• Volume 36,Issue 6,2019 Table of Contents
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    • >Functional materials
    • Adsorption of Acid Red R on Magnetic Graphene Oxide Modified by β-cyclodextrin

      2019, 36(6).

      Abstract (472) HTML (0) PDF 790.68 K (0) Comment (0) Favorites

      Abstract:In this study, the graphene oxide (GO) was prepared by Hummers oxidation method, the magnetic graphene oxide modified by β-cyclodextrin (Fe3O4@GO/β-CD) composite was fabricated by the in-situ co-precipitation method and characterized by SEM, TEM, FT-IR, laser granularity analyzer, Brunauer-Emmett-Teller(BET) surface area measurement and vibrating sample magnetometer. The results show that the particle size of Fe3O4@GO/β-CD is about 460 nm, the specific surface area is 252.3 m2/g and the saturation magnetization of Fe3O4@GO/β-CD is 73.5 emu/g. The adsorption of Acid Red R on Fe3O4@GO/β-CD is a pseudo second-rate kinetic process, the adsorption kinetics constant of Acid Red R is found to be 5.18′10-3 g/(mg•min), and the adsorption pattern of Acid Red R on the Fe3O4@GO/β-CD follows the Langmuir model very well, and the maximum adsorption capacity of Acid Red R on the Fe3O4@GO/β-CD is 228.31 mg/g at pH=3.0.

    • Preparation of pentaerythritol phosphate - expandable graphite /waterborne epoxy composite coating and its flame retardant and anticorrosive properties

      2019, 36(6).

      Abstract (642) HTML (0) PDF 5.32 M (1) Comment (0) Favorites

      Abstract:PEPA-EG/EP composite coatings were prepared by adding pentaerythritol phosphate (PEPA) and ex-pandable graphite (EG) as composite fillers to waterborne epoxy resin (EP). The effects of composite fillers with different mass ratios on the flame retardancy and corrosion resistance of PEPA-EG/EP com-posite coatings were investigated by fire resistance limit analysis, thermogravimetric analysis, limiting oxygen index test, vertical burning test, residual carbon scanning electron microscopy analysis, residual carbon infrared analysis, electrochemical impedance spectroscopy testing and adhesion experiments. The results show that when the mass ratio of composite filler to waterborne epoxy resin is 15:100, composite coating has the best flame retardant properties and corrosion resistance. The time when the back temper-ature of the steel sheet reaches 500℃ is 38 min,the limiting oxygen index reaches 27.2%,the vertical combustion performance exhibits V-1 level,the residual carbon amount increases from 0.55% to 27.79% at 800℃,and EP2 has the highest impedance value during electrochemical impedance spectroscopy testing af ter 480 hours of immersing.

    • Preparation and Thermal Properties of Nanoencapsulated Binary Phase Change Materials

      2019, 36(6).

      Abstract (652) HTML (0) PDF 2.08 M (0) Comment (0) Favorites

      Abstract:Nanoencapsulated phase change materials were prepared through surfactant-free emulsion polymerization with n-octadecane (C18) and n-butyl stearate (BS) as binary cores and poly(methyl methacrylate) (PMMA) as shell. The effects of the type and dosage of emulsifier, the type and dosage of initiator and core/shell mass ratio on nanocapsules were studied. The surface morphology, chemical structure and thermal properties of phase change nanocapsules were characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-Ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analyzer (TGA). The results indicate that the best preparation conditions of nanocapsules are when the alkyl vinyl sulfonate (AVS) dosage is 3.0wt% to oil phase, ammonium persulfate (APS) dosage is 1.2wt% to MMA and core/shell mass ratio is 2:4. At the moment the monomer conversion of nanocapsules is the highest, particle size is the smallest and spherical morphology is the most regular. In addition, phase change nanocapsules have good latent heat storage capacity and heat resistance, and their melting enthalpy and crystallization enthalpy are 56.89 J/g and 54.02 J/g, respectively. The finished fabrics with phase change nanocapsules have better thermoregulation effect.

    • Synthesis and Characterization of 1-(2-Furyl)-3-phenyl- 2-propen-1-one

      2019, 36(6).

      Abstract (606) HTML (0) PDF 1.14 M (0) Comment (0) Favorites

      Abstract:A chalcone compound 1-(2-furyl)-3-phenyl-2-propen-1-one was synthesized by using 2-acetylfuran and benzaldehyde as raw material and a Claisen-Schmidt condensation reaction with in alkaline solution. After examining the effects of various factors on the condensation reaction,The effect of reaction time, KOH mass fraction and molar ratio of benzaldehyde to 2-acetyl furan on yield of product FPPO was investigated by response surface experiment optimization method, and the optimum process parameters were obtained. The experimental results show that when n (benzaldehyde): n (2-acetylfuran) = 1.47:1, the reaction time is 1 h, and the mass fraction of potassium hydroxide of the catalyst is 5.75%, the yield of product FPPO is 63.3%. After the phase transfer catalyst Polyethylene glycol-400(PEG-400) 6g was added to the reaction system, the product yield was up to 88.5%.The structure was confirmed by UV, FTIR and 1H NMR.At the same time, the fluorescence performance and thermal stability of FPPO were tested by fluorescence spectrometer, DSC and TGA. The fluorescence performance test results show that FPPO has good fluorescence performance and the fluorescence intensity is 3.13 × 105 a.u. DSC and TGA results show that FPPO has good thermal stability,and heat resistant temperature is about 140 °C.

    • Preparation and Corrosion Resistance of Sulfonated Polyaniline/Silicone Resin Coatings

      2019, 36(6).

      Abstract (769) HTML (0) PDF 5.62 M (0) Comment (0) Favorites

      Abstract:Two kinds of sulfonated polyaniline (PANI-SDS, PANI-LGS) were synthesized by chemical oxide method with sodium dodecyl sulfate (SDS) and sodium lignosulfonate (LGS) as dopant, followed by mixed with silicone resin (SiR) prepared by gel-gel method, and then coated on the surface of Q235 steel to prepare composite aniticorrosion coatings. The structures of sulfonated PANI were characterized by FTIR, and the basic properties of PANI-SDS and PANI-LGS were compared. The hydrophobicity, adhesion, mechanical properties and anticorrosion properties of SiR, PANI-SDS/SiR and PANI-LGS/SiR composite coatings were investigated, and the anticorrosion mechanism of the composite coating was described. The results showed that PANI-LGS/SiR composite coating had better hydrophobic property. The water contact angle of the coating was 113.0°, and the water absorption was only 7.58%. Electrochemical test results showed that the composite coating had better corrosion resistance to Q235 steel. The corrosion rate was 5.56×10-3 mm/a. The metal corrosion is protected by the effect of physical barrier and anodic protection of the composite coatings.

    • Preparation of Functionalized Graphene Modified Amine-Free Waterborne Polyurethane

      2019, 36(6).

      Abstract (834) HTML (0) PDF 1.06 M (1) Comment (0) Favorites

      Abstract:Using polycaprolactone diol (PCL), toluene diisocyanate (TDI) and methyl methacrylate ( MMA ) as main raw materials, waterborne polyurethane-acrylate emulsion (WPUA ) prepolymer was synthesized. the product obtained by coupling modified nano - SiO2 with graphene oxide was polymerized in situ with the prepolymer. at the same time, carboxylic acid hydrophilic chain extender and sulfonic acid hydrophilic chain extender were used to prepare functionalized graphene-modified waterborne polyurethane-acrylate composite emulsion ( SiO2-NH2-go/ WPUA ) with solvent-free and zero VOC characteristics by self-emulsifying method .Compared with waterborne polyurethane-acrylate ( WPUA ), the composite emulsion ( SiO2-NH2-go/ WPUA) has better temperature resistance and film properties. when the mass fraction of SiO2-NH2-go is 0.75 %, the thermal decomposition temperature of the composite emulsion film is 77.32 ℃ higher than that of the unmodified emulsion film;The tensile strength increased to 81.28 MPa;and the T- peel strength of the adhesive prepared by the composite emulsion reached 15.4 N in aluminum foil / PVC film;Indicators such as easy oxides meet the standards for pharmaceutical packaging containers, indicating that the waterborne polyurethane adhesive is suitable for pharmaceutical packaging.

    • Preparation and Photocatalytic Water Splitting for H2 Production of CDots-(001)TiO2 nanosheets

      2019, 36(6).

      Abstract (766) HTML (0) PDF 9.55 M (0) Comment (0) Favorites

      Abstract:Using tetrabutyl titanate, hydrofluoric acid and graphite rod as raw materials, the carbon dots with high catalytic activity were loaded on the (001) crystal plane of TiO2 nanosheets by simple hydrothermal method to prepare CDots-(001) TiO2 nanosheets. Through the synergistic effect of the high catalytic activity of the (001) crystal plane and the carbon point, the light absorption, the transport and sepa-ration efficiency of carriers of TiO2 nanosheets improves, thus the hydrogen production performance of the material is effectively improved. The UV-vis DRS, PL, and transient photoresponse analysis results show that the visible light absorption of TiO2 nanosheets with exposed (001) crystal plane enhances after loading with carbon dots, and the separation and transmission rate of photogenerated carriers are accelerated. The photocurrent density of CDots-(001)TiO2 nanosheets is roughly fourth as high as that of TiO2 under intermittent visible light irradiation. The photocatalytic hydrogen production rate of CDots-(001)TiO2 nanosheets is up to 5859 μmol/(h·g), and the quantum efficiency is up to 9.6%.

    • Steam Crystallization of EMT Zeolite and Effect on Olefins Purification Performance

      2019, 36(6).

      Abstract (773) HTML (0) PDF 2.54 M (0) Comment (0) Favorites

      Abstract:In this study, a hexagonal EMT zeolite (denoted as SEMC-2) was successfully fabricated by combination of template 18-crown-6 ether with a steam crystallization (SAC) method. The effects of both SAC time and temperature on the crystal form were emphatically studied at the Na2O/Al2O3 molar ratio of 2.4. The regular hexagonal platelet SEMC-2 zeolite with diameter of 3~4 μm and thickness of 300~400 nm was synthesized under crystallization temperature 110℃, crystallization time 6 days. Similar to EMT zeolite prepared by the traditional hydrothermal crystallization method (denoted as HEMC-2), SEMC-2 zeolite could also deeply purify the trace amounts of polar methanol and propanal to below mole percent 0.0001% from gaseous olefins at an initial mole percent 0.02% or 0.1%. Moreover, the breakthrough times and cumulative adsorption amounts of HEMC-2 and SEMC-2 zeolite had no obvious difference. The regeneration experiment indicated that the SEMC-2 zeolite had more stable structure and longer service life. The in-situ FTIR spectra demonstrated the adsorption processes of the SEMC-2 zeolite for methanol and propanal were a physical adsorption mainly via interaction between the polar-oxygenated compounds O lone-pair eletrons and the SEMC-2 zeolite Na+.

    • Synthesis and Properties Characterization of Fe3+Fluorescent Probe Based on Rhodamine B

      2019, 36(6).

      Abstract (1040) HTML (0) PDF 801.26 K (1) Comment (0) Favorites

      Abstract:Abstract: A probe base on Rhodamine B derivative F-1(3',6'-bis(diethylamino)-2-phenylspiro [isoindo-line-1,9'-xanthen]-3-one) has been synthesized and developed, which was prepared by condensation reac-tion of Rhodamine B with aniline. Its structure was characterized by 1H NMR, 13C NMR and HRMS. It was found that after the Fe3+ added, the probe system changed from colorless to purple and the fluores-cence intensity was significantly enhanced, while other metal ions (Na+, K+, Ca2+, Mg2+, Zn2+, Hg2+, Co2+, Cd2+, Ni2+, Cu2+, Mn2+, Ag+, Pb2+, Cr3+, Fe2+) were not disturbed. By measuring the ion selectivity, ion competi-tiveness, concentration gradient, Job curve, and the effect of pH on the fluorescence intensity of probe compound F-1, we found that probe compound F-1 presents a good linear relationship in pH=5-7 (2.0×10-6~1.8×10-5 mol/L), and has the potential of qualitative and quantitative detection of trace Fe3+ in bio-logical organisms and environment.

    • Preparation and Properties of Comb-like Modified Styrene - Maleic Anhydride Copolymer

      2019, 36(6):0-0.

      Abstract (852) HTML (0) PDF 1.08 M (0) Comment (0) Favorites

      Abstract:The active branched chain (IP550) with primary amine was synthesized by isatoic anhydride (IA) and methoxypolyethylene glycols550 (MPEG550). The comb-like modified polymer surfactant (SMA-IP550) was prepared by amidation reaction between styrene-maleic anhydride copolymer (SMA) and IP550. The synthesis process of products was investigated and the chemical structure of SMA-IP550 was characterized by FTIR and 1HNMR. The results showed that the IP550 with 79.3% yield were achieved when the conditions were controlled as the amount of catalyst(4-dimethylaminopyridine) 0.9% based on the total mass of reactants, the molar ratio of IA to MPEG550 1:1, reaction temperature 120℃ and reaction time 30 min. The modified SMA(SMA-IP550) with 42.5% grafting yield was obtained when the temperature was 140℃, the molar ratio of IP550 to MA was 0.5:1, the solid content was 30% and the reaction time was 2 h. By comparing the dispersion, viscosity reduction, emulsification and wettability of modified SMA with different branched-chain lengths, the results showed that the structure of comb-like modified styrene-maleic anhydride copolymer can be adjusted, which was closely related to the emulsification and dispersion.

    • >Surfactants
    • Solubilization Performance for Quaternary Ammonium Salt Cationic Surfactants Microemulsion Systems

      2019, 36(6).

      Abstract (794) HTML (0) PDF 565.05 K (0) Comment (0) Favorites

      Abstract:Two kinds of microemulsion systems for quaternary ammonium salts surfactan, octadecyl trimethyl ammonium chloride (OTAC) and hexadecyl trimethyl ammonium bromide (CTAB) ,were studied on their solubilization properties for single organic compound and organic mixtures (n-octaneand binary mixtures of n-dodecane/n-hexane, n-dodecane/ n-heptane and n-dodecane/n-octane). The optimal alcohol dosage (A*) and the optimum solubilization parameter (SP*) of Winsor III microemulsions were studied. The results suggested that the two surfactant microemulsion systems showed similar patterns. With the increase of salinity, SP* increased monotonically and A*decreased monotonically. With the increase of surfactant concentration, A* increased, while, SP *increased first and then decreased. For the binary organic mixtures, the relationship between A* and EACN or SP* and EACN is the same no matter what is the components in the organic mixtures. The fitted equations for the binary organic mixtures were used in the prediction for quaternary organic mixtures. The predicted A* and SP* data coincided with the experimental values satisfactorily, which means that the obtained functional relationship can be used to predict A* and SP*in the similar range of EACN for different organic mixtures.

    • >Biological engineering
    • Preparation, antioxidant and lymphocyte proliferation activities of Spirulina Polysaccharide Iron Complex

      2019, 36(6):0-0.

      Abstract (868) HTML (0) PDF 1.42 M (0) Comment (0) Favorites

      Abstract:【Objective】The aim of the present research was to prepare an organic iron compound, Spirulina polysaccharide iron complex (SP-Fe), evaluate its antioxidant activity and lymphocyte proliferation activities. 【Method】SP-Fe was prepared by chemically modification using chloride ferric and Spirulina polysaccharide (SP), which was characterized by fourier transform infrared (FTIR), differential scanning calorimetry (DSC), pyrolysis gravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM).【Results】The iron content (16.42?1.17%) of SP-Fe complex was obtained. By 5-axe cobweb charts, the results showed antioxidant activity of SP-Fe complex was higher than that of SP. The released iron content reached 83.64% in artificial intestinal juice for a prolonged time after arti-ficial gastric juice conditions. The lymphocytes proliferation of SP-Fe complex was increased by 44.35% comparing with that of SP at the sample concentration of 31.25μg/mL.【Conclusion】The SP-Fe complex had potent antioxidant activities in vitro assays and could be applied as a novel iron source in dietary supplements.

    • >Modernization technology of traditional Chinese medicines
    • Purification, antioxidant activity and antibacterial effect of tannins from Eucalyptus Grandis x E. Urophylla

      2019, 36(6):0-0.

      Abstract (715) HTML (0) PDF 586.07 K (0) Comment (0) Favorites

      Abstract:The tannins from bark and leaf of Eucalyptus Grandis x E.Urophylla were purified by NKA-9 macroporous resin, the antioxidant activities were evaluated from the scavenging activities of 1,1-diphenyl-2 -picrylhydrazyl radical (DPPH•) and hydroxy radical (•OH), and the antimicrobial activities against 5 food-borne pathogenic bacterium were tested by the disk diffusion method. When the conditions for dynamic purification were loading of 0.8 g/L sample solution with 10 mL, and complete desorption with 3 BV of 80% ethanol, the mass fraction of bark tannins purified products was 47.82%. When the conditions for dynamic purification were loading of 0.5 g/L sample solution with 10 mL, and complete desorption with 3 BV of 80% ethanol, the mass fraction of tannins purified products from leaf was 37.00%. IC50 values of the purified tannins of bark and leaf on DPPH· scavenging effect were 0.0119 and 0.0121g/L, respectively. When the concentration was 0.5g/L, the scavenging rates on ·OH of the purified tannins of bark and leaf were equivalent to 2.55 and 2.19 times of VC, that of VC was 24.20%. The antimicrobial activities of purified tannins against Escherichia coli, Staphyloccocus aureus, Shigella, Salmonella, Bacillus cereus were better than the crude extracts, and the diameter of antibacterial zone of purified tannins of bark and leaf against Shigella were 13.25 and 12.50mm.

    • >Catalysis,separation and purification technology
    • Visible light driven reduction of CO2 to methanol over CuO/TiO2 nanofibers

      2019, 36(6).

      Abstract (681) HTML (0) PDF 3.50 M (0) Comment (0) Favorites

      Abstract:TiO2 nanofibers with a diameter of 8~10nm were successfully prepared by vapor-phase growth with mesoporous SiO2 spheres as templates and TiCl4 as precursor. Furthermore, CuO/TiO2 nanofibers with a heterojunction structure were also prepared through impregnation method for visible-light driven reduction of CO2 to methanol. XRD, SEM, TEM, XPS, ultraviolet visible diffuse reflection(UV-Vis) and photoluminescence(PL) were used to characterize the crystal structure, morphology, chemical valence, visible light absorption intensity and electron-hole recombination rate, respectively. Compared to P25 and anatase TiO2 nanoparticles, TiO2 nanofibers show much lower fluorescence intensity and more stable photogenerated electron-hole pair. Loading of CuO onto TiO2 nanofibers may further reduce the fluorescence intensity and enhance absorption of visible light. Under the irradiation of 300W xenon lamp for 5h, the yields of methanol over CuO/P25 was 696μmol/g-cat, and further enhanced to 1791μmol/g-cat over CuO/TiO2 nanofibers, 165% higher than that over CuO/P25.

    • Preparation and Catalytic Benzylation Performance of Fe-hierarchical Porous Hβ

      2019, 36(6).

      Abstract (815) HTML (0) PDF 1.05 M (0) Comment (0) Favorites

      Abstract:Hierarchical porous Hβ molecular sieve was obtained by alkaline treatment of NaOH solution for Hβ molecular sieve. Fe-hierarchical porous Hβ molecular sieve was prepared by impregnation method under the condition of 0.1 mol/L alkali concentration. The samples were characterized by XRD, XRF, N2 adsorption-desorption, SEM-EDS, Fourier transform infrared spectroscopy, NH3-TPD and Py-FTIR. The results showed that the samples with the proper alkali concentration treatment could maintain the microporous framework of Hβ molecular sieve while mesopore was introduced. Fe-hierarchical porous Hβ molecular sieve also could maintain the micro-mesoporous structure, and the active component Fe2O3 could be well dispersed on the surface of the carrier. The benzene and benzyl chloride were used to investigate the performance of Fe-hierarchical porous Hβ in the synthesis of diphenylmethane reaction. Compared with the Fe-Hβ catalyst, Fe-hierarchical porous Hβ effectively improved the diffusion performance of the reactants and products. The conversion of benzyl chloride and the selectivity of diphenylmethane increased by 9.4% and 3.2%. In the meantime, the catalyst showed excellent anti-deactivation ability.

    • Preparation of Low-load Ru-W-B/NaY Catalyst and Catalytic Performance for Hydrogenation of Hydroquinone

      2019, 36(6).

      Abstract (786) HTML (0) PDF 1.22 M (1) Comment (0) Favorites

      Abstract:A series of low-load ruthenium-based catalysts were prepared by impregnation-chemical reduction method. A small amount of W was added to the Ru-B binary catalyst system, and the catalytic performance of the catalysts was improved. Furthermore, when the inverse addition, ultrasonic assisted, and PEG-coated carrier NaY were used, the performance of the ruthenium-based catalysts is superior. The structure, composition and surface morphology of the catalyst were characterized by XPS, H2-TPD, XRD, SEM and ICP-OES. It was found that the reverse addition, W addition, ultrasonic assisted, and PEG-coated carrier NaY are beneficial to more uniformly dispersed for the active particles and have more active sites. The activity of the prepared catalysts was tested via hydrogenation of hydroquinone to 1,4-cyclohexanediol. It was found that Ru-W-B/NaY-IUP(1500)0.6 has the most excellent hydrogenation performance. The conversion of hydroquinone was 99.7 %, the selectivity to 1,4-cyclohexanediol was 92.3 %, while the ruthenium loading was only 0.45 %. In addition, the effect of pH value on the hydrogenation of hydroquinone was studied, the results showed that the pH value of the reaction solution had a great influence on the reaction. When the reaction solution was alkaline, the reaction rate was greatly accelerated, indicating that the alkaline environment is more favorable to the hydrogenation of hydroquinone to 1,4-cyclohexanediol.

    • The catalytic performance of MOx/Y catalyst in toluene oxidation with ozone at room temperature

      2019, 36(6).

      Abstract (1523) HTML (0) PDF 580.76 K (0) Comment (0) Favorites

      Abstract:10%MOx/Y (M= Mn, Co, Ni, Fe, Ce, Cu) and 5%MnO2-5%MOx/Y (M= Ce, Co, Cu) catalysts prepared by incipient-wetness impregnation method for toluene oxidation with ozone at room temperature. The catalysts were characterized by XRD, BET, H2-TPR and toluene adsorption techniques. The re-sults revealed that 10%MnO2/Y catalyst showed a larger surface area and pore volume, a better tolu-ene adsorption performance, promoting the reaction of toluene oxidation with ozone and the further oxidation of the by-products, thus, 10%MnO2/Y catalyst gave a higher toluene conversion and COx selectivity. With the addition of CuO, the interaction between CuO and MnO2 improved the reduction property of 10%MnO2/Y catalyst and promoted the further oxidation of CO into CO2 with a higher CO2: CO molar ratio. Thus, 5%MnO2-5%CuO/Y catalyst exhibited a high catalytic activity in toluene oxidation with ozone at room temperature with t95 of 240 min, COx selectivity of 80.6% and CO2: CO molar ratio of 4.970. It could be speculated from the results of GC-MS that benzociacid and formic acid phenylmethyl ester as the by-products blocked the catalysts pores and occupied active sites on the surface of the catalysts, resulting in the inactivation of the catalysts.

    • Properties of FeCoY catalysts and catalytic reduction activity for desulfurization and denitrification

      2019, 36(6).

      Abstract (663) HTML (0) PDF 832.86 K (0) Comment (0) Favorites

      Abstract:Abstract:The catalyst samples of different load and different supports were prepared by equal volume impregnation method using FeCoY as active component, the catalyst was characterized by XRD, BET and H2-TPR. The experiments were investigated on aminiature fixed bed reactor about the activity of catalysts for simultaneous desulfurization and denitrification and oxidation resistance by using CO as reducing agent gas. The results show: the nitric acid pretreated catalyst can significantly improve the performance of the catalyst. The catalyst 10Fe6Co3Y/AC with the active components Fe, Co and Y respectively occupying 10%, 6% and 3% of the carrier is the best combination and the conversion rate of desulfurization and denitrification can reach 100%, The temperature at which the desulfurization and denitrification conversion rate reaches 90% at the same time is about 218 °C. XRD results shows that the catalyst has a spinel structure. The results of antioxidant experiments show that: it is preliminarily judged that the desulfurization process follows the Redox-COS synergistic mechanism, while the denitration only follows the COS mechanism., O2 with a volume fraction of 1% exhibits different toxic effects on the active sites of NO and SO2.

    • Synthesis of Esters of Succinic Acid by Acetylene Dicarbonylation

      2019, 36(6).

      Abstract (860) HTML (0) PDF 560.40 K (0) Comment (0) Favorites

      Abstract:Using C2H2, CO and n-butanol as raw materials, using PdBr2 as the main catalyst in the synthesis of succinate by the dicarbonylaon under normal pressure and 55℃ conditions. The effects of the amount of catalyst, the type and amount of auxiliaries, the type of solvent, reaction temperature and reaction time on yield of dibutyl succinate, dibutyl maleate and dibutyl fumarate were investigated. The experimental results showed that in optimal conditions : the amount of PdBr2 was 0.04g, n(PdBr2):n(LiBr)=1:8, 0.1mL methanesulfonic acid, the solvent was acetonitrile, n(C2H2):n(CO)=1:2, 101KPa, reaction at 55°C for 3h, the yield of dibutyl succinate, dibutyl maleate and dibutyl fumarate reached 76.11%.

    • >Perfumes and essences
    • Synthesis and Characterization of a Dipeptide Sweetener

      2019, 36(6).

      Abstract (948) HTML (0) PDF 514.04 K (0) Comment (0) Favorites

      Abstract:The dipeptide sweetener N-[3-(3-Hydroxy-4-methoxyphenyl)propyl]-α-L-aspartyl-β-cyclohexyl-L-alanine-1-methyleste (III) was synthesized from 3-(3-hydroxy-4-methoxyphenyl)propanal (II) and a dipeptide (I) via a reductive amination reaction under an overall yield of 50%. The intermediate viz. 3-(3-hydroxy-4-methoxyphenyl)propanal (II) was prepared via a Witting reaction followed by a hydrogenation and a DIBAL-H reduction; while the dipeptide (I) was synthesized via a condensation of 3-cyclohexyl-L-alanine and Boc-L-aspartic acid-4-benzyl ester. The structure of product (III) was confirmed by IR, 1HNMR, 13CNMR and HRMS spectroscopic methods, and its sweetness was verified to be about 25000 times than sucrose. The optimum reaction conditions for the synthesis of product (III) were determined as follows: n(II):n(I)=1:1, the loading of Pd/C catalyst is 10% of the total weight of the reaction material in 80% methanol, the preferred reaction temperature was 40 ℃, and reaction time was 20 h.

    • >Drug and cosmetic materials
    • Study on the antioxidant properties of 4-methyl-7-hydroxycoumarin

      2019, 36(6).

      Abstract (1012) HTML (0) PDF 1.03 M (0) Comment (0) Favorites

      Abstract:4-methyl-7-hydroxycoumarin was prepared by the acid-catalytic reaction of the resorcinol with ethyl acetoacetate and then 4-methyl-7-acetoxylcoumarin was obtained by the esterification of 4-methyl-7-hydroxycoumarin. The structure of the compound was confirmed by melting point, nuclear magnetic resonance hydrogen spectroscopy (1H NMR), nuclear magnetic resonance carbon spectroscopy(13C NMR) spectrum, and ultra high performance liquid chromatograph electrospray ion source mass spectrometer(UHPLC-ESI-MS). Antioxidant abilities of the obtained compounds were evaluated by inhibiting 2,2’-azobis(2-amidinopropanehydrochloride) (AAPH)-, Cu2 /glutathione (GSH)-, and ?OH- induced oxidation of DNA. The radical-scavenging properties of the obtained compounds were estimated by quenching 2,2’-azinobis(3-ethylbenzothiazoline-6-sulfonate) cationic radical (ABTS ?), 2,2’-diphenyl-1-picrylhydrazyl (DPPH), and galvinoxyl radicals, and then the structure-activity relationship of these compounds could be explored. The results showed: (1) 4-methyl-7-hydroxylcoumarin not only exhibited the ability to protect DNA against AAPH, Cu2 /GSH and ?OH-induced oxidation, but also scavenged ABTS ?, DPPH, and galvinoxyl radical, respectively; (2) 4-methyl-7-acetoxylcoumarin can only inhibit the DNA oxidation reaction by ?OH and Cu2 /GSH, and scavenge ABTS ? and DPPH radicals; (3) 4-methyl-7-acetoxylcoumarin had antioxidant property, while antioxidant property was reduced when hydroxyl was protected, revealing that 4-methyl-7-hydroxylcoumarin has strong radical-scavenging properties and reduction ability , can be a potential antioxidant.

    • Separation and Purification of Flavonoids in Malus toringoides (Rehd.) Hughes Leaves with Macroporous Resins and Evaluation of Anti-Inflammation Activities in Vitro

      2019, 36(6).

      Abstract (749) HTML (0) PDF 688.53 K (0) Comment (0) Favorites

      Abstract:The purpose of this research was to study the purification process of flavonoids in Malus toringoides (Rehd.) Hughes leaves (FMTs), and the purification parameters were optimised by adsorption and desorption tests. AB-8 resin was selected by comparing the adsorption and desorption ability of FMTs on twelve types of resins. The results showed that the optimal purification parameters of static adsorption and desorption were the sample at pH=4 with 3 h of adsorption; the desorption solvent was 70 % ethanol (pH = 7.0) with 3 h of desorption. The best dynamic parameters were a sample loading amount of 9 bed volumes (BV) at a feeding flow rate of 2 BV h-1 and washing the column with 6 BV of water, followed by subsequent flushing with 20 % (6 BV), 40 % (6 BV), 60 % (6 BV) and 80 % (6 BV) ethanol in water (v/v) at an elution flow rate of 2 BV h-1. Under these conditions, the purity of FMTs increased from 32.79% to 59.18%. The existence of flavonoids was confirmed by their characteristic functional groups that were identified by infrared spectroscopy. Meanwhile, FMTs in the dosage range of 50 to 400 ?g mL-1 showed a significant anti-inflammatory effect on lipopolysaccharide (LPS)-induced RAW 264.7 mouse macrophage cells, which could inhibit the secretion of NO, IL-6, IL-1β and TNF-α through the inhibition of inflammatory-related gene expression.

    • Preparation and Release Properties of Methotrexate Intercalated MgAl-LDH Composites

      2019, 36(6).

      Abstract (862) HTML (0) PDF 1.32 M (0) Comment (0) Favorites

      Abstract:Methotrexate intercalated Mg-Al layered double hydroxide composites (MTX-LDH) were prepared via combination of coprecipitation and hydrothermal synthesis by using Mg(NO3)2•6H2O and Al(NO3)3•9H2O as main materials. The effects of main technological conditions on drug loading rate, particle size and dispersion of MTX-LDH composite were analyzed by orthogonal test. The results showed that the composites had good monodispersity, suitable particle size (175.6nm), and high drug loading rate (18.9%) when the reaction temperature was 60℃, and the amount of Mg(NO3)2•6H2O, Al(NO3)3•9H2O, MTX and polyethylene glycol 400 were 2.67 mmol, 1.33 mmol, 0.2 mmol and 15 mL respectively. The structure, thermodynamic properties and micro-morphology of the samples were studied by FTIR, XRD, TG and TEM. The release properties of MTX-LDH composite particles in different pH buffer solutions were investigated emphatically. It was indicated that the composites had the characteristics of pH-responsive release and good sustained release properties in weak acid environment with pH=5.8, and the cumulative release rate at 12 h was up to 93.7%. Moreover, the release mechanism of laminate dissolution coexist with displacement diffusion was confirmed by the thermodynamic release model.

    • >Food and feedstuff chemicals
    • Antioxidant Behavior of Protocatechuic Acid Alkyl Esters in Oil-in-water Emulsion

      2019, 36(6).

      Abstract (677) HTML (0) PDF 861.62 K (0) Comment (0) Favorites

      Abstract:Four protocatechuic alkyl esters were synthesized by direct esterification reaction with protocatechuic acid and a series of alkyl alcohols as raw materials, and their structures were identified by infrared and 1HNMR spectrometers. The DPPH assay and ABTS assay were used to determine their free radical scavenging capacity. The Schaal oven test was used to determine their antioxidant efficiency in oil-in-water emulsion. Results showed that the free radical scavenging capacity of protocatechuic acid was enhanced by esterification, and it increased with the increase of alkyl chain length. Esterification of protocatechuic acid enhanced its antioxidant activity in the oil-in-water emulsion. As the alkyl chain length increased, the antioxidant efficiency increased first and then decreased, it reached the maximum at PA-C8. All protocatechuic alkyl esters have a maximum of antioxidant efficiency in rapeseed oil emulsions with the volume fraction of emulsifier 4% and the oil to water ratio 2:8. Compared with emulsions with the addition of protocatechuic acid, the time to reach a conjugated diene value of 1 and the p-anisidine value of 6 was significantly increased.

    • >Electro-organic chemistry and industry
    • Preparation and Electrochemical Performance of Lithium Ion Battery cathode Materials Li4Ti4.9Ni0.1O12

      2019, 36(6).

      Abstract (531) HTML (0) PDF 634.86 K (0) Comment (0) Favorites

      Abstract:The spinel Li4Ti4.9Ni0.1O12 anode material for lithium-ion batteries were successfully synthesized by solid-state reaction method using Ti(OC4H9)4, CH3COOLi?2H2O and Ni(CH3COO)2?4H2O as raw materials.The crystalline structure, morphology and electrochemical properties of the obtained materials were characterized by XRD, SEM, half cell charge-discharge tests and AC impedance. The results showed that The synthesized Li4Ti4.9Ni0.1O12 composite particles were homogeneous without impure phase. The first discharge capacity was 173.3mAh g-1 and coulombic efficiency was 97.4% at 0.5 C rate.The specific capacity remained163.4mAh g-1 after 50 cycles with a capacity retention of 94.3%。

    • Lithium storage properties of Si/VGCF composite electrodes

      2019, 36(6).

      Abstract (497) HTML (0) PDF 4.52 M (0) Comment (0) Favorites

      Abstract:Nano-silicon particles and vapor-grown carbon fiber composites (Si/VGCF) were prepared by liquid phase mixing method in order to improve the conductivity and cycling stability of the silicon anode of lithium ion batteries. The preparation conditions of the Si/VGCF, the optimum content of VGCF were investigated. The morphology and crystal structure of the Si/VGCF materials were characterized using Scanning Electron Microscopy and Transmission Electron Microscopy. The electrical conductivity, BET specific surface area and pore size of the Si/VGCF composites were tested and calculated. The electrochemical properties of Si/VGCF electrodes were tested by using cyclic voltammetry, galvanostatic charge-discharge and alternating current impedance methods. The results indicate that the hierarchical network structure formed by Si and VGCF has abundant ions and electrons conductive channels. Also, the structure with the rich pores can alleviates the volume effect of Si particles during the processes of the intercalation/deintercalation of Li , which significantly improves the utilization and electrochemical stability of the electrode active materials. When m(Si):m(VGCF) is 1:0.5, the Si/VGCF electrode delivers a reversible capacity of 1470 mAh?g-1 at a current density of 500 mA?g-1 after 100 cycles.

    • >Leather chemicals
    • Preparation and Properties of Blocked Solvent – free Polyurethane

      2019, 36(6).

      Abstract (945) HTML (0) PDF 533.66 K (0) Comment (0) Favorites

      Abstract:The blocked solvent-free polyurethane is mainly composed of hydrogenated phenylmethane diisocyanate (H12MDI) and polyester diol 2000, using methyl ethyl ketone oxime (MEKO) and caprolactam as blocking agents and dibutyltin dilaurate (DBTD) as catalyst. The blocked Solvent – free Polyurethane(SFPU) film was prepared by a prepolymer blocking method. The deblocking temperature and thermal properties of the blocked SFPU membrane were investigated by TGA and DSC. The effects of different sealers, leveling agents, catalyst dosage, oven temperature and blocking ratio on the deblocking temperature of the blocked SFPU, the curing conditions of the blocked SFPU and the film forming properties were investigated. The results showed that the deblocking temperature of the blocked SFPU with MEKO as a blocking agent was 143 ° C and the deblocking temperature of the blocked SFPU with caprolactam as a blocking agent was 163 ° C by differential scanning calorimetry (DSC).TGA analysis showed that at the same deblocking temperature, the blocking speed of the blocked SFPU with MEKO as the blocking agent was significantly higher than that of the blocked SFPU with caprolactam as the blocking agent. Under suitable curing conditions(The oven temperature is 140 ° C, the leveling agent mass fraction is 5%, and the catalyst mass fraction is 5‰. ), the blocked SFPU can be cured into a film, and the lower the blocking ratio of the blocked SFPU, the higher the curing temperature, the shorter the initial film forming time and the complete curing time of the blocked SFPU. From the five percentage closure gradients of 75%, 80%, 85%, 90%, 95%and100%, the mechanical properties of the membrane increased with the increase of the blocking ratio.

    • >Water treatment technology and environmental protection
    • Relationship between material and microstructure of filter cloth and water permeability

      2019, 36(6).

      Abstract (695) HTML (0) PDF 1.64 M (0) Comment (0) Favorites

      Abstract:The water permeability of the woven filter cloth directly affects the production efficiency of the filter equipment. In order to clarify the relationship between the material, microstructure and the water flux of the filter cloth, a dozen of woven filter cloth with control variables were customized for the research. FTIR, dynamic and static contact angles and surface energy measurements were measured on filter cloths of different materials, and the key indicators affecting the water flux were analyzed from the perspective of mechanism. The microstructure of the filter cloth was characterized by SEM, and the influence of weaving method, thickness and pore size on the water flux was analyzed, and a semi-empirical model between the microstructure of the filter cloth and the water flux was established. Results show that the hydrophilicity of the material is polypropylene>polycarbonate>polyamide, the corresponding water flux is 6.34, 5.75, 5.46 m/min, respectively. And hydrophilic materials have a larger water flux. The water flux under different weaving methods is the satin filter cloth>twill filter cloth>plain filter cloth, the factor of pore diameter and thickness are positively and negatively correlated with the through-water flux, respectively. The semi-empirical model between the fitted microstructure and the water flux can provide a theoretical reference for the selection of the woven filter cloth.

    • Functional preparation of Pectin-PDA Microsphere and Its Adsorption Properties for Th4

      2019, 36(6).

      Abstract (846) HTML (0) PDF 1.43 M (0) Comment (0) Favorites

      Abstract:Pectin-Ca microsphere was prepared by sol-gel method with Ca2 as cross-linking agent, and Functional pectin-PDA microsphere adsorbent was modified with dopamine-modified pectin microsphere. The adsorption performance of this adsorbent for removing Th4 was discussed. SEM, FTIR and XPS were used to analyze the preparation and adsorption mechanism.The results showed that the pectin-PDA microsphere had the best effect at pH=3.5. The adsorption capacity of adsorbent reached 37.172 mg/g under the conditions of 25℃, 20 mg/L mass concentration of Th4 , 0.03 g adsorbent, and 1200 min contact time. Co-existing ions Cs , Sr2 , Mn2 and Mg2 had little effect on the adsorption of Th4 . indicating that the adsorbent had better adsorption selectivity;The results of thermodynamics and kinetics showed that the adsorption process conformed to the Langmuir linearisotherm model and the pseudo-second-order kinetics model. The maximum adsorption capacity was 99.010 mg/g. The thermodynamic data showed that the adsorption of Th4 by pectin-PDA was a spontaneous absorption.The thermal stability of pectin-PDA was improved by TG analysis compared to that before modification. The mechanism of adsorption of Th4 by pectin-PDA microsphere was due to the sequestration of N and O on pectin-PDA and Th4 in solution.

    • Preparation of ZM-CSt-PVA composite gel though freezing cross-linking method and adsorption performance of Cu2+

      2019, 36(6).

      Abstract (1050) HTML (0) PDF 1.03 M (0) Comment (0) Favorites

      Abstract:Using zwitterionic monomer (ZM), cassava starch (CSt) and polyvinyl alcohol (PVA) as main raw materials,a ZM graft copolymerized CSt-PVA interpenetrating network composite gel (ZPG2) was prepared through a freezing cross-linking method with a one-pot process. ZPG2 was characterized by Fourier infrared spectrometer(FTIR), Thermogravimetric analyzer(TGA), Polarized light microscopy (POM), Scanning electron microscope and Energy dispersive spectrometer (SEM-EDS). Static adsorption effects of ZPG2 on Cu2+ was evaluated. The results showed that ZPG2 had good thermal stability below 300 ℃. The presence of ZM produced an anti-polyelectrolyte effect and a chemical coordination effect, which could increase gel adsorption capacity significantly. Saturated adsorption amount could be as much as 199 mg/g when adsorption temperature was 25℃, ZPG2 dosage was 0.1g, Cu2+ concentration was 2×103 mg/L, and the solution volume was 100mL. The data of adsorption was in accord with Langmuir isotherm adsorption model and pseudo-second-order kinetic model.

    • Synthesis and Adsorption Properties of Cu2+ Imprinted Crosslinked Chitosan Microspheres

      2019, 36(6):0-0.

      Abstract (742) HTML (0) PDF 1.77 M (0) Comment (0) Favorites

      Abstract:By using molecular imprinting techniques, the Cu2+ imprinted crosslinked chitosan microspheres were prepared by using chitosan as functional monomer, Cu2+ as template ions, solidified by dilute ammonia, epoxy chloropropane crosslinked, and eluted Cu2+ by hydrochloric acid. The products were characterized by fourier transform infrared spectroscopy、X-ray diffractometer and field emission scanning electron microscopy. The physical properties such as skeleton density, water content, crosslinking degree etc of Cu2+ imprinted crosslinked chitosan microspheres were measured. The results showed that crosslinking modification can make the microspheres have porous structure and good structural stability, it also solve the acid solubility of chitosan very well, and the adsorption properties of microspheres on Cu2+ were improved. Through the orthogonal test and used table L9(34), the optimum preparation conditions of Cu2+ imprinted crosslinked chitosan microspheres were as follows: the quality of chitosan was 1.5 g, the dosage of epoxy chloropropane was 2.5 mL, crosslinked temperature was 80℃, crosslinked time was 3 h, the best adsorption property of microspheres on Cu2+ was obtained. The adsorption properties of microspheres to Cu2+ were also studied in single component system. The results showed that when the mount of microspheres was 50 mg, the initial concentration of Cu2+ was 338.65 mg/L, the pH value was 5, the adsorption capacity of Cu2+ was 72.8 mg/g.

    • >Rubber and plastics auxiliaries
    • Preparation and properties of ZnO/MoO3/Al(OH)3 flame retardant polypropylene

      2019, 36(6).

      Abstract (570) HTML (0) PDF 5.63 M (0) Comment (0) Favorites

      Abstract:One-dimensional materials of ZnO and MoO3 nanowires (NWs) were prepared via hydrothermal method. The morphology and structure of nanowires were characterized by SEM and XRD. ZnO/MoO3/Al(OH)3/PP composites (NWs/ATH/PP) were prepared by melt blending one-dimensional nanowires and nano-aluminum hydroxide (ATH) with polypropylene (PP). The thermal stability and combustion properties of the composites were characterized by thermogravimetric analyzer (TGA), limiting oxygen index (LOI) analyzer and cone calorimeter (CCT). The mechanical properties of the composites were tested by universal testing machine. The results showed that when the adding amounts of ZnO nanowires, MoO3 nanowires and nano-ATH were 3.75%, 3.25% and 21% (mass fraction), respectively, the initial decomposition temperature of NWs/ATH/PP composites was 17.8 °C higher than that of pure PP, and the residual weight is 24.6%. And the peak heat release rate (PHRR) and total heat release (THR) were decreased by 54.3% and 25.7%, respectively, and the LOI was increased by 7.1%. The results of SEM analysis showed that the surface of carbon residue of NWs/ATH/PP was well improved, dense, continuous and flat.

    • Synthesis and Properties of Silicone Acrylate Modified Waterborne Polyurethane

      2019, 36(6).

      Abstract (820) HTML (0) PDF 2.41 M (0) Comment (0) Favorites

      Abstract:Waterborne polyurethane prepolymer (WPU), polyacrylate (PA), silicone modified waterborne polyurethane prepolymer (SiWPU) and polyacrylate (SiPA) were synthesized using isophorone diisocyanate (IPDI), γ-aminopropyltriethoxysilane (KH550), methyl methacrylate (MMA) and γ-(methacryloyloxy)propyltrimethoxysilane (KH570) as main raw materials. Then, silicone acrylate double modified waterborne polyurethane (SiWPUA) emulsions were synthesized by interpenetrating network polymerization using WPU, SiWPU and SiPA as raw materials. The effects of PA addition amount, SiPA addition amount and SiWPU addition amount on the water resistance of the emulsion films were investigated by measuring water absorption rate and water contact angle and the mechanism was analyzed. The results showed that the water absorption rate of SiWPU-40%-SiPA-37.5% (40% is the content of SiWPU based on the total mass of WPU and SiWPU, the same below, and 37.5% is the mass fraction of SiPA in the system) film was reduced from 37.4% before modification to 6.8%, the contact angle was increased from 56.8° to 86.4°, and pencil hardness was increased from HB to H. Thermogravimetric analysis demonstrated that the Tmax (the temperature at which the decomposition reaction occurs) of SiWPU-40%-SiPA-37.5% was 412.4℃, higher than that of WPU (340.2℃). TEM results revealed that the modified latex particles had a core-shell structure. SEM of film section and XRD results showed that both PA and silicone modification increased the crosslinking degree of the polymer.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Evaluation of PAAD-16 Acid Thickener

      2019, 36(6).

      Abstract (684) HTML (0) PDF 819.30 K (0) Comment (0) Favorites

      Abstract:A hydrophobic monomer was synthesized by using amino propyl intermediates dimethyl methyl acrylamide (DMAPMA) and 1-bromohexadecane. The new hydrophobically associating copolymer PAAD-16 has been prepared by aqueous solution polymerization , which can be used as an acid thicker and the monomers are acrylamide(AM), anionic monomer 2-acryamido-2-methylpropane sulfate acid (AMPS) and DHAB. And it had been characterized by means of IR, FL and SEM. Evaluated the performance of the PAAD-16, and the results show that the acid dissolving time of this thickener is about 90 min; the apparent viscosity of this viscous acid is 59mPa·s at 30 ℃ and 170 s-1; ω of this viscous acid was respectively 85.0% and 66.1% at 60 ℃ and 90 ℃. Under the conditions of 30 ℃, 170 s-1, ω' of this viscous acid is 81.4%, it has excellent viscosity increasing, temperature resistance, shear resistance and retarding performance. Key words: hydrophobic association; polymer; thickener;acid solution

    • >Fine chemical intermediates
    • Synthesis of the 1-Chloromethyl Sulfonamide Compounds

      2019, 36(6).

      Abstract (854) HTML (0) PDF 506.82 K (0) Comment (0) Favorites

      Abstract:Sulfonamide is a special type of compound known for its versatile biological activity. The synthesis of these compounds has attracted manyattention of pharmaceutical chemists and organic chemists. Sulfonylation was accomplished between chloromethanesulfonyl chloride and aromatic primary amine in the presence of pyridine in this article. The reaction conditions such as catalyst, solvent, molar ratio of the material and reaction temperature were investigated.The results indicated that the optimized reaction conditions were determined as follows: n (amine) : n (chloromethanesulfonyl chloride) = 1 :1.3, pyridine as catalyst, dichloromethane as solvent , reaction at 0 ℃ to room temperature for 4~8 h. Under the optimized reaction conditions, a series of chloromethyl sulfonamide was obtained in 42%~95% yields. The structure of newly synthesized compounds was determined by IR, 1HNMR and 13CNMR.