SIMA Li-feng , WANG Yue , LIN Yan , CHEN Li-gong , LI Yang
2011, 28(11).
Abstract:The synthesis of N-Hydroxyalkyl-4-piperidones was studied. N-Hydroxyalkyl-4-piperidones can be obtained from aminoalcohols and methyl acrylate through Michael reaction, followed by Dieckmann cyclization and decarboxylation in the yield of 21.9%~45.6%. The amount of sodium methoxide was investigated in the Dieckmann cyclization and the best result was received under the molar ratio 1:1.6 of diadduct to sodium methoxide. The by-products through aldol condensation and chloro substitution were separated and characterized in the process of synthesizing N-6’-hydroxyhexyl-4-piperidone.
2011, 28(11).
Abstract:Ethyl 4-bromo-4,4-dinitrobutyrate was synthesized by Michael addition reaction of bromodinitromethane potassium salt and ethyl acrylate, and the effects of the ratio of raw materials, reaction temperature and time on the reaction were studied. The optimum synthetic technology conditions with 52% yield are: molar ratio 2:1 of ethyl acrylate to bromodinitromethane potassium salt, reaction temperature 30 ℃, reaction time 30 min, TBAB as phase transfer catalyst. The quality of TATB is equivalent to 25% of bromodinitromethane potassium salt. The structure of the product ethyl 4-bromo-4, 4-dinitrobutanoate was identified by IR, NMR, UV-Vis, MS and elementl analysis.
CHEN Zhuo , LIU Xiu-mei , GAO Yu-rong , WANG Lin-lin , MA Ting-li
2011, 28(11).
Abstract:Six kinds of binary ionic liquid electrolytes were used for DSC and the photoelectric conversion efficiency (PCE) of the device varies from 1.39% to 4.98%. Among these ionic liquids, the electrolyte composed of 1-butyl-3-methylimidazolium iodide (BMII) and 1-ethyl-3-methylimidazolium tetrafluoroborate (EmimBF4) reached the highest efficiency. In order to optimize this binary ionic liquids electrolytes, Electrochemical impendence spectroscopy (EIS), UV-Vis spectroscopy, and photovoltaic performance of DSC based on BMII and EMIMBF4 with the different concentration of iodine were performed. The results showed that the Pt-electrolyte charge-transfer resistance (RPT) , the TiO2-electrolyte charge-transfer resistance (RcT)and Warburg impedance (Zw) decreased with the iodine concentration increasing, however, the absorption intensity of the electrolytes increased. When the concentration of iodine was 0.25 mol/L, the highest PCE of 5.20% was obtained for the DSC based on the binary BMII/EMIMBF4 ionic liquid electrolyte under AM1.5.
2011, 28(11).
Abstract:Sulphonated waterborne polyurethane (SWPU) emulsions were synthesized by the reaction of polyethylene glycol adipate diol (PBA) and isophorone diisocyanate(IPDI) , hexamethylene diisocyanate (HDI), and N-(2-aminoethyl)-amino ethane sulphonated sodium was used as hydrophilic chain extender. The influences of the feeding methods and chain extension time of AAS on performance of SWPU were investigated by using FT-IR, TEM, XRD and so on. The results showed that when the one-time feeding mode of AAS was applied and the chain extension time was 25min, SWPU with 50% solid content was obtained, and the particles of SWPU were spherical shapes, the average particle size, viscosity and hardness were appropriate, and two sharp diffraction peaks at 2θ=21.30?and 22.34?in XRD indicated the crystallization of the synthesized sulphonated waterborne polyurethane films.
Zhang Ming-yue , Zhang Xiao-liang , Chen Guang-mei , Huang Yi-ping , Wu Li-xia
2011, 28(11).
Abstract:A series of FPUA hybrid emulsions with core-shell structure were synthesized by methyl methylacrylate (MMA), butyl acrylate (BA) and dodecafluoroheptyl methacrylate (G04), with the double-bond caped polyurethane as reactable macromolecule and potassium nonafluoro-1-butanesulfonate as fluorinated emulsifier. The structure of copolymer was characterized through Fourier transform infrared spectrometer (FT-IR) and and the particle morphology of hybrid emulsion latex was observed by transmission electron microscopy (TEM). Contact angles, tensile test and thermogravimetry (TG) were taken on the film to research water resistance, mechanical and thermo properties of the resins modified by acrylate and fluorinated acrylate. The results stated, when the mass fraction of fluorinated emulsifier and fluorinated monomer were 0.15% and 20% mass of all monomers respectively, the FPUA emulsion showed good stability. Surface energy of the sample declined from 45.6dyn/cm to 22.5dyn/cm and the copolymer showed excellent refusal of water and oil. The temperatures of rapidest mass loss increased from 348℃ to 398℃.
FANG Xiao-min , HU Yong-jia , ZHANG Pu , XU Yuan-qing , DING Tao , REN Yan-rong
2011, 28(11).
Abstract:A PEPA-containing benzoxazine (PEPA-Bz) was synthesized from phenol, aniline and PEPA derivative. The structure of target compound was confirmed by fourier transform infrared spectroscopy (FT-IR) and 1H nuclear magnetic resonance spectroscopy (1H NMR). And the properties of its homopolymer and its copolymer with bisphenol-based benzoxazine(Ba) were investigated. Thermal gravimetric analysis (TGA) showed that PEPA-containing polybenzoxazine has good thermal stability and char formation. The temperature at 5% weight loss is 235℃, the char yield ratio is 53% at 700℃and the LOI is 38.7. FT-IR and TGA were utilized to investigate the ring-opening copolymerization behavior of PEPA-Bz and Ba and their thermal properties, respectively. The results shows that the Flame retardant properties and char yield of the copolymer were both better than the homopolymer of Ba.
2011, 28(11).
Abstract:Spinel LiMn2O4 was synthesized via solid state process with different raw materials. The phase identification, surface morphology and electrochemical properties of the synthesized powders were characterized with x-ray diffraction, scanning electron micrograph, cyclic voltammetry and galvanostatic charge-discharge experiments. LiMn2O4 powders prepared by Mn3O4 shows better crystallization than the one prepared by electrolytic MnO2(EMD). The specific capacity of LiMn2O4 prepared by Mn3O4 is 128.7mAh/g, which is slightly higher than that of 123.7mAh/g for LiMn2O4 prepared by electrolytic MnO2. The capacity retention of the LiMn2O4 prepared by Mn3O4 after being cycled 30 times at room temperature and room temperature of 55℃ is 98.4% and 85.0% respectively, which are much higher than the values of 91.03% and 80.3% for the one prepared by electrolytic MnO2. Preparation of LiMn2O4 by Mn3O4 can not only improve the specific capacity but also significantly increase the cycle performance and high temperature performance.
WANG Ai-qin , CHEN Wen-juan , HUANG Da-jian
2011, 28(11).
Abstract:Aattapulgite (APT) was treated by 1% (v/v) HCl, H2SO4, H3PO4, HClO4 and H4P2O7 solution at a ratio of solid to liquid of 1:10. Poly(vinyl alcohol) / attapulgite (PVA/APT) nanocomposite films with different acids treated APT were prepared using film-casting method. The microstructures of the nanocomposite films were investigated using FTIR, SEM and XRD. The mechanical properties and water-resistance of the nanocomposite films were also tested. The experimental results indicate that the acid treated way can increase the dispersing capability of APT by dissolving the impurities and carbonate in the pore canal, and then APT can be dispersed better in PVA matrix,thus mechanical properties and water-resistance of the nanocomposite films have been significantly improved. Compare to nature APT, when adding APT treated with 1% (v/v) HClO4, the nanocomposite film has optimum performances, and the tensile strength, elongation at break and water resistance of the nanocomposite films have an increase of 29.3%, 74.9% and 32.2%, respectively.
ZHANGYan , ZHONG Guo-qing , XIONG Xin , JIANG Qi-ying
2011, 28(11).
Abstract:Zinc(II) and copper(II) complexes of o-phthalic acid (H2phth) were synthesized by microwave solid-state method with o-phthalic acid, zinc acetate or copper acetate as raw materials. Chemical and element analysis, FT-IR, X-ray powder diffraction and TG-DTG analysis were applied to characterize the composition and structure of the compounds. The results show that the compositions of the complexes are Zn(phth)?2H2O and Cu(phth)?H2O, the ligand is coordinated simultaneity with Zn(II) or Cu(II) via the carboxyl group of o-phthalic acid to form bidentate chelates. Thermal decomposition processes of the complexes include dehydration, oxidation and pyrolysis of the ligand, and finally as metallic oxide.
2011, 28(11).
Abstract:The effects of impurities ions Al3+,Fe3+,F-,Mg2+ and SO42 - on the crystallization yield of urea phosphate(UP),its crystallization period, product size and crystal morphology were studied by means of batch crystallization process.The results showed that the dopant of Al3+,Fe3+ had siginificate effect on UP crystallization process,and without the crystal seed added in the reaction system, no crystals appeared when the system was cooled to normal temperature.On the conditions of 1% crystal seed added,with the increase of Al3+,Fe3+ mass fraction, the yield of UP gradually decreased,the crystallization period significantly prolonged, the product size was obviously reduced and the crystal morphology become irregular.Moreover, the aggregation degree was higher. The effect of Al3+ was somewhat larger than that of Fe3+ on above many aspects. With the increase of F- mass fraction,the yield of UP gradually decreased,the crystallization period did not change significantly,the product size decreased firstly and then increased slowly because of the embedding of the particle with each other and the crystal morphology become irregular.The impurity ions Mg2+and SO42 - had very little influence on the UP crystallization process,and the crystal morphology is regular and still is prism,the particles are in high dispersion state.
2011, 28(11).
Abstract:In this paper, lactose,ethylene glycol,higher alcohol are used as the raw materail,adopting trans-glycosylation to synthetize lactose-based glycoside surfactant,regarding yield of the product as the target, the optimum conditions of synthesizing lactose-based glycosides were investigated by orthogonal and single factor experiments as follow: reaction temperature 110℃, reaction time 4h, lactose:PTSA: DBSA:ethylene glycol:higher alcohol=1:0.013:0.02:4.9:1.2(mass ratios).The yield is 129.7%,the conversion rate of lactose is 98.37%.The properties of product have been characterized by FT-IR,GC-MS, surface tension and so on.The result shows that the lactose is able to synthetize glycoside surfactant.
LIU Hai-di , YUE Ren-liang , ZHANG Jing-kun , WU Zhen-jiang , CHEN Yun-fa
2011, 28(11).
Abstract:Abstract:Sustained-release antibacterial organic/inorganic composite material was prepared with TEOS,trichlosan and γ-aminopropyl triethoxy silane (KH-550). Low-temperature N2 adsorption, SEM and FTIR methods were employed to investigate the BET specific surface area, particle morphology and functional group on the sample surface, Sustained-release ability of the as-made samples was investigated with dissolving experiment on rotary shaker. Bacteriostasis circle experiments were conducted to assess the dissolving antibacterial performance of the samples. It was revealed by the results that organic/inorganic composite antibacterial material with good sustained-release ability could be successfully prepared, and the sustained-release ability could be improved by coupling agent (KH-550).
2011, 28(11).
Abstract:p-Chlorobenzoyl isothiocyanate was obtained via the reaction of p-chlorobenzoyl chloride with potassium isothiocyanate. Seven p-chlorobenzoyl substituted benzoyl thiosemicarbazides, including N-p-chlorobenzoyl-N’-benzoyl thiosemicarbazide(Ⅱ1), N-p-chlorobenzoyl-N’-p-hydroxybenzoyl thiosemicarbazide(Ⅱ2), N-p-chlorobenzoyl-N’-p-nitrobenzoyl thiosemicarbazide(Ⅱ3), N-p-chlorobenzoyl- N’-o-methoxybenzoyl thiosemicarbazide(Ⅱ4), N-p-chlorobenzoyl-N’-p-chlorobenzoyl thiosemicarbazide (Ⅱ5), N-p-chlorobenzoyl-N’-α-naphthalene acyl thiosemicarbazide(Ⅱ6) and N-p-chlorobenzoyl-N’-p- methylbenzoyl thiosemicarbazide(Ⅱ7), were synthesized by addition reaction of p-chlorobenzoyl isothiocyanates with aroyl hydrazines, in the yield of 79.8%%, 84.8%, 65.6%, 64.6%, 88.8%, 72.2% and 82.6% respectively. The structures of the products were characterized by 1H NMR, IR and elemental analysis. The preliminary biological activity test indicated that the synthesized compounds had antibacterial activity against B. subtilis, but had no obvious inhibition activity against E. coli.
WANG Jing-xia , PENG Chao-rong
2011, 28(11).
Abstract:For improving the hydrophilicity and cell compatibility of PLA, electron beam was used to induce grafting of NVP on PLA in different conditions (irradiation dose, ethylic acid concentration). PLA-g-PVP copolymers with different graft ratio were attained. The degradation behaviors of the materials were investigated by mass loss, molecule weight loss and water intake measurement. The experimental results showed that the hydrophilicity and degradation rate of the grafted materials were improved with the increase of the graft ratio. Compared with PLA, the PLA-g-PVP copolymers showed higher hydrophilicity and faster degradation rate due to the incorporation of hydrophilic PVP units. These PLA-g-PVP copolymers can be expected to apply in tissue engineering for their great potentials in having good cell affinity to be cell scaffold materials.
2011, 28(11).
Abstract:The temperature-responsive silica core-poly(N-isopropylacrylamide) shell (SiO2/PNIPAm) hybrid microspheres were prepared by grafting PNIPAm chains to SiO2 nanoparticles via the combination of reversible addition - fragmentation chain transfer (RAFT) and thiol-ene click chemistry. The SiO2/PNIPAm hybrid microspheres were characterized by FTIR, thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and dynamic laser scattering (DLS). Nearly monodispersed SiO2/PNIPAm hybrid microspheres of 286 nm in average diameters were obtained. The grafting yield and grafting density of PNIPAm brushes on the SiO2 nanoparticles was about 87% and 0.40 chains/nm2. The temperature-responsive of SiO2/PNIPAm hybrid microspheres were investigated by DLS. The hydrodynamic diameters (Dh) of SiO2/PNIPAm hybrid microspheres decreased from about 286 nm to about 268 nm as the temperature of the aqueous medium increased from 25 to 35 oC, the PNIPAm shell thicknesses decreased from about 16 nm to about 7 nm.
LI Cheng-cheng , JIANG Ping-ping
2011, 28(11).
Abstract:Di(2-ethylhexyl) 1,2-cyclohexane dicarboxylate(DEHCH) was synthesized by reaction of HHPA with iso-octanol using active carbon supported methanesulfonic acid as catalyst. The optimal reaction conditions are as follows: n(iso-octano):n(HHPA)= 2.4: 1.0, catalyst (2.1% of mass of HHPA and iso-octano), water entrainer cyclohexane 6 mL, reaction temperature 160 ℃~180 ℃, reaction time 2.5 h. The esterification yield is 99.82%. The catalyst was repeatedly used 4 times and esterification rate was still more than 90%. The product is light yellow transparent oily liquid and the content of DEHCH ranges up to 99.15% by means of HPLC test. The acid value,density,heat weight loss,viscosity and TG curve of product were respectively measured.In conclusion,DEHCH can satisfy the requirements of plasticizer.
TANG Shi-fu , JIANG Guo-qiang , Yu yang , Ding Fu-xin
2011, 28(11).
Abstract:Bile acid transporter, which is aboundent on the hepatic cell surface, provides a promising way accessing the hepatic cell targeted drug delivery. In the present study, poly-[3 alpha-(4-vinylbenzonate)-7 alpha,12 alpha-dihydroxy-5 beta-cholan-24-oic acid] (PVBCA), a amphiphilic polymer with bile acid structure in the side-chain, was designed and synthesized. PVBCA coated PLGA nanoparticles with the diameter of 350nm were prepared by emulsion-solvent evaporation method and PVBCA assembled on the nanoparticle surface due to its amphiphilicity. The specific interactions between PVBCA and hepatic cells, as well as the uptake of the PVBCA coated PLGA nanoparticles were evaluated by SMMC-7721 cells in vitro, with fluorescent probe coumarin 6 employed as the model drug. The results showed the cells absorbed on the PVBCA film were more than the twice of those absorbed on the polystyrene surface of culture dash. In comparison with the delivery by unmodified nanoparticles, the intracellular concentration of coumarin 6 was increased by more than 8 times with the vehicle of PVBCA coated nanoparticle. In conclusion, PVBCA, as the nanopartice-coating polymer, exhibited significant potential in liver-targeted drug delivery.
2011, 28(11).
Abstract:Zirconia coatings(ZrO2)were deposited on silicon carbide (SiC) fibers with sol-gel method. The influence of precursor zirconium sol and sintering temperature on ZrO2 coatings was studied in this paper. The phase and morphology of ZrO2 coatings were evaluated by X-ray diffraction (XRD) and scanning electron microscope (SEM). The results showed that the desired ZrO2 coatings were fabricated through dipping out SiC fibers with the precursor of concentration of Zr4 cation 1.0mol/L, polyvinyl alcohol (PVA) 30wt.% and then heated at 1000℃ for 60min.
CHEN De-li , XIAO Man , LIU Ping-huai
2011, 28(11).
Abstract:The dry stems and leaves of Drypetes hainanensis were extracted with ethnol, then the total extracts were respectively extracted with petroleum ether, ethyl acetate and n-butanol. Whereafter, the antioxidant activities of the total extracts with ethnol and all the other extractions were investigated with DPPH and FRAP assay. The results displayed that the IC50 of extracts of D.hainanensis (DH), extracts of petroleum ether (DHMSO), extracts of ethyl acetate (DHEtOAC), extracts of n-butanol (DHNBA), extracts of water (DHH2O) were 77.3, 115.2, 51.4, 342.9, and 205.7 μg/mL, respectively, with DPPH method, and their FRAP values were 11712.2±931.8, 10820.9±690.5, 14386.4±568.8, 1157.6±63.3, 5584.1±182.3 μmol Fe2+/g, respectively, as well. The IC50 of ascorbic acid (Vc) and BHT are respectively 10.7 and 47.1 μg/mL, and their FRAP values are 18022.8±63.3 and 14568.7±137.0 μmol Fe2+/g, respectively. In addition, multi-cluster showed that DH, DHMSO, DHEtOAC, BHT and Vc had a similar intensity of antioxidant activity, therefore, they could be classified into the same type material. Also, it was found that the antioxidant activity of DHEtOAC could be comparable with BHT, accordingly, the crude extracts had strong antioxidant activity. So in those domains of pharmaceutical, health care, cosmetics and so on forth, D.hainanensis has wide-ranging research and application prospects.
SHI Jiao-xue , ZHANG Wen , LAN Yun-jun , GAO Xiu-yun , ZOU Xiang-long
2011, 28(11).
Abstract:Series styrene-alt-maleic anhydride (SMA) copolymer with different molecular weight were prepared by solution polymerization, the structure of which were characterized by FTIR, 1H-NMR, 13C-NMR. And its thermal property was analyzed by DSC. The effects of molecular weight of SMA to its retanning-filling properties in leather was studied. The results show that the molecular weight of copolymer is an important factor to affect the retanning-filling properties. With the molecular weight increasing, the tear strength and reduction rare of location difference of leather are increasing, while the tensile strength decreasing. When the Mn of SMA is 6620, the tensile strength, tear strength and reduction rare of location difference are 18.325 N/mm, 9.519 N/mm2 and 7.44%; When the Mn is 59058, the tensile strength, tear strength and reduction rare of location difference are 20.577N/mm, 5.539 N/mm2 and 44.98%.
2011, 28(11).
Abstract:With methylene dichloride and diethyl ether being the solvent separately, and with low temperature water bath condensation utilized on simultaneous distillation and solvent extraction (SDE), volatiles of the dry leaves of Taxus chinensis var mairei were extracted and then analyzed on a polar column of DB-WAX by GC/MS. Sixty-three compounds were identified, among which the aliphatic class (60.44%) was the most abundant followed by the aromatic (6.56%), whereas the class of terpenoid was rather less (4.57%). Based on average result by the two extraction solvents, hexadecanoic acid (21.19%), tetradecanoic acid (8.87%), and ethyl linolenate (3.49 %) belonged to the majors. In contrast with what had been reported previously on volatile composition of Taxus chinensis var maire, 34 trace components of low boiling point e.g. hexanal, 2-hexenal, 1-octen-3-ol, 2, 4-heptadienal, benzaldehyde, benzyl alcohol, and acetophenone, which have green, floral, and fruity aroma, should be new identifications. Finally, with 1, 2-dichlorobenzene as internal standard, each compound identified was quantified; the total content of them turned out to be 88.16 礸/g of dry leaves.
2011, 28(11).
Abstract:The foaming properties of Di-n-alkyl disulfate surfactants in aqueous solution were measured by the Foamscan, and the effect of different additives such as sodium chloride and polymers were investigated. Results show that these surfactants have excellent foam properties. Foam stability decreased significantly with the increase of spacer length. With temperature rising, half foam life period decreased remarkably. The electrolyte deduced the foaming volume, while the foam stability increased firstly with the increase of sodium chloride concentration to a certain extent and then dropped. The polymer can enhance foam stability.
2011, 28(11).
Abstract:Abstract: The Supercritical carbon dioxide fluid extraction (SFE) technique was applied to extract the oil of Xinjiang Nigella Sativa L seeds. First we have optimized the SFE extraction conditions by using single-factor and orthogonal testing methods. Second we have determined the fatty acid components in the oil that was extracted by SFE using GC-MS. the results showed that the optimized conditions for the SFE of oil from Xinjiang Nigella Sativa L seeds were as follows: extraction press20MPa, extraction temperature 35℃, extraction time 1.5 h ,CO2 fellow 25kg/h. Under these conditions, extraction yield could up to36.12%. the results of GC-MS analysis shows that the main contents of them are unsaturated fatty acids, in which the relative content of 9,12-Octadecadienoic acid was 60.95%, 9-Octadecenoic acid was 20.54%,eicosenoic acid was 2.43%, the total content of unsaturated fatty acids were 84%。SFE are can selective extraction unsaturated fatty acid which in the Nigella Sativa L seeds,It is worth popularizing and promising extraction and separation technology.
2011, 28(11):0-0.
Abstract:The rheological behavior of cationic gemini surfactant (C18-4-C18•2Br) solution and the influencing factors, such as, surfactant concentration, sodium salicylate concentration and temperature, were investigated. The viscosity of gemini surfactant solution increases with the increase of surfactant concentration. Both the viscosity and the viscoelasticity of gemini surfactant solution undergoes a maximum with the addition of sodium salicylate. Temperature has a great effect on the viscosity of gemini surfactant solution. The addition of sodium salicylate can enhance the resistance performance of gemini surfactant solution to the temperature. TEM experiments show that appropriate amount of sodium salicylate adding in the gemini surfactant solution can lead to the transition of surfactant micelles from spherical micelles to wormlike micelles, however, overmuch addition of sodium salicylate will bring about the formation of vesicles in the gemini surfactant solution.