• Volume 36,Issue 4,2019 Table of Contents
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    • >Functional materials
    • polyurethane with high lithium salt concentration as solid electrolyte for solid-sate lithium batteries

      2019, 36(4).

      Abstract (1211) HTML (0) PDF 608.94 K (0) Comment (0) Favorites

      Abstract:Polycarbonate polyurethane (PCPU) with 30% hard segment was synthesized from isophoronediisocyanate, polycarbonate diol and diethylene glycol. Solid polymer electrolytes (SPE) with various concentration of lithium salts were prepared by the complexing of polyurethane and Lithium bistrifluoromethane sulfonyl imide(LiTFSI). The structure of polyurethane was analyzed by infrared spectroscopy. The thermal properties of polyurethane and electrolyte were tested by TG and DSC. The effects of different LiTFSI contents on the electrochemical properties of electrolyte were investigated by AC impedance and linear sweep voltammetry.The results indicated that the ionic conductivity of PU-based solid polymer electrolytes at room temperature increase with the increase of LiTFSI content then decrease and then increase. The ionic conductivity of the solid polymer electrolytes with 70% lithium salt concentration reached the maximum value among the as-prepared electrolytes, the all-solid-state battery using the PU-based electrolytes and LiFePO4 delivered the discharge capacity of 153 mA·h/g at 0.2C at 60°C, and the capacity retention reached 84% after 100 cycles.

    • Synthesis and Characterization of GA-g-P AA / ST Composite Hydro-gels

      2019, 36(4).

      Abstract (817) HTML (0) PDF 803.22 K (0) Comment (0) Favorites

      Abstract:GA-g-PAA/ST composite hydrogels were prepared by graft copolymerization of gum arabic (GA),acrylic acid (AA),sepiolite clay (ST) under microwave irradiation.The structure and morphology of GA-g-PAA/ST composite hydrogels were characterized by FTIR XRD and SEM.The thermal stability of the hydrogel was analyzed by TG.The swelling behavior and water retention of the hydrogel in different cationic salt solutions were also discussed.The results showed that the graft copolymerization reaction took place between the two groups,and the copolymer intercalated into the interlayer of ST to form a delaminated three-dimensional network composite hydrogel.When the concentration of salt is 20mmol/L,the absorbency of the hydrogel in NaCl、BaCl2、AlCl3 solution is 112、38 and 29g/g,respectively.When the concentration of surfactant solution was 20mmol/L,the absorbency of the hydrogel in SDS solution and CTAB solution was 135 and 105g/g,repectively.After three cycles of NaCl and BaCl2 salt solution,the water absorption ratio of the hydrogel is 80 and 12g/g,indicating that the hydrogel has strong salt responsive property and good reversible behavior in NaCl and BaCl2 salt solution.The hydrogel has good thermal stability and water retetion.

    • >Review and monographs
    • Preparation and Formation Mechanism of Graphene Oxide

      2019, 36(4).

      Abstract (1375) HTML (0) PDF 619.05 K (0) Comment (0) Favorites

      Abstract:As a kind of graphene derivative, graphene oxide (GO) contains a large number of oxygen-containing groups such as hydroxyl, epoxy, carboxyl and carbonyl. This makes it easy to interact with other substances to enhance and broaden the performance and application of traditional materials. The structure and size of GO are also affected by many factors such as preparation methods, graphite source, oxidant type and reaction conditions in the oxidation process of graphite. The research on the preparation, formation mechanism and structure control of GO has gradually attracted the attention of researchers. In this paper, the research progress on the preparation of GO, the improvement of the method, the chemical reaction and formation mechanism involved in the preparation process, and the influence of GO structure on its properties and applications are reviewed. From the perspective of industrial production and sustainable development, the problems and research directions of broadening and realizing the application of GO are summarized and forecasted.

    • >Water treatment technology and environmental protection
    • Preparation of ZnS/AC composites and its adsorption performance of uranyl ions in aqueous solution

      2019, 36(4).

      Abstract (610) HTML (0) PDF 1.18 M (0) Comment (0) Favorites

      Abstract:The composite ZnS/Ac of nano-zinc sulfide supported on activated carbon was prepared by chemical precipitation method. The composites were characterized by SEM, EDS, XRD, FTIR and BET. The adsorption performance of ZnS/Ac on uranyl ions in aqueous solution was studied. The effects of adsorption time, initial uranyl ion concentration, pH value, adsorbent dosage and temperature on adsorption performance were discussed. Thermodynamic and kinetic simulations explored the adsorption mechanism. The results show that the specific surface area of ZnS/Ac is 201.1961 m2/g, which is significantly higher than that of activated carbon (165.0240 m2/g). The average pore diameter is 4.70 nm and the pore volume is 0.038 cm3/g. At an initial mass concentration of 35 mg/L, pH=6, adsorption time of 120 min, dosage of 10 mg, and treatment temperature of 50 ?C, the adsorption capacity of the adsorbent for uranyl ion is 64.4736 mg/g. The adsorption process conforms to the pseudo second order kinetic equation and the Langmuir adsorption isotherm model. The thermodynamic parameters<0、>0、>0, indicate that the adsorption is a spontaneous endothermic process.

    • >Drug and cosmetic materials
    • Synthesis of N-(3-Chloro-4-fluorophenyl)-7-fluoro-6-nitroquinazolin-4-amine under Microwave Irradiation

      2019, 36(4).

      Abstract (615) HTML (0) PDF 450.96 K (0) Comment (0) Favorites

      Abstract:N-(3-Chloro-4-fluorophenyl)-7-fluoro-6-nitroquinazolin-4-amine, the key intermediate of the anticancer drug Afatinib and Dacomitinib, was synthesized via the addition of 2-bromo-4-fluoro-5-nitrobenzonitrile with 3-chloro-4-fluoroaniline, following cascade amination and condensation-cyclization with formamide catalyzed by cuprous iodide under microwave irradiation. The optimal reaction conditions were investigated. The reaction results showed that 2-bromo-N-(3-chloro-4-fluorophenyl)-4-fluoro-5-nitrobenzimidamide in 93.8% yield was synthesized when 20% cuprous iodide (mole fraction) was used as catalyst, molar ratio of 3-methoxyaniline and 3,3-dimethoxypropionate was 1:1, refluxed for 20 min under microwave irradiation. Subsequently, the target product, N-(3-chloro-4-fluorophenyl)-7-fluoro-6-nitroquinazolin-4-amine was obtained with a yield of 84.5% in the presence of 10% cuprous iodide/4-hydroxyl-L-proline (mole fraction), and with n(2-bromo-N-(3-chloro-4-fluorophenyl)-4-fluoro-5-nitrobenzimidamide):n(formamide) of 1:2 at 80℃ for 10 min under microwave irradiation.

    • >Fine chemical intermediates
    • synthesis of tris(3-hydroxypropyl)phosphate

      2019, 36(4).

      Abstract (996) HTML (0) PDF 584.84 K (0) Comment (0) Favorites

      Abstract:In this paper, phosphoric acid and propylene oxide were used as raw materials, and a reactive flame retardant tris(2-hydroxypropyl) phosphate was synthesized by using a Lewis acid ionic liquid as a catalyst in a green solvent. The structure was characterized by infrared, nuclear magnetic and mass spectrometry. The effects of the type and amount of catalyst, material ratio, reaction time and reaction temperature on the reaction were studied. The results show that the optimum conditions are n (phosphoric acid): n (propylene oxide) = 1:3.2, the reaction temperature is 90 ? C, the reaction time is 3 h, the amount of the catalyst is 3%, and the yield of the obtained product can reach 92.8%. The product performance index is excellent, and the thermogravimetric analysis shows that its stability meets the material processing requirements.

    • >Electro-organic chemistry and industry
    • Self-assembly and Photoelectric Properties of Triaryla-mine-1,3,5-benzenetricarboxamide Derivative

      2019, 36(4).

      Abstract (782) HTML (0) PDF 1.21 M (1) Comment (0) Favorites

      Abstract:To achieve excellent conductivity and hole transport capability of organic photoelectric functional materials, ordered long range arrangement of triarylamine functional units is achieved by using a su-pramolecular assembly method. A new compound N1,N3,N5-tris(3-((4-(bis(4-(dodecyloxy)phenyl)amino)phenyl)amino)propyl)benzene-1,3,5-trimethamide (H1) was thus synthesized. UV-Vis absorption and fluorescence spectra showed that H1 had self-assembly characteristics in the weak polar solvent n-heptane. The self-assembly morphology of H1 was observed by optical microscope and Scanning Electron Microscope (SEM), respectively. Further, quantum chemical calculations and electrochemical measurements were performed. The calculated results and measured HOMO level (-5.14 eV) and LUMO level (-1.80 eV) were matched with the energy levels of perovskite. The thermal decomposition temperature of H1 was found to be 445 °C. Thus, H1 could be potentially applied as a hole transport material in the perovskite solar cell.

    • >Food and feedstuff chemicals
    • Clathration of Squalene with Different Cyclodextrins

      2019, 36(4).

      Abstract (587) HTML (0) PDF 552.12 K (0) Comment (0) Favorites

      Abstract:Squalene is a linear triterpenoid with six non-conjugated double bonds. Its physiological function is remarkable, but its application is limited due to its poor water solubility and stability. The clathration of squalene with alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-beta-cyclodextrin and methyl-beta-cyclodextrin were studied by phase solubility method at temperatures of 25℃, 40℃ and 55℃. While the phase dissolution diagrams were plotted and the thermodynamic parameters during the inclusion process were calculated. The results showed that all the phase dissolving diagrams were AL type, and the inclusion effect and solubilization effect of gamma-cyclodextrin were the most significant. The inclusion constant K of gamma-cyclodextrin for squalene was up to 1778.0860 L/mol, and the solubility of squalene was increased to 309.0935 times. The thermodynamic parameters enthalpy change (ΔH) and entropy change (ΔS) of the inclusion process are both positive values, while the Gibbs free energy (ΔG) are both negative values, indicated that the inclusion process is an endothermic spontaneous reaction, and the increase of disorder (entropy increase) is the main driving force for the encapsulation of squalene molecules in cyclodextrin cavities.

    • >Catalysis,separation and purification technology
    • Synthesis of Rubber Antioxidant 7PPD by Pt-S/C Catalyst

      2019, 36(4).

      Abstract (675) HTML (0) PDF 3.80 M (0) Comment (0) Favorites

      Abstract:The nano-zinc oxide was used as the template and the phenolic resin was used as the carbon source. The mesoporous carbon was prepared by a hard template method and used as support for the preparation of Pt-based catalysts. BET, SEM, ICP, TEM were used to characterize the mesoporous carbon and its supported Pt catalysts. The results show that surface area and pore structure of mesoporous carbon can be effectively controlled by varying the size of the nano-zinc oxide particles. The Pt/MC catalytic performance for the antioxidant 7PPD synthesis reaction was studied. Compared with the conventional Pt/AC catalyst, the conversion of p-ADPA reached to 100% from 97.5% and the selectivity of 7PPD reached 99.5% from 94.5% and the stability of the catalysts were significantly improved. The catalysts used ten times were characterized by CO chemisorption, ICP, BET, etc. The results show that the pore structure of the support is an important factor affecting the stability of the catalyst. When the average pore diameter is small, molecules with large molecular sizes such as 7PPD was easy to block the pores. When the average pore diameter is largest, the pore walls are thinner, the catalyst was worn easily during use, and the active components were lost easily.

    • >Food and feedstuff chemicals
    • Structure and Inhibitory Activity against α-glucosidase of Polygonatum kingjanttm Polysaccharides

      2019, 36(4).

      Abstract (713) HTML (0) PDF 823.40 K (0) Comment (0) Favorites

      Abstract:Chemical structure of Polygonatum kingjanttm polysaccharides was determined Fourier-transform infrared spectroscopy (FTIR) and circular dichroism (CD). Micromorphology of polysaccharides was observed by scanning electron microscopy (SEM). Thermal stability of polysaccharides was evaluated by thermogravimetric analysis (TGA). And effects of Polygonatum kingjanttm polysaccharides on α-glucosidase and α-amylase were investigated. The results suggested that there were pyranosidic linkages in Polygonatum kingjanttm polysaccharides. And Polygonatum kingjanttm polysaccharides might be acidic polysaccharides containing uronic acids. Polysaccharides exhibited positive cotton effect at wavelength of 210 nm. Micromorphology of polysaccharides included porous sheet-like structure and multichain aggregation structure. The loss rate of polysaccharides was high at 248~350 ℃, followed by 30~200 ℃ and 400~700 ℃. Polygonatum kingjanttm polysaccharides did not effectively inhibit α-amylase, but drastically inhibit α-glucosidase with IC50 (concentration that inhibited enzyme activity by 50%) of 4.572 g/L.

    • >Biological engineering
    • Antibacterial Activity and Mechanism of Sunflower Stalk Pith Extracts

      2019, 36(4).

      Abstract (708) HTML (0) PDF 1.59 M (0) Comment (0) Favorites

      Abstract:Three different polarity extracts were prepared from sunflower stalk pith. The agar diffusion assay was used to investigate the antibacterial activities of the extracts, and the action mechanism of the ethyl acetate extract (EE) against Staphylococcus aureus and Escherichia coli was detected in this study. Results showed that all extracts have good bacteriostatic effects on the four tested bacteria. Both MIC values of Staphylococcus aureus group and Escherichia coli group which treated by EE were 0.78 g/L, and the IC50 valueswere1.11±0.01 and 1.59±0.03g/L, respectively. There was positive correlation between the antibacterial activities and the content of total phenols and total flavonoids (P<0.05).The damaged membrane structures induced by EE were observed by SEM. EE also increased the permeability of the cell wall and cell membrane of the tested bacterial strains with the release of the electrolytes, proteins and alkline phosphatase (AKP) in the cell. Finally, EE also could inhibit the replication of bacterial genetic material (DNA) and ultimately inhibited bacterial reproduction by 4',6-diamidino-2-phenylindole (DAPI) method.

    • >Functional materials
    • Preparation of Polydiacetylene/α-FeOOH Nanocomposites and Its Reversible Thermochromic Properties

      2019, 36(4).

      Abstract (1123) HTML (0) PDF 2.98 M (0) Comment (0) Favorites

      Abstract:10,12-Pentacosadiynoic acid(DA)-assembled on the surface of α-FeOOH was irradiated with ultraviolet light (=254 nm) to obtain polydiacetylene/α-FeOOH(PDA/α-FeOOH) nanocomposites. The structure and morphology of nanocomposites were analyzed by XRD, SEM and DLS. Thermochromism experiment showed that PDA/α-FeOOH had a reversible change from blue to red between 30℃ and 80℃. The effects of irradiation time and amount of α-FeOOH on reversible thermochromic of PDA/α-FeOOH nanocomposites were investigated. The results revealed that bule PDA/α-FeOOH nanocomposites(m(DA):m(α-FeOOH)=3:1) with UV light irradiated for 10 min was the fastest color change. When the composites were warmed at 60℃, its color changed red and the maximum absorption wavelength happened shift-blue from 650 nm to 540 nm. The heating and cooling cycles indicated that PDA/α-FeOOH composites had higher thermal stability.

    • Preparation of Magnetically Driven Superhydrophobic Sponge for Oil/Water Mixtures Separation

      2019, 36(4).

      Abstract (861) HTML (0) PDF 2.85 M (0) Comment (0) Favorites

      Abstract:The application of superhydrophobic materials in the separation of oil/water mixtures has been widely concerned, because of its unique interface properties. The research was prepared magnetic driving superhydrophobic sponge, which adopts the dipping method with Fe3O4 nanoparticles and stearic acid to modify the surface of polyurethane sponge. The magnetic driving superhydrophobic sponge was characterized by XRD, FTIR, TG, etc. The water contact angle up to 158˚ and the thermal stability of sponge is significantly improved; its elastic performance is not damaged. Moreover, the water contact angle is still higher than 148 ˚of the as-prepared sponge under severe conditions such as high temperature (50~90℃ hot water and air) and strong corrosion (pH=2~13), etc. The as-prepared sponge exhibited excellent separation capacities for oil/water mixtures, and it can be driven and recycled oil simply by magnets.

    • Preparation of 2-Hydroxy-3-allyloxypropyl Hydroxyethyl Cellulose and Temperature-sensitive Properties

      2019, 36(4).

      Abstract (731) HTML (0) PDF 2.04 M (0) Comment (0) Favorites

      Abstract:Hydroxyethyl cellulose is used as the hydrophilic polymer backbone, the hydrophobic agent allyl glycidyl ether (AGE) is grafted onto the hydroxyethyl cellulose backbone by etherification reaction, the suitable hydrophilic and lipophilic balance of hydroxyethyl cellulose are adjusted by adjusting the substitution of the hydrophobic allyl group, 2-hydroxy-3-allyloxypropyl hydroxyethyl cellulose (HAPEC) with temperature sensitivity was prepared. The transmittance change of the HAPEC aqueous solution with different temperature is studied by a temperature-controlled UV spectrophotometer and the lowest critical solution temperature (LCST) of HAPEC is determined. The study shows that LCST decreases linearly with the increase of molar substitution (MS) of hydrophobic allyl groups. When the MS of HAPEC increases from 1.30 to 2.71, the LCST decreases from 64.3℃ to 28.5℃. The results of this study indicate that the LCST of HAPEC can be adjusted by changing the MS of hydrophobic groups. The self-assembly behavior of amphiphilic HAPEC in aqueous solution is investigated by fluorescence spectroscopy and dynamic light scattering (DLS) , the critical micelle concentration (CMC) is determined. The result shows that HAPEC can be self-assembled to be micelle in solution, and CMC decreases with the increase of MS. When the MS of HAPEC increases from 1.11 to 2.71, the CMC decreases from 0.145 mg/mL to 0.021 mg/mL. The biodegradation of HAPEC is studied according to ASTMD 5988-03, and scanning electron microscope (SEM) is used to compare the morphology of HAPEC samples before and after degradation. The result shows that HAPEC has good biodegradability. After 90 days of degradation, the shape of HAPEC samples changes significantly, and the biodegradation rate is as high as 36.5%.

    • >Acrylic series chemicals
    • Synthesis and application of self-crosslinkable polyacrylate emulsion for water-based ink

      2019, 36(4).

      Abstract (904) HTML (0) PDF 814.82 K (0) Comment (0) Favorites

      Abstract:The waterborne polyacrylate emulsions with soft core-hard shell structure were synthesized by semi-continuous emulsion polymerization technology using methyl methacrylate (MMA), 2-ethylhexyl acrylate (2-EHA), methylacrylic acid (MAA), diacetone acrylamide (DAAM) as monomers, and adipic dihydrazide (ADH) as crosslinker. ATR-FTIR, TEM, GPC, TG and DMA were utilized to characterize the bulk structures and properties of waterborne polyacrylate. The results show that crosslinking reaction between -CO-groups of DAAM and -NHNH2 groups of ADH can occur during emulsion film formation. The water resistance of emulsion film and the adhesion ratio of emulsion on biaxially oriented polypropylene (BOPP) film were improved due to the increased crosslinking density. Compared with the without crosslinked film, the crosslinked film improves thermal stability and glass transition temperature of the emulsion film. As DAAM content increased from 0% to 2%, water absorption ratio of emulsion film decreased from 24.2% to 7.6%, adhesion ratio on BOPP film increased from 87% to 100%. While the m(ADH)/m(DAAM) ratio increased from 0:1 to 0.7:1, water absorption ratio of emulsion film decreased from 28.1% to 7.6%, adhesion ratio on BOPP film increased from 0% to 100%. The optimal DAAM content and m(ADH)/m(DAAM) ratio was 2% and 0.7:1. The emulsion has good potential application in water-based ink for BOPP film.

    • >Functional materials
    • Preparation of White Carbon Black from Fly Ash Modified with Silane Coupling Agents and Its Dispersion Properties

      2019, 36(4).

      Abstract (283) HTML (0) PDF 1.92 M (0) Comment (0) Favorites

      Abstract:Abstract:Three silane coupling agents, 3-(aminopropyl)triethoxysilane (APTES), 3-(mercaptopropyl)- triethoxysilane (MPTES) and 3-glycidoxypropytriethoxysilane (GPTES) were used to modify the white carbon black derived from fly ash. The effects of amino, thiol and epoxy silane coupling agents on the dispersion of modified white carbon black were studied by FTIR, TGA, zeta potentiometer and SEM. The results showed that three different silane coupling agents were grafted successfully onto the surface of white carbon black. The dispersity of modified white carbon black was improved obviously, which was related not only to the particle size of modified white carbon black but also to the loading amounts of silane coupling agents. Among them, the modification effect of MPTES was the best. Under the conditions of pH=10 and n(MPTES):n(SiO2)=1.0:1.0, the obtained product had the best dispersity in alcohol, the size was 557 nm and the absolute value of zeta potential was 36.43 mV.

    • >Review and monographs
    • The Application of Microreaction Technology in Fluorination

      2019, 36(4).

      Abstract (686) HTML (0) PDF 1.04 M (0) Comment (0) Favorites

      Abstract:The organic fluorochemical has an extensive application in the field of fine chemicals due to the unique physical properties. However, there are some problems existed in the traditional fluorination process. There is no doubt that, as a new technology of high efficiency mass and heat transfer, microreaction technology is expected to solve some of the problems. Therefore, according to the types of fluorinated substrate, the main progress made in the field of microreaction technology in recent twenty years, and the application of microreaction technology in fluorination is reviewed. The application of microreaction technology can greatly improve the of efficiency fluorination and it is believed that the emergence of microreaction technology will promote the development of fluorination reaction towards a more efficient, safe, environmentally friendly, controllable and continuous direction. Neverthless, it is necessary to break through the traditional thinking mode and further study on the application of microreaction technology in continuous post-processing.

    • >Functional materials
    • Synthesis and Photodynamic Study of Glutathione Modified Fullerenene

      2019, 36(4).

      Abstract (1004) HTML (0) PDF 1.38 M (2) Comment (0) Favorites

      Abstract:It is important to design and synthesize safe and effective photosensitizers in photodynamic therapy for tumors. In this paper, a water-soluble fullerene photosensitizer (C60-OH-GSH) was synthesized by bonding reduced glutathione to fullerene C60 via nucleophilic addition reaction, and its chemical composition and structure were confirmed. C60-OH-GSH aggregates to nanoparticles of uniform size in aqueous solution, and it gives high stability in multiple physiological solutions, indicating its excellent biocompatibility. Under irradiation, C60-OH-GSH at low concentration of 1 ?mol/L can generate sufficient reactive oxygen species to induce cellular damage and apoptosis of various tumor cells, while in the dark it exhibit non negative effect on normal cells even at concentrations up to 50 ?mol/L, which makes it a promising photosensitizer for phototherapeutic application.

    • Synthesis and properties of epoxy modified water-alkyd resin

      2019, 36(4).

      Abstract (967) HTML (0) PDF 778.54 K (0) Comment (0) Favorites

      Abstract:The epoxy esters was prepared by linoleic acid and epoxy resin E-51 after ring-opening reaction, then using it to replace part of the polyols involved in the reaction. After neutralization with amine, an epoxy modified water-alkyd resin was prepared. The structure of the product was investigated characterized by FTIR. We discussed the synthesis process of epoxy esters, and in-depth analysis of the epoxy ester dosage on the performance of the resin and its film. The results showed that the epoxy ester was obtained under the condition as followed: reaction temperature 110 ?C, reaction time 4h, tetrabutylammonium bromide dosage 8‰, acid value 13.3 mgKOH?g-1. When the epoxy ester content was 10%, the overall performance of the resin and the paint film was optimal, and the thermal stability of the waterborne alkyd resin paint film after epoxy modification was significantly improved.

    • >Oil field chemicals and petroleum additives
    • Reverse Demulsifier for Slickwater Flowback Fluid and Its Demulfication Mechanism

      2019, 36(4).

      Abstract (612) HTML (0) PDF 573.52 K (0) Comment (0) Favorites

      Abstract:In this paper, a series of two-block and thri-block polyether reverse demulsifiers were synthesized under 120 ℃ conditions by using trimethyl-hydroxypropyl propane diamine as initiator, potassium hydroxide as catalyst and through open-loop polymerization of ethylene oxide (EO) and propylene oxide (PO) as monomers. The infrared spectra and NMR spectra show that the synthesized products are consistent with the design structure.The demulsification results showed that the reverse demulsifier with tri-block structure and block mass ratio n(EO): n(PO): n(EO)=1:6:12 has a well demulsification performance for slickwater flowback fluid. Its dehydration rate is greater than 97%. The results of dynamic interfacial tension and interfacial dilatation modulus experiments presented that EPO-8 has faster diffusion rate to interface and better performance for decreasing the film strength. That is why it had the best demulsification performance.

    • >Catalysis,separation and purification technology
    • Extraction and GC - ms analysis of volatile oil from arhat pine by microcapsule aqueous two-phase method

      2019, 36(4).

      Abstract (544) HTML (0) PDF 3.39 M (0) Comment (0) Favorites

      Abstract:In this study, the extraction technology of total flavonoids from Podocarpus was studied. the optimum extraction conditions of volatile oil from the leaves and branches of Podocarpus were determined as follows: extraction time 35 mi n, concentration of β -cyclodextrin 40 %, concentration of sodium sulfate 15 %, extraction temperature 30 ℃, under these conditions, the yield of volatile oil from the leaves and branches of Podocarpus was 1. 372 %. A total of 22 compounds were identified by mass spectrometry, accounting for 93.72% of the total chromatographic area. There are 18 terpenes and their oxygen-containing derivatives, accounting for 73.74 % of the total content, including 4 terpineol compounds, 2 terpinealdehyde compounds, 4 aliphatic compounds, accounting for 19.98%, including 2 ester compounds and 2 acid compounds. The main components of the volatile oil were caryophyllene, α-pinene and β-pinene, and the contents were 17.62 %, 9.78 % and 7.47 %, respectively.

    • >Modernization technology of traditional Chinese medicines
    • Purification of total flavonoids from Empetrum nigrum L. var. japonicum with macroreticular resin

      2019, 36(4).

      Abstract (672) HTML (0) PDF 820.29 K (0) Comment (0) Favorites

      Abstract:Abstract: Eight types of macroporous resins were compared via static adsorption-desorption methods with adsorption capacity and desorption capacity as dexes. Result indicated that AB-8 resin performed better adsorption and desorption properties to total flavonoids from Empetrum nigrum L. var. Japonicum. Then, the purification process was study by static and dynamic adsorption-desorption experiments. The optimal conditions were as follow: static adsorption equilibrium time was 1.0 h, desorption solvent was 95% ethanol and desorption equilibrium time was 1.5 h. Adsorption isotherm of five components from Empetrum nigrum L. var. japonicum by AB-8 macroporous adsorption resin according with Freundlich model and Langmuir model at different temperatures(25℃、30℃、35℃). The maximum sample volume was 400 mL, the impurities were washed by 5 BV 20% ethanol, and the components eluted with 95% ethanol, elution volume was 5 BV and elution flow rate was 3 mL/min. Finally, the purity of total flavonoids from Empetrum nigrum L. var. Japonicum increased from 49.16% to 89.59% at the optimal experimental conditions. This experiment provides a reference for further study of Empetrum nigrum L. var. japonicum.

    • >Food and feedstuff chemicals
    • Effects of L-Valine on the natamycin biosynthesis of Streptomyces natalensis HW-2

      2019, 36(4).

      Abstract (804) HTML (0) PDF 827.39 K (1) Comment (0) Favorites

      Abstract:The effect of L-valine (L-Val) on biosynthesis pathway of natamycin by Streptomyces natalensis HW-2 was investigated. The experimental results showed that the maximal yield of natamycin reached 1.83 g/L when the adding amount of L-Val was 0.5 g/L during the fermentation of Streptomyces natalensis HW-2 for 36 h, which was 84.85% higher than that of the control. The addition of L-Val resulted in a decrease of biomass and an increase of pH, and an improvement of glucose utilization. The activities of pyruvate kinase (PK), phosphoenolpyruvate carboxylase (PEPC) and pyruvate carboxylase (PC) in intracellular enhanced, while that of citroyl synthetase (CS) decreased by 26.57%. Comparing with the control, the contents of pyruvic acid, oxaloacetic acid, acetyl-CoA in the broth increased by 80.50%, 53.28% and 47.19%, respectively. And, the contents of acetic acid, propionic acid and α-ketoglutaric acid increased by 16.98%, 10.65% and 15.40%, respectively. But, the content of citric acid decreased by 27.01%.

    • >Catalysis,separation and purification technology
    • Effect of thermal treatment temperature of support on Catalytic Performance of Pt/FeOx Catalysts for HCHO oxidation

      2019, 36(4).

      Abstract (705) HTML (0) PDF 787.45 K (0) Comment (0) Favorites

      Abstract:A few FeOx following a thermal-treatment at different temperatures supported Pt catalysts (Pt/FeOx-T) were prepared by a facile colloid deposition method, and their catalytic properties were investigated in the oxidation of formaldehyde at ambient temperature. These catalysts were characterized by XRD, BET, H2-TPR, FTIR and TEM. The results showed the thermal treatment temperature could affect the BET surface area, oxidation-reduction property of FeOx, the amount of surface hydroxyls of Pt/FeOx and a strong interaction was observed between Pt species and FeOx. The activity test indicated that the optimal catalytic performance was obtained over 1.5wt% Pt/FeOx-100 showed the best catalytic performance, under the conditions of 25?C, the relative humidity of 55%, a gaseous hourly space velocity of 60 000 cm3g-1h-1, and the HCHO conversion was 96.2%.

    • >Functional materials
    • Preparation and Properties of an Isoindigo-Derived Semiconductor and OTFT Application

      2019, 36(4).

      Abstract (652) HTML (0) PDF 933.36 K (0) Comment (0) Favorites

      Abstract:4-Decyl-1-hexadecyl side chin is introduced into (3E,7E)-3,7-bis(2-oxoindolin-3-ylidene)benzo [1,2-b: 4,5-b']difuran-2,6(3H,7H)-dione(IBDF) with the material 4-Decyl-1-hexadecyl bromide and 6-bromoindoline-2,3-dione, and then Stille couple with (E)-1,2-bis(tributylstannyl)ethene to obtain a poly-mer semiconductor PIBDFV-26 with large fused ring based on isoindigo (IID). The property, structure and morphology of PIBDFV-26 are characterized by TGA, DSC, UV, CV, XRD and ATM. The results show that the semiconductor PIBDFV-26 has good solubility in trichloroethylene (TCE) and good thermal stability. The HOMO/LUMO energy level is -5.66 eV/-4.62 eV and the optical gap is 1.34 eV. XRD results show that the polymer chains are likely packed in a lamellar crystalline structure with an edge-on orientation and the d-spacing and π-π stacking distance are 2.55×10-6 mm and 3.46 ×10-7 mm, respectively. AFM shows that the surface of the annealed PIBDFV-26 film contains nano-crystalline particles. The PIBDFV-26 is assembled into an organic thin film transistor (OTFT) device and tested, and the results show that the OTFT device ex-hibits n-type charge transfer characteristic. The average electron mobility of the polymer film annealed at 150oC is 0.13 cm2/V∙s.

    • >Food and feedstuff chemicals
    • Effects of Metal Ions and Food Additives on Antimicrobial Activity of Hexahydro-β-Acid/Methyl-β-Cyclodextrin Inclusion Complexes

      2019, 36(4).

      Abstract (582) HTML (0) PDF 489.81 K (1) Comment (0) Favorites

      Abstract:The minimum inhibitory concentration of HBA/M-β-CD on seven test bacteria was determined by two-fold dilution method. Take Staphylococcus aureus and enterobacter sakazakii as indicator bacteria, the effect of metal ions and food additives on antimicrobial activity was studied. The result showed that the HBA/M-β-CD inclusion complex has broad-spectrum antimicrobial activity against the tested strains, except for S. paratyphi A. And the MICs of HBA/M-β-CD against S. aureus and E. sakazakii were 16.25μg/mL and 32.5μg/mL respectively. The metal ion Ca2 , K , Na , Mg2 , Zn2 have no significant effect on their antibacterial activity of inclusion complex, conversely, Fe2 /3 , Cu2 showed significant effects on the antibacterial activity. Furthermore, for food additives, there were no significant effect on antibacterial activity of NaNO2 and sodium benzoate, and a slight effect for E. sakazakii were observed on increasing the activity of Na2SO3 and decreasing the activity of potassium sorbate in a high concentration. However, antimicrobial activity decreased with the addition of H2O2 and KMnO4 in high concentration.

    • >Review and monographs
    • Research progress of fuel ethanol fermentation and the tolerance of saccharomyces cerevisiae

      2019, 36(4).

      Abstract (872) HTML (0) PDF 1.51 M (0) Comment (0) Favorites

      Abstract:Usually, emphasizing the production capacity and controlling the process cost cause the strain unbalanced growth and production, and bearing the multiple stresses from the fermentation microenvironment. At the same time, most researches of the yeast tolerance are based on the laboratory model strain and composition medium, it is difficult to implement industrial applications. Therefore, this article analyzes the current domestic fuel ethanol production status and production process, the fermentation process of stress factors and molecular mechanisms of S. cerevisiae tolerance and transformation methods and other related content, then we put forward the fermentation industry in the future fermentation of microbial tolerance and possible transformation direction.

    • >Functional materials
    • Microwave Assisted High-energy Ball Milling Synthesis and Application of Nano Vanadium and Chromium Carbides Composite Powders

      2019, 36(4).

      Abstract (786) HTML (0) PDF 1.19 M (0) Comment (0) Favorites

      Abstract:Nano-sized vanadium and chromium carbides composite powders were prepared by mechanical alloying assisted microwave heating method using micron size vanadium oxide, chromium oxide and carbon black nanoparticles as raw materials. The products were characterized by XRD, XPS, TG-DSC, SEM, TEM and BET techniques. The results showed that the optimum synthesis conditions of nano vanadium /chromium carbides composite powders were obtained as follows: mass fraction of carbon black 35%, reaction temperature 900℃, and holding time 1 h. Under these conditions, the reaction products are mainly composed of V3Cr2C5, Cr2VC2 and Cr3C2. The particles are spherical or nearly spherical with good disper-sion and no obvious agglomeration. The average particle size is about 50 nm and the specific surface area is 115.53 m2/g. The addition of nano vanadium and chromium carbides composite powders can enhance the mechanical properties and grinding efficiency of vitrified bond cBN grinding tool, which reduces the wastage of the grinding tool, and has a good friction-reducing effect.

    • >Drug and cosmetic materials
    • Preparation of Terpolymer and Its Application in Hair Gel

      2019, 36(4).

      Abstract (541) HTML (0) PDF 1.24 M (0) Comment (0) Favorites

      Abstract:Abstract: A hair gel-NVV polymer was synthesized from N-vinylpyrrolidone (NVP), vinyl versatate (VeoVa10) and vinyl acetate (VA) under the action of azobisisobutyronitrile (AIBN). NVV was characterized by ATR-FTIR and 1HNMR. The influence of the amount of NVP on the properties of the resin, the curl retention of the NVV polymer used in the hair gel, and the carding performance were analyzed. The results show that when n(NVP): n(VA): n(VeoVa10) was 2:1:1, the styling performance of NVV polymer was improved by 50% compared with polyvinylpyrrolidone (PVP), and the carding performance was improved by 100%. NVV resin is natural and long-lasting, has good affinity with hair, is not easy to be wetted by moisture, and can form a uniform smooth coating on the hair. So it is suitable for hair styling products.

    • >Functional materials
    • Hydrothermal Synthesis of Co@TiO2/PEI/RGO Nanocomposites and Their Photocatalytic Activities

      2019, 36(4).

      Abstract (1017) HTML (0) PDF 1.14 M (1) Comment (0) Favorites

      Abstract:Graphene oxide (GO) was firstly prepared from graphite flake powder according to a modified Hummers method. Subsequently, we developed a one-step hydrothermal method to prepare a three-dimensional (3D) cobalt loading TiO2/RGO architecture nanocomposites by using Ti(SO4)2 and CoCl2 as precursor and Polyetheylenimine (PEI) modified graphene oxide sheets as a support. PEI is used as the connection linker to successfully achieve in situ growth of TiO2 on reduced graphene oxide surfaces among the composites. Their structure and photoelectrical properties were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, UV-Vis absorption spectroscopy, and X-ray diffraction. The photocatalytic activities of the nanocomposites with respect to methylene blue (MB)were also investigated under UV and visible illumination. The results showed that the nanocomposites exhibited high catalytic performancetoward methylene blue with a high degradation efficiency above 99 % in aqueous solution. Meanwhile, the catalyst was recycled over ten times without showing a signi?cant loss in its activity.

    • >Modernization technology of traditional Chinese medicines
    • Synthesis and Application of Isoliquiritigenin Boned Silica Gel Stationary Phases

      2019, 36(4).

      Abstract (582) HTML (0) PDF 4.61 M (0) Comment (0) Favorites

      Abstract:Isoliquiritigenin is an important chalcone component with plane-conjugated structure. The 10 μm silica gel was used as the substrate and the isoliquiritigenin was used as the ligand. The new isoliquiritigenin bonded silica gel stationary phases (ISLSP-Ⅰ, ISLSP-Ⅱ) were synthesized by continuous liquid phase reaction and intermediate method, respectively. The synthesized stationary phases were characterized by FTIR spectrum and SEM. The stationary phase ISLSP-Ⅰ was packed in a 50 mm × 10 mm i.d. column 1. The stationary phase ISLSP-Ⅱ was packed in a 30 mm × 10 mm i.d. column 2, and the chromatographic performences of the stationary phases synthesized by the two methods were systematically evaluated. The results showed that the column efficiency of both and the peak shapes are good, and the retentions depend on mass transfer at higher flowrate for the test sample. In the methanol-water solvent, column 2 exhibited a certain reversed-phase chromatographic separation mechanism. The relative deviation of retention times do not exceed 0.9 % for test components after 6 months’ use, indicating that the stabilities of the synthesized stationary phases were good. The test results showed that the two columns have good separation abilities for the multi-component samples of standard mixtures and the Chinese medicine extracts.

    • >Functional materials
    • Properties of Fe3O4@SiO2@IPDI-HEA Modified Waterborne Polysiloxane-Polyurethane UV-Cured Film

      2019, 36(4).

      Abstract (584) HTML (0) PDF 873.89 K (0) Comment (0) Favorites

      Abstract:Abstract: Fe3O4@SiO2@IPDI-HEA nanoparticle was prepared by solvothermal method with Fe3O4 nanoparticle as the core and acrylate as the shell. The structure of the nanoparticle was characterized by IR, TEM and XRD. The effect of the nanoparticle on the performances of water-borne polysiloxane-polyurethane photocuring system were studied by photo-DSC and TGA. The results show that the addition of Fe3O4@SiO2@IPDI-HEA particle did not obviously influence the photopolymerization property of the system, but improved significantly the heat resistance and tensile strength of the cured film. When the mass fraction of Fe3O4@SiO2@IPDI-HEA was 1.5%, the initial decomposition temperature (T5%) of the cured film was increased by 21.9 ℃, and the tensile strength was enhanced by 6.9 MPa. Moreover, Fe3O4@SiO2@IPDI-HEA can impart certain electromagnetic properties to the UV-cured film. When the frequency is in the range of 0 to 107 Hz, the dielectric constant is above 4.

    • >Review and monographs
    • Research progress in functional materials of vermiculite

      2019, 36(4).

      Abstract (1014) HTML (0) PDF 2.95 M (0) Comment (0) Favorites

      Abstract:Vermiculite is considered to be a promising non-metallic mineral in China. With two-dimensional (2D) lay-ered material structure function and high expansion performance, new functional materials of vermiculite could be designed and synthesized according to the actual needs. However, the research problems are the stability and control of the nano-scale structural for vermiculite materials. Advantages and associations of structure and properties in layered functional material are described in this paper. The structure and prop-erties of natural vermiculite are not only described, but also the research progress on the composite mate-rials of vermiculite is reviewed in recent years. Especially, the composite materials of vermiculite are de-scribed in vermiculite peeling, adsorption, catalyst carrier, organic and inorganic composites, energy stor-age, and drug carrier, which have great industrial relevance for vermiculite functional materials. The exist-ing problems in the study of functional materials of vermiculite are introduced. Finally, the research trends of this field are brought forward: the future study should be focused on vermiculite exfoliation, fabrication of multistage composite functional materials, organic-inorganic composites of vermiculite, and explora-tion of related mechanisms.

    • >Food and feedstuff chemicals
    • Purification and Thermal Degradation Kinetics of Anthocyanins from Blackcurrant

      2019, 36(4).

      Abstract (694) HTML (0) PDF 885.51 K (0) Comment (0) Favorites

      Abstract:The anthocyanins of blackcurrant were isolated and purified by combination of AB-8 macroporous resin and Sephadex LH-20, and the liquid chromatography-mass spectrometry was employed to identified anthocyanins components of blackcurrant. The degradation kinetics of anthocyanins with different purity were analyzed under different pH values and temperatures. Besides, the antioxidant activities were assessed by hydroxyl, 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2-amino-di(3-ethyl-benzothiazoline sulphonic acid-6) ammonium salt(ABTS) free radical scavenging assays. The results showed that five anthocyanins were identified in terms of delphinidin-3-glucoside,cyanidin-3-rutinoside, petunidin-3-glucoside, paeoniflorin-3,5-dihexoside and malvidin-3-galactoside. The two purified anthocyanins fractions were obtained, which were identified as delphinidin-3-glucoside (A3) and cyanidin-3-rutinoside (A4), respectively. The thermal stability of anthocyanins was strongest at pH 3.0 and temperature 50 ℃. The thermal degradation of anthocyanins with different purity were fitted well to the first-order reaction kinetics, and the correlation coefficients R2 are all above 0.9. Under the same pH value, the degradation rate constant increased, but the half-life and activation energy decreased with the increase of temperature. The IC50 of DPPH free radical scavenging rate of anthocyanins purified by macroporous resin (A1), anthocyanins extracted by ethyl acetate (A2), (A3) and (A4) were 9.45, 8.17, 5.95 and 7.62 mg/L, respectively, and the IC50 of ABTS+ free radical scavenging rate of them were 99.38, 97.21, 78.19 and 85.54 mg/L, respectively. and malvidin-3-galactoside. The two purified anthocyanins fractions were obtained by combination of AB-8 macroporous resin and Sephadex LH-20, which were identified as delphinidin-3-glucoside and cyanidin-3-rutinoside, respectively. The thermal stability of anthocyanins was strongest at pH 3.0 and temperature 50 ℃. The thermal degradation of anthocyanins with different purity were fitted well to the first-order reaction kinetics. Under the same pH value, the degradation rate constant increased, but the half-life and activation energy decreased with the increase of temperature. In vitro antioxidant experiments showed that blackcurrant anthocyanins had significant scavenging abilities of DPPH and ABTS+ free radicals.

    • >Surfactants
    • Synthesis and properties of linear-type azobenzene polyoxyethylene ether foam stabilizer

      2019, 36(4):0-0.

      Abstract (688) HTML (0) PDF 606.09 K (352) Comment (0) Favorites

      Abstract:A linear-type azobenzenepolyoxyethylene ether nonionic surfactant (PEP-600) was synthesized by p-benzeneazophenol, 1,2-dibromoethane and polyethylene glycol (PEG600), used as a foam stabilizer, to reversibly photo-control foam stability. PEP-600 was characterized by FT-IR spectra and 1H-NMR spec-trum. Besides, its surface activity and foam properties were analyzed. The results showed that the critical micelle concentration (CMC) of PEP-600 was 4.99×10-3 mol/L and the surface tension was 48.09 mN/m at this concentration. The surface excess and HLB value of PEP-600 were 2.48×10-3 mmol/m2 and 14.20, respectively. Meanwhile, the foaming ratio of PEP-600 was about 12 and foam half-life was 220 s with sodium dodecyl sulfate (0.1 g·L-1), meaning that PEP-600 owned the excellent foaming property, which was attributed to the tight arrangement at the surface of foam film. PEP-600 had the potential to apply in foam dyeing as a foam stabilizer.

    • Synthesis and Properties of Surfactants: Long-Chain n-Alkyl-3-Methylpyridinium Bromide

      2019, 36(4):0-0.

      Abstract (917) HTML (0) PDF 607.90 K (658) Comment (0) Favorites

      Abstract:Long-chain ionic liquids surfactants: n-alkyl-3-methylpyridinium bromide [Cnmpy][Br] (n: the carbon numbers of hydrophobic tails, n=12, 14, 16) was synthesized by condensation reaction using 3-methylpyridinium and n-alkyl bromide as raw materials. The ionic liquids surfactants were characterized by FT-IR and NMR (1H, 13C). The critical micelle concentrations (CMC) of surfactants were determined by employing conductometry and Du Noüy ring method. The effects of temperature, carbon chain length on the CMC were also investigated, and the micellization thermodynamic parameters were calculated. The antibacterial activities were screened for compounds against three bacteria. The results showed that the CMC values for [Cnmpy][Br] (n=12, 14, 16) was found to be 9.52, 2.32 and 0.591 mmol/L, respectively. The CMC value measured by Du Noüy ring method were 1.21 to 1.31 times lower than that by conduc-tometry, The relationship between the number of carbon atoms in alkyl chain and CMC value were in ac-cordance with the Stauff-Klevens rule. The variation of CMC values of the compounds with temperature were first decreased and finally increased. The ΔGm and ΔHm values of the [Cnmpy][Br] surfactants were negative indicated spontaneous and radiative nature of the micellization process. The results of antibacterial activities showed that the [C14mpy][Br] surfactants had most intense antibacterial activities against three bacteria. The diameter of inhibition zone was 25.0, 28.0 and 26.0 mm, respectively.