization and Interaction with Bovine Serum Albumin of Schiff Base Containing Dihydropyrimidinone

      2016, 33(12).

      Abstract (811) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A series of Schiff base containing dihydropyrimidinone (3a-3g) has been synthesized by condensation reactions of aromatic aldehydes with 4-(4-aminophenyl)-5-ethoxycarbonyl-6-methyl-3,4-dihydropyrimidone, which prepared from ethyl acetoacetate, 4-nitrobenzaldehyde and urea through condensation and reduction reactions. The compounds were characterized by IR、1H NMR and 13C NMR. The interactions between 3g and bovine serum albumin (BSA) were investigated using fluorescence spectroscopy at different temperatures, the results revealed that 3g can effectively quench the intrinsic fluorescence of BSA; the corresponding thermodynamic parameters shown that the action forces were mainly hydrophobic interaction; the binding distance was estimated to be about 2.59 nm according to F鰎ster’s non-radioactive energy transfer theory; the synchronous fluorescence showed that the 3g induced conformational changes of BSA

    • >Functional materials
    • Synthesis and Aggregation-Induced Emission Properties of Tetraphenylene Derivatives

      2016, 33(12).

      Abstract (2047) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Two fluorescent molecules with aggregation-induced emission (AIE) feature, 5-(4-(1,2,2-triphenylvinyl)phenyl)-2,2'-bipyridine (Bpy-1TPE) and 5,5'-bis(4-(1,2,2-triphenylvinyl)phenyl)-2,2'-bipyridine (Bpy-2TPE), were synthesized from 5-bromo-2,2'-bipyridine, 5,5'-dibromo-2,2'-bipyridine, and 4-(1,2,2-triphenylvinyl)phenylboronic acid via Suzuki coupling reaction. All proposed structures were characterized by 1HNMR, 13CNMR and elemental analyses. Their UV-vis absorption, fluorescence, AIE and piezochromic properties were investigated with the aim of understanding the structure-property correlations. Compared with Bpy-1TPE, Bpy-2TPE with two TPE units has a larger conjugation and a symmetrical charge distribution, which exhibited a lower energy gap width, and a red-shift of the emission from 483 to 490 nm in CH2Cl2. Bpy-2TPE showed obvious AIE and piezochromic properties, the emission maximum of its solid sample was red shifted from 485 to 500 nm after grinding.

    • Preparation of Pomelo Peel Powder Grafted P(AA-AM) Resin and its Urea Load/Release Properties

      2016, 33(12).

      Abstract (1203) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:superabsorbent polymer composite (PP-SA) was synthesized from the pomelo peel powder (PP) and poly acrylic acid-co-acrylamide(P(AA-AM)) using solution polymerization method. The components of PP were analyzed and the mechanisms for formation of PP-SA were proposed. The molecular structure characteristic of PP-SA was characterized by FTIR. It shows that P(AA-AM) was successfully grafted on PP. The TG result indicates that the thermostability of P(AA-AM) is strengthened by introducing PP into P(AA-AM). The properties of urea solution retention and urea load/release were researched systematically. The retention capability of PP-SA in 6 g/L urea solution was the highest, reaching to 362 g?g-1. The urea loading ratio of PP-SA swelling in urea solution of 10 g/L was 66.7%. And its urea release ratio can reach to 74% in distilled water.

    • A Fe3+ Schiff Fluorescence Probe based on Diphenyl Ketone

      2016, 33(12).

      Abstract (919) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this paper, a Schiff base L was prepared from 2,4-dihydroxyl diphenyl ketone (UV-0) and o-phenylenediamine. It was characterized by FT-IR, 1H NMR and HRMS. In the solution of V(EtOH):V(HEPES)=95:5 at pH 7.2, L displayed an “on-off” recognition ability for Fe3+ with good selectivity and without obvious disturbances by other metal ions. In the concentration range of Fe3+ from 0 to 7.0  10-5 mol/L, the intensity of this solution showed a good linear relationship with the concentration of Fe3+. According to this curve, the detection limit of L for Fe3+ was calculated to be 1.9410-7 mol/L, and the binding constant between them was 2.0104 (mol/L)-1.

    • Preparation And Graphene Modification of Nano Perovskite La1-xSrxMnO3

      2016, 33(12).

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      Abstract:The perovskite La1-xSrxMnO3 was prepared by sol-gel method under ultrasonic assistant with lanthanum nitrate, strontium nitrate and manganese nitrate as raw materials and doped with grapheme. The La1-xSrxMnO3 and Graphene/La1-xSrxMnO3 composites were characterized by XRD, SEM-EDS, DLS. The effects of calcination temperature and pH on the crystal structure were investigated. We also have investigated the effect of graphene modification on properties of materials. The results show that the La1-xSrxMnO3 prepared by the sol-gel method under ultrasonic assistant have good dispersibility, uniform particle size about 210nm. XRD analysis that Graphene doping does not change the La1-xSrxMnO3 metallography. The first charge and discharge results show that: Compared with pre-modification, the discharge capacity of the Li-air battery with the composite modified by graphene as catalyst was improved to 7900mAh/g from 4300mAh/g.

    • >Starch chemicals
    • Effect of Ultrasound Treatment on Properties of Oxidized Cassava Starch

      2016, 33(12).

      Abstract (1065) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this work, the ultrasound was applied to oxidation of cassava starch, and the properties of the oxidized starch were studied,moreover, the properties of oxidized starch with and without ultrasound, and natural cassava starch (NCS) were compared. The results show that, compared to NCS,the solubility, transparency and whiteness of oxidized starch increased by 4.55 times, 3.38 times and 1.23% respectively, and retrogradation and gelatinization enthalpy value decreased by 99.05% and 45.79%, oxidized starch prepared by above two treatments had good capacity of forming film,its film was uniform and resilient, but the NCS was very difficult to form film. Under the same conditions, the properties of oxidized starch could be improved by ultrasound significantly, the solubility, transparency of the oxidized starch under ultrasound were increased by 97.23%, 33.68% respectively, whiteness had a 0.26% improvement(they had significant difference at 5% level),the retrogradation and gelatinization enthalpy value were reduced by 78.80% and 24.13%. So, ultrasound can applied to effectively modify cassava starch.

    • >Water treatment technology and environmental protection
    • Preparation and Adsorption for Cu2 and Cd2 Ions of Chitosan/Poly(acrylic acid) Hydrogel

      2016, 33(12).

      Abstract (1568) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The chitosan/poly(acrylic acid) (CS/PAA) hydrogel was synthesized in aqueous solution using glow-discharge electrolysis plasma (GDEP) technique, in which chitosan and acrylic acid were used as materials, N,N'-methylenebisacrylamide (MBA) as a crosslinking agent. The structure of CS/PAA hydrogel was characterized by FT-IR, XRD and SEM. The effects of the solution pH, contacted time and initial metal concentration of Cu2 and Cd2 on the adsorption were investigated systematically. Moveover, the reusability of hydrogel was studied as well. The results showed that the acrylic acid has been successfully grafted into the chitosan backbone. The hydorgel exhibits a three-dimensional network structure with a large number of pores on the surface. The adsorption of hydrogel for Cu2 and Cd2 is agreed well with the pseudo-second-order kinetic model and the Langmuir isotherm model at room temperature. The maximum adsorption capacities of Cu2 and Cd2 obtained by Langmuir model are 161.8 and 327.9 mg/g, respectively. CS/PAA hydrogel displays excellent reusability using EDTA-4Na as eluent.

    • Preparation and Activity of Ag/TiO2/AC Photo-catalyst with Double Function

      2016, 33(12).

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      Abstract:A series of composite photo-catalysts were synthesized by sol-gel and impregnation process using silver nitrate, titanium tetrachloride and activated carbon as raw materials. The physical and chemical properties of the composite photo-catalyst, such as morphology、phase composition、specific surface area and optical absorption properties, were characterized by using TEM、XRD、BET and UV-Vis techniques. Taking methyl orange degradation as a model reaction, the photo-catalytic activity of the photo-catalysts were investigated. The results indicate: Ag/TiO2/AC>Ag/TiO2>TiO2. Among them the Ag/TiO2/AC with adsorption, photo-catalytic double-effect function have the highest photo-catalytic activity and its absorption of light extended to visible light region because of its larger specific surface area and modification by loading of silver. Its photo-catalytic activity didn’t basically decrease when it was repeatedly used for 5 times.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Properties of a Type of Flocculation and Demulsification Dual-Effect Organic Polymer

      2016, 33(12).

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      Abstract:Sodium benzoate of p-acrylamide (a) was synthesized by amine hydrolysis reaction and neutralization reaction,redox initiator of ammonium persulfate /sodium bisulfite,a binary copolymer (b) was synthesized with sodium benzoate of p-acrylamide and methacryloxyethyl trimethyl ammonium chloride as monomers.Using Yanchang heavy oil simulated heavy oil emulsion to evaluate the performance of homemade tetrapolymers demulsifier.The flocculation and oil removal performances of binary copolymer were also investigated.The results showed that under the condition of demulsification temperature 70℃,demulsification dosage 110 mg /L ,demulsification time 2 h,the dehydration was reached up 92.04%,the supernatant transparency was up to 98.6% and the flocculation time was 9 s,at room temperature and copolymer dosage of 12 mg/L and the oil removal rate of copolymer was 94.5%,under the conditions of 30 mg/L copolymer dosage,50℃ and 7 h. The flocculation-demulsification performance of self made polymer was superior to BQ-05、SP-169 and PAM、PDMC.

    • Synthesis and Properties of Polyacrylamide Drag Reducer for Fracturing Fluid

      2016, 33(12).

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      Abstract:For reducing fracturing pressure and increasing pump output volume,A of water-soluble drag reducing agent emulsion was synthesized by using acrylamide,octadecyl acrylate and 2-hydroxy-3-(2-propenyloxy)-1-propanesulfonicacimonosodiumsalt as raw materials by inverse emulsion polymerization. The chemical structure and surface morphology of polymer were characterized by means of FTIR and SEM. In addition, the ability of solubility, drag reducing rate, shear resistance, viscoelasticity and cooperation were investigated. Results showed that the solid content of emulsion was 29.6%, the viscosity average molecular weight was 8.5×105g/mol, the viscosity of emlusion was 1800mPa.s. the dissolusion time of polymer was 48s at shear rate of 6.8m/s. the drag reducing rate of polymer exceeds 70% at 10m/s and 300s. the concentration of 1g/L drag reduction agent in aqueous exceed 78% at shear rate of 10m/s. The drag reduction test showed that the drag reduction rate of polymer increased at first and stable latter with the increment of the polymer. Viscoelasticity result shown that the polymer was viscoelastic structure fluid, the value of storage modulus (G') is larger than loss modulus (G'') at 1Hz and 5%. The drag reduction rate of polymer exceeds 53% at 10m/s, 1g/L, 80℃ and 2000mg/L, the additive and clay stabilizer have no effect to drag reducing rate of polymer.

    • Effects of retarder on the evolution process of water in the cement paste

      2016, 33(12).

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      Abstract:Low-field NMR was used to study the effects of retarder HN-1 on the transverse relaxation time (T_2) and the states evolution of water in the cement paste. Analyses the results can be seen that the retarder HN-1 reduces the early hydration rate and extend the induction period of cement hydrated. The changes in the pore structure of hydrating cement paste are accompanied by changes of the states of water in cement paste such. Low-field NMR techniques can be used to observe these changes in the case without destroying the structure of the samples. It can be found from the changes of the relaxation time of water in the hardened paste that the relaxation time of volatile water in hardened paste tends to be shorter while curing time increases, and the migrated rate slows down with the increase of water-cement ratio and the amount of retarder, Capillary water gradually transforms into gel water and physically bound water. The decrease of the average relaxation time of main peak indicates the refining of pore structure in hardened paste. ?The study of X diffraction showed the addition of retarder only changed the process of hydration, but had no effect on the final hydration degree of cement paste.

    • Effects of the Protective Additives on Thermostability of NAD Kinase Recombinanted in E. coli

      2016, 33(12).

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      Abstract:The effects of several sugars (glucose, maltose and sucrose), polyols (glycerol, ethanol and sorbitol) and surfactants (tween 20 and span 20) on thermostability of nicotinamide adenine dinucleotide (NAD) kinase were studied. In addition, a composite protective additive was obtained by the orthogonal experiment and its effects on the thermostability, optimum reaction temperature, optimum pH and storage stability of NAD kinase were also investigated. The results showed that maltose, glycerol, ethanol, and tween 20 could improve the thermostability of NAD kinase significantly. The obtained composite protective additive included mass fraction of maltose 0.6%, volume fraction of glycerol 8%, volume fraction of ethanol 8%, and volume fraction of tween 20 0.6%. After treatment of the composite protective additive, at 55℃, the half-life of NAD kinase was increased by 16.7 times, and it increased from 1.1 h to 18.4 h. Meanwhile, the optimum reaction temperature increased from 35℃ to 50℃, the range of pH stability expanded from 6.5~9 to 5.5~9.5. The retention of enzyme activity was an improvement of 31% at 4℃ storage for 28 d.

    • Determination of Intrinsic Viscosity of Hydrophobic Association Polymer by the Usage of Cyclodextrin

      2016, 33(12).

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      Abstract:Due to the change of the intra- and intermolecular hydrophobic association with the concentration of hydrophobic association polymer solution, the result of intrinsic viscosity for the hydrophobic association polymer tested according to the method in the national standard (GB12005.1-89), could not accurately reflect the single chain character. In this study, based on the inclusion of cyclodextrin and hydrophobes, the intrinsic viscosities of hydrophobic association polymer solution with various molar ratios of cyclodextrin and hydrophobes (CD: [H]) were measured by capillary method and calculated by one point and extrapolation method respectively. The results obtained by the two methods are consistent with each other. With the increase of CD: [H], the intrinsic viscosity of the hydrophobic associating polymer increased and then stabilized, and the Flory-Huggins interaction parameter decreased and then tended to plateau. The results of comparison experiment show that the intrinsic viscosities of the hydrophobic associating polymer change by the inclusion of cyclodextrin with hydrophobes, and the excess cyclodextrin has little effect on the conformation of polymer backbone. Key words:intrinsic viscosity; hydrophobic association polymer; cyclodextrin; polyelectrolyte effect

    • >Adhesives
    • Synthesis and characterization of UV-curing non-solvent acrylic pressure-sensitive adhesive

      2016, 33(12):0-0.

      Abstract (2080) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: UV curing non-solvent acrylic pressure-sensitive adhesives (PSA) were synthesized through bulk polymerization with 2-Ethylhexyl acrylate (2-EHA),Butyl Acrylate (BA),Methyl methacrylate (MMA) and Tetrahydrofurfuryl acrylate (THFA) used as acrylic monomers,acrylic acid (AA) and N,N-dimethylacrylamide (DMAA) used as functional monomers,4-acryloyloxy benzophenone (ABP) used as copolymerizable photoinitiators,2,2′-Azobisisobutyronitrile (AIBN) used as radical initiators and 1-dodecanethiol (NDM) used as chain transfer agent. The influences of functional monomers AA and DMAA, copolymerizable photoinitiators ABP and chain transfer NDM agent were discussed on performances of UV curing non-solvent acrylic pressure-sensitive adhesive (PSA). The other relative performances were then characterized. The results showed that when ω(DMAA)=10% and ω(AA)=2%,120℃ melt viscosity and the adhesive property of PSA were optimal; Copolymerizable photoinitiator ABP is suitable for the system of non-solvent acrylic PSA and PSA had the good UV-curing when mass fraction of ABP was 0.2%. The integrated properties of PSA are the best when mass fraction of NDM was 1.5%.

    • >Catalysis,separation and purification technology
    • Supercritical Fluid Extraction Maleic Hydrazide of Pesticide Residues in Tobacco

      2016, 33(12).

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      Abstract:The research adopts the supercritical carbon dioxide extraction as a tobacco leaf middle peasants maleic hydrazide residue before processing, high performance liquid chromatography (HPLC) as the analysis of detection means.Through single factor and orthogonal experiment, the effects of different entrainers, extraction pressure, extraction temperature, extraction time and carbon dioxide flow were determined as: the entrainer was methanol and isopropanol with methanol: isopropanol = 1: 1 (V: V), the extraction pressure was 20MPa, temperature was 55 ℃, time was 100min, the carbon dioxide flow was 23g/min. High performance liquid chromatography (HPLC) testing conditions, analysis of the adjustment better reproducibility and stability The results showed that the recovery of this method was 94.08%~97.86%, RSD were less than 6%, maleic爃ydrazide燿etection爈imit爓as 2.7μg/g.

    • Catalytic Hydrogenation for Cyclohexyl Multifluorobenzene Preparation by Mo Modified Raney Ni Catalysts

      2016, 33(12).

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      Abstract:A series Raney Ni catalysts were prepared and characterized by inductive coupling plasma emission spectrum, N2 adsorption-desorption, X-ray powder diffraction (XRD), H2-temperature programmed desorption (H2-TPD) and scanning electron microscopy (SEM) to investigate their physical and chemical properties. The catalyst were applied to catalyze 4-(trans-4-propyl) cyclohexyl-1-cyclohexene-4-methyl-2,3-difluorophenyl (TF) hydrogenation to trans-4-(trans-4-propyl) cyclohexyl-1-cyclohexyl-4-methyl-2,3-difluorophenyl (trans-TFT). The results showed RQ Ni-Mo catalyst prepared from Mo-modified rapidly quenched Ni-Al alloy had a higher specific surface area, larger pore volume, pore size and smaller crystal particle size. Under the optimized reaction conditions of the solvent toluene 5ml, the RQ Ni-Mo catalyst 0.05g, TF 0.20g, reaction temperature 40℃, reaction pressure 1.5MPa and reaction time 2h, the conversion of TF and the selectivity to trans-TFT could reach 100% and 69.72%, respectively.

    • Synthesis of Bimetallic Catalyst Mo-Ti-SBA-15 and Its Catalysis of Epoxidation Cyclohexene

      2016, 33(12).

      Abstract (926) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A series of catalysts, including monometallic catalyst Ti-SBA-15-36, Mo-SBA-15-(180/28) and bimetallic catalyst Mo-Ti-SBA-15-(X), were synthesized by the one-step method. The influence of Mo content in the bimetallic Mo-Ti-SBA-15-(X) on catalyst structure and catalytic property was investigated. The reasons for the differences’ catalytic activity in the epoxidation cyclohexene and their synergy mechanism were analyzed. The reaction conditions in the epoxidation cyclohexene reaction were studied. The results showed that the optimum bimetallic catalyst Mo-Ti-SBA-15-(180/28) more catalytic activities than the monometallic catalyst Ti-SBA-15-36, Mo-SBA-15-(180/28). When the reaction condition (catalyst amount: 25mg, cyclohexene: 2.5mmol, TBHP: 5mmol, 1,2-DCE: 10mL, reaction temperature: 80oC, reaction time: 8h) was used, the conversion of Ti-SBA-15-36, Mo-SBA-15-(180/28) and Mo-Ti-SBA-15-(180/28) was 41.07%, 46.44%, 98.33%, respectively, and the selectivity was 97.56%, 93.19%, 98.86%, correspondingly. And the catalyst Mo-Ti-SBA-15-(180/28) has a good reusability.

    • Ceriummolybdovanadophosphoric Heteropoly Acid Salt Catalytic Oxidation of Cyclohexane with Hydrogen Peroxide

      2016, 33(12).

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      Abstract:Keggin-type rare earth ceriummolybdovanadophosphoric of four yuan heteropoly acid salt (CeHPMo11VO40?nH2O)has been synthesized and characterized by FT-IR, X-ray diffraction. CeHPMo11VO40?nH2O showed highest catalytic activity in the yield of cyclohexanol and cyclohexane when cyclohexane as raw materials, H2O2 as oxidant, the optimum reaction conditions are investigated that (amount of catalyst, reaction temperature, reaction time, H2O2 dosage) 0.1mol cyclohexane as a reference, the amount of CeHPMo11VO40?nH2O is 0.2mmol , added 30% hydrogen peroxide 0.2mol ,the reaction temperature is 75 ℃, though reacting 9h, the conversion of cyclohexane was 41.29%, the total yield of cyclohexanol and cyclohexane up to 27.49%.

    • >Drug and cosmetic materials
    • Study on Whitening Efficacyt of Bamboo Leaf Flavonoids Nanoparticles Based on B16 Melanoma Cell Evaluation System

      2016, 33(12).

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      Abstract:The bamboo leaf flavonoids nanoparticles(BLFN) were prepared by ionic cross-linking method, using turnip polysaccharide as a carrier, ε-polylysine as a crosslinking agent. The particle diameter is about 400 nm, particle size distribution is concentrated and of good dispersibility. After B16 melanoma cells were treated with BLFN, the cell proliferation rate, tyrosinase activity and melanin content were measured respectively, and the effects of BLFN on B16 cells were compared with that of arbutin. Results showed that the tyrosinase activity, the synthesis of melanin and proliferation rate of B16 cells were all negatively related to the drugs concentration. When the concentration is 100 μg/mL, the inhibition rate reached at 69.68%, 62.35% and 59.14% respectively, showing significant difference as compared to arbutin (p <0.05). In conclusion, BLFN is a potential substitute for arbutin which has been proved to be an effective inhibitor for melanin synthesis. Meanwhile, the nanoparticle is a combination of various natural products with lower toxicity, which ensuring broad prospects in its application as whitening products.

    • >Food and feedstuff chemicals
    • Preparation and characterization of Pickering emulsions modified by anionic polysaccharides

      2016, 33(12).

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      Abstract:In order to improve the stability of Pickering emulsions stabilized by starch nanocrystal (SNC) and quaternary chitosan (QCS) in response to the change of pH, anionic polysaccharides, sodium alginate and pectin, were used to modify the emulsion droplet surfaces by electrostatic interaction. The stability and digestion properties of these Pickering emulsions were characterized by droplet size, zeta potential and in vitro digestion profiles. The results showed that when the concentration of sodium alginate and pectin in water phase was constant at 0.1% by weight, the droplet sizes of Pickering emulsions after modification were almost unchanged at pH 2~7, and the creaming would be not occurred after a period of 90 days storage at 25°C with a constant of droplet size. Besides, the addition of anionic polysaccharides could inhibit the digestion of lipids and SNCs during in vitro digestion.