ZHANG Tai-liang , LIU Wan-qin , LI Liang
2014, 31(10).
Abstract:A novel copolymer was synthesized using acrylamide(AM),sodium allylsulfonate (SAS),sodium p-Styrene sulfonate (SSS) and Acrylic polyethers(APEG), it could be used as an anti-temperatureand and salt-tolerant fluid loss additive. We obtained the optimal reaction conditions, which is, m(AM):m(APEG):m(SSS):m(SAS)= 6.5:2.0:0.5:1.0, monomer concentration is 20%, dosage of initiator is 0.2%, temperature of reaction is 60℃. Meanwile, the structure of this polymer was confirmed through FTIR, the result show that the molecular sturcture of the artificial synthesis product is in accord with the ideal one. The thermogravimetric experiment indicates good therm stability of this polymer. Compared the morphology of filter cake by SEM, it could forn a thin and dense filter cake by the fluid loss agent .Moreover, the fluid loss additive had reveal good temperature resistance and salt tolerance.
2014, 31(10).
Abstract:Abstract: LiMn2O4 were prepared by CMD and pretreated CMD. The structure and morphology of different LiMn2O4 were studied through XRD and SEM.Electrochemical properties were investigated through Charge-discharge testing.The result shows that all of LiMn2O4 have regular spinel structures. LiMn2O4 synthesized by CMD pretreated at 800℃ has the most stable crystal structure and uniform particle size, which shows the best electrochemical performance. The first discharge capacity is 118.4mAh/g,and the capacity retention is 92.74% after 100 cycles. Key words:CMD; pretreatment; LiMn2O4;electrochemical properties
2014, 31(10).
Abstract:Silicone with functional amino group was synthesized by several silicone monomers though hydrolysis and condensation. Different content of silicones modified epoxy resin was prepared though curing reaction of silicone and epoxy resin and curing agent. The influences of different silicone content on the properties of the modified epoxy resin were investigated. The results indicated that: with 30% addition, the tensile strength was 68.27MPa, bending strength was 81.68MPa, 800 oC residues was 26.45%, contact angle was 109.3°, 24h water absorption was 2.59%, which was 17.24%, 6.6%, 17.3%, 21.3% much higher and 0.12% lower than the original resin.
2014, 31(10).
Abstract:Abstract: Five organic dyes of D-x series were synthesized which contained triphenylamine (TPA) moieties as electron donors and cyanoacrylic acid moieties as electron acceptors, alkyl thiophene (alkyl chain were H、CH3、C4H9、C6H13、C8H17 respectively )as π-conjugated linker. The effects of both the alkyl chains and the length of the alkyl chains on the photo-physical, electrochemical and photovoltaic properties of the dyes were studied. The results indicated that D-2~D-5 dyes with alkyl chains the UV-Vis absorption spectra were occurred blue shift; With prolonging alkyl chains, the short-circuit photocurrent density (Jsc) decreased gradually, while open-circuit photovoltage(Voc) and fill factor (FF) were improved. The results of photovoltaic performance indicated that PCE of D-2 with methyl substituent (5.64%) is slightly higher than that of other dyes.
XIE Zhong-wei , LIU Si-si , XIAO Wen-de , YAN Jian-min
2014, 31(10).
Abstract:In this paper, the homogeneous products by silane pyrolysis in a vertical tube reactor were obtained under different operating conditions. The characterization techniques of FT-IR and SEM were applied to investigate the morphology, particle size distribution and components of the products. The effects of the operating conditions including the operating temperature, total gas flux and inlet silane concentration on the properties of the amorphous silicon products were studied. The content of hydrogen was especially analyzed by infrared diffuse reflection, which allows quantization of the special absorption peaks in SiH2 and SiH structures and helps with a further understanding on the mechanism of silane homogeneous pyrolysis by the structure form of the amorphous silicon. The results reveals that the product shows larger particle size under higher operating temperature(550℃), lower gas velocity(600mL/min) and higher silane concentration(5%). And higher operating temperature also results in wider range of particle size distribution. Besides, the Si-H structure is mostly affected by temperature and least by silane concentration.
2014, 31(10).
Abstract:A facile microporous polypropylene membrane (MPPM) surface modification method was developed with controllable grafting density and distribution of amino groups in this paper. Firstly, polymethyl acrylate (PMA) was grafted on the MPPM surface via UV graft polymerization. Then, the grafted membrane was alternately performed the amidation condensation and Michael addition reaction with ethylenediamine and methyl acrylate as the raw reactants for several times. The aminated membranes were characterized by Fourier transform infrared spectroscopy (FTIR), x-ray photoelectron spectroscopy (XPS) and environmental scanning electron microscopy (ESEM). The aminated membranes show greatly enhanced surface hydrophilicity and can adsorb water up to 1311.29±97.56 μg/cm2, which is 145 times as much as that of the origin membrane. Furthermore, the aminated membranes have satisfactory performance for water flux and metal ions permeability.
EN Da , SUN Xiao-hong , YAN Yong
2014, 31(10):0-0.
Abstract:Coumarin derivatives with imino groups were synthesized by using 8-formyl-7-hydroxylcoumarin-3-carboxylic acid ethyl ester and 2-aminophenol as raw materials, then the coumarin- copper ions coordination compounds fluorescent probe was made after the complexation of the derivatives and copper ions. In 50% ethanol aqueous solution, this probe shows a good selectivity to the kind of amino acid with thiols. The measurement mechanism of determination was explored by studied the fluorescence spectrum. During the recognizing of the probe, its fluorescence intensity whose visual colour was changed from green to blue, becomes more and more stronger. Thus, the visual detection was achieved by this method.
2014, 31(10).
Abstract:polyether modified silicone oil (PESO) was hydrosilylated from hydrogen content silicone(PHMS)and allyl polyether(APE)in the presence of Pt catalyst, the structure of the product was investigated by IR. Polyether modified silicone oil, self-made silicone paste and liquid paraffin as the raw material, together with the compound emulsifier S and other additives, polyether organosilicone defoamer was successively prepared with mechanical emulsification. The results showed that the defoamer was compounded in the conditions of emulsification temperature 70℃ and emulsification time 40min was characterized by better water-solubility, speedy defoaming ability and long-term inhabitation of foam, XP defoaming time is 5s, and the time of foam inhibiting performing is 60min. And the XP defoaming time is about 6s, the time of foam inhibiting performing is about 50min in constant of high temperature of 100℃ and strong alkali of pH 14.
2014, 31(10).
Abstract:Abstract: M-MCM-41 mesoporous molecular sieve with different metal doping(M=Ce、Y、Nd) was synthesized by hydrothermal method.The surface acidity, mesoporous structure, and chemical state of metal were characterized by X-ray diffraction(XRD), NH3 temperature programmed desorption (NH3-TPD), transmission electron microscopy(TEM), X-ray photoelectron spectroscopy(XPS) and N2 adsorption-desorption. The results indicated that M-MCM-41 mesoporous molecular sieve exhibited the typical hexagonal mesoporous structure, the Specific surface area and pore volume decrease with average pore diameter increasing, The metal element introduced to the molecular sieve was M3 valence state. The M-MCM-41 produced acid with metal doping and corresponding medium strong acid.
GAO Ting-ting , LIU Yu-ping , SUN Bao-guo
2014, 31(10).
Abstract:The volatile components in Durian pulp were extracted by two different kinds of solid-phase microextraction and analyzed by GC-MS in order to investigate those volatile compounds. These compounds were determined by MS and RI qualitative analysis. A total of sixty volatile constituents were identified, including 26 esters, 12 sulfur-containing compounds, 7 alcohols, 7 hydrocarbons, 5 aldehydes, 2 acids, 2 nitrogen-containing compounds and 1 phenol. The relative contents were determined by peak area normalization method. The major volatile components were ethyl 2-methylbutyrate, ethyl propionate, 1-tetradecanol, ethyl acetate, ethyl butyrate, ethyl E-2-butenoate, diethyl disulfide, propyl 2-methylbutanoate, tetradecanal and ethanethiol. Based on the odor characteristics of those identified compounds, it can be concluded that the odor of Durian pulp is mainly from ester compounds and sulfur-containing compounds. Most of ester compounds are fatty acid ethyl esters; the contents of mercaptan and sulfide are higher in the identified sulfur-containing compounds.
ZHANG Yue-qi , ZHANG Hui-ying , CHEN Hai-tao , SUN Bao-guo , ZHANG Yu-yu
2014, 31(10).
Abstract:The volatile flavor components in Yu-Shiang Shredded Pork were extracted by solid-phase micro extraction (SPME) or simultaneous distillation extraction (SDE) and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 93 volatile compounds were identified in Yu-Shiang Shredded Pork, Including 20 hydrocarbons, 20 aldehydes, 7 ketones, 2 acids, 9 esters, 16 alcohols, 2 ethers, 5 phenols, 12 sulfur-containing compounds or nitrogen-containing compounds or heterocyclic compounds. Aldehydes, esters, sulfur-containing compounds,nitrogen-containing compounds,and heterocyclic compounds may have an important influence on the formation of fish flavor.
2014, 31(10).
Abstract:An intermediate, 1-(4’-methoxyethoxyl phenyl) piperazine (Ⅲ), was synthesized from 1-(4’-hydroxylphenyl)-piperazinyl ethanone (Ⅰ) via etherification and hydrolysis. Another intermediate (Ⅶ) with a nitrogen condensed ring was prepared from methyl furan-2-carboxylate (Ⅳ) by acylation, ring-closure and halogenation. Finally, Preladenant was prepared from the both intermediates by condensation reaction. FT-IR, 1HNMR and ESI-MS were employed to characterize these intermediates and the aim compound. Through common synthetic method, the yields of these 6 steps are 99.0%, 95.4%, 98.0%, 78.9%, 86.9%(calculated by Cl) and 52.5% , respectively. To obtain higher total yield, ultrasonic was used in the last condensation reaction. The results showed that the condensation yield reached 85.4% when the reaction conditions were as follows the ultrasonic power (150W), the molar ration of intermediate 2 to 5 (1.2 : 1), soluent (DMSO), acid-bonding agent (Na2CO3), reaction temperature (90 ℃) and reaction time (1.5 h). The yield of the condensation is greatly increased by ultrasonic method.
ZHANG Teng , ZHANG Zhongqi , WANG Hui , JING Shan-gang , HAN Bin , FENG Ling-yun , YANG Xiao-lin , LIU Jian-li
2014, 31(10).
Abstract:Exenatide, an analogue of glucagons-like peptide 1 (GLP-1), consists of 39 amino-acid residues and adjusts blood glucose level through bidirectional hormone-targeted regulation. However, there are still many challenges about its synthetic methods. Herein, we split Exenatide into six fully protected peptide fragments and each fragment was synthesized by the solid-phase or liquid-phase method, respectively. After two-step cleavages and purifications, the final products 0.98 g (yield: 33.8%, Purity﹥98%) is obtained. The Fmoc- protective group attached to the Exenatide after the first step cleavage can enhance the separation of target and impurity efficiently in purification step. The results show that, with the advantages of both solid-phase and liquid-phase method, is an short-cycled, more convenient method and the yield is higher.
LIU Wei-wei , ZHANG Qiang , CHENG Feng-chang , LI Qu-xiang , HUO Yun-feng
2014, 31(10).
Abstract:Kinds of 1,4 - disubstituted D-Glucosamine urea derivatives were synthesized from 1,3,4,6-tetra-O-benzyl-β-D-glucosamine hydrochloride, solid phosgene and hydrazine to demand for new compounds containing semicarbazide glucosamine molecule fragments. The method used in the experiments have characteristics of mild conditions, short reaction time, simple operation, easy post-processing, high yield and so on. For the synthesis of varieties of the representative target products, the method had good adaptability. Used acetyl hydrazide as the model to sort out the experimental conditions. The optimum conditions obtained by optimization of experimental conditions. The target products were synthesized in high yield with low toxicity and available materials. A convenient method was provided for the synthesis of urea derivatives containing glucosamine molecule fragment. The structure of target products were confirmed by IR spectroscopy, 1HNMR and ESI-MS spectra.
Li Cui-juan , Zhao Chuan-sheng , Zhang Bing-bin , Le Zhi-ping
2014, 31(10):0-0.
Abstract:By analyzing the structure-activity relationship of alogliptin with DPP-Ⅳ, We used the strategy of skeleton transition and functional groups swap to design and synthesize 15 multi-substituted pyridone compounds. And we determined their structures of all compounds by 1H NMR and ESI-Mass and got three compounds 11a, 38, 41 which had quite activity with alogliptin through preliminary activity screening in vitro, initially identified the structure-activity relationships of these compounds with DPP-Ⅳ.
LEI Hong , CHEN Peng , XIA Li-ying , HUO Ji-chuan , GUO Jiong , LI Jun
2014, 31(10).
Abstract:The present work studied the hydrolysis of pea starch by isoamylase, and the hydrolyzed product was applied in glass fibre sizing. Results indicated that the isoamylase hydrolyzed pea starch by pitting and splitting. The aggregation behavior of the starch particles was affected by hydrolysis, which was manifested in the fluctuation of particle size, XRD intensity and viscosity. When the hydrolysis temperature was 50 oC, the surface tension of the hydrolyzed starch suspension could be reduced to 40 mN/m, which is close to the critical surface tension of glass fibre (30 mN/m). By breaking the starch granules with isoamylase, more hydroxyl groups of the starch molecules would be exposed. Therefore, the hydrolyzed product could easily spread over the surface of glass fibre, and conglutinated to glass surface firmly. Using the hydrolyzed product as sizing agent, the glass fibre-forming process was accomplished smoothly. Uniform protective film formed on the surface of glass fibre. The average breaking force of the 68 tex glass fibre was 25.0 N.
ZHONG Shang-fu , ZHU Yan-an , QU Jin-qing
2014, 31(10):0-0.
Abstract:The polyacrylate emulsion (PA) were synthesized by seeded semi-continuous emulsion polymerizations,which used as a coalescent of the hard resin latexes to replace small organic molecules, to prepare ultra-low volatile organic compound (VOC) contents waterborne wood coatings. Effects of Tg of PA, proportions and dosages of emulsifiers, and amounts of MAA on emulsion polymerization stability, properties and assistant-film-forming performance of PA were studied. It was found that the assistant-film-forming ability of PA was obvious increased with decreasing of polymer Tg from 0℃ to -20℃; and the gel contents of PA reduced from 0.83% to 0.10% with increasing of the reactive emulsifier contents; the PA average particle sizes could be reduced to 69nm with increasing of emulsifier dosage up to 2.1% and the assistant-film-forming ability of PA was enhanced as well; The total VOC content waterborne wood coatings formulated by PA with 4.5% MAA dosage was low to 33 g/L.
2014, 31(10).
Abstract:A novel organic dye with fluorenone as ?-conjugation bridge was designed and synthesized as sensitizers for dye sensitized solar cells (DSSCs). The dye was characterized by mass spectrometry (MS), proton nuclear magnetic resonance spectrometry (1H–NMR), and carbon nuclear magnetic resonance spectrometry (13C–NMR). The photophysical and electrochemical properties of the dye were studied. The dye achieved a light to electricity conversion efficiency (η) of 2.51% (open-circuit photovoltage Voc = 0.73 V, short-circuit photocurrent density Jsc = 4.46 mA/cm2 and fill factor FF= 0.77) under 100 mW/cm2 (AM 1.5G).
2014, 31(10).
Abstract:Four kinds of diallylmethylalkyl(C12,C14,C16,C18) ammonium bromide were synthesized by using diallylmethylamine and 1-bromoalkane straight chain alkanes as raw materials.The effects of reaction temperature, reaction time, molar ratio of raw materials and solvents type on product yields were discussed.The synthesis conditions were optimized. Structures of the products were characterized by IR, 1HNMR and 13CNMR.The results showed that solvent of ethanol was appropriate, the better reaction temperature was 60-65℃, reaction time was 72-78h and molar ratio of DAM to bromoalkane was 1:1.1,the product yields were 80.05%,78.52%, 76.90% and 62.82% for diallylmethylalkyl(C12,C14,C16,C18) ammonium bromide,respectivly,under the optimum synthetic conditions. The obtained products have expected structures and good solubility in polar solvents. The present work would be the foundation for further researche on preparation and the relationship between structure and properties of the corresponding polymers.
2014, 31(10).
Abstract:We established a green cogeneration of high purity of zinc glycerolate(ZMG) and glycerol carbonate(GC) by using glycerol.Through just one pot, we synthesized impure zinc glycerolate first. And then we continued to synthesize glycerol carbonate. During this moment, the zinc glycerolate acted as a catalyst for glycerol carbonate synthesis and the process promoted the purity of zinc glycerolate. After the reaction, put some precipitating agent and the zinc glycerolate was precipitated. The purity of zinc glycerolate was above 97%.After the separation of the liquid mixture, we got glycerol carbonate which the purity above 97%. We discussed the product’s structure based on FTIR、XRD and elemental analysis as well. After all, the cogeneration provided a means to give a high-value conversion of glycerol and had broad application prospects.