• Volume 27,Issue 6,2010 Table of Contents
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    • >Drug and cosmetic materials
    • Preparation and characterization of amphiphilic polyethyleneglycol-graft- poly(lactic acid)(PPLA) copolymer micelles

      2010, 27(6).

      Abstract (489) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:To prepare PPLA polymeric micelle and investigate their general properties, in vitro drug release characteristics. The surface hydrophilicity investigated by static water contact angle method. Using rotary evaporation method for reparation graft copolymer micelles. Critical micelle concentration(CMC), diameter, morphology and surface potential of the micelles were investigated by pyrene fluorescent probe technique,inverted imaging microscope and dynamic light scattering (DLS), respectively. Single factor tests and orthogonal tests on the the ratio of acetone, addition amount and addition sequence of material and drug were carried out for optimization. The in vitro release behavior of naproxen from polymeric micelles was investigated using dialysis method .The results indicated the water contact angle of the PPLA film was nearly 5? CMC was 3?0-4g?L-1. The micelle was globular-shaped ,had a narrow size distribution with an average particle size under of 200nm,the Zeta potential was lower than-20 mV, while dilution, standing and alkaline change to basic condition had no effect after preparation. The optimum preparation conditions were 0.8mg naproxen,10mgPPLA simultaneous dissolution in 1.0ml acetone,then drop into 10ml water. In PBS(0.01 mol?L-1)at 37℃ can duration release be up to 5 days. So we can concluded that PPLA would be a noveles applied Polymer Carriers as promising drug delivery system for hydrophobic drugs.

    • >Functional materials
    • Properties of degradable Polypropylene carbonate composite materials

      2010, 27(6).

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      Abstract:Blending modification of poly(propylene carbonate)(PPC) and Blending modification of poly(propylene carbonate)(PPC) and polylactic acid (PLA) was finished, thermal performance, mechanical properties and biodegradability were raised. Properties of composites were studied by SEM, XRD, DSC, TG and tensile test. The results showed that no chemical reaction had occurred, and blends were partially compatible. Thermal properties of PPC were improved. The optimal Tg of composites was 30℃ higher than that of PPC. The optimal Td5% of composites was 42℃ higher than that of PPC. The optimal Td50% of composites was 67℃ higher than that of PPC. With PLA addition the degradation of composites was better than that of PPC. After 40 days degradation, the largest weight loss rate of composites was 33.37% which was 9 times of that of PPC. The PPC-PLA composites had good film forming ability and the film transparent and uniform. The tensile strength of composites ranges from 36 to 58MPa. The maximum young's modulus of composites was 2943MPa.

    • Synthesis and characterization of 2-substituted-benzimidazolato copper(II) complexes under microwave irradiation

      2010, 27(6).

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      Abstract:Abstract: Using reactants of copper chloride and correspoinding 2-substituted benzimidazole in organic solvent of acetone or 2-butanone, Copper complexes of 2-phenyl-benzimidazole (BIm_a) and 1-(p-methoxybenzul)-2- (p-methoxyphenzyl)-benzimidazole (BIm_b) were synthesized under microwave irradiation with the yield of 80% and 75% respectively. The melting point of BIm_a or BIm_b copper complex was measured as 145℃ and 225 ℃ separately. Methods of equipment analyses, such as IR, XRD, UV, DSC / TG, SEM, melting point, were employed to characterize the properties and structures of the complexes. Coordination reaction was confirmed from measurements of molar conductivity, infrared spectra, and UV spectra. The crystal was determined as monoclinic from XRD and SEM characterization. The coordination number was determined as 1 and 0.5 for copper complex of BIm_a and BIm_b.

    • Synthesis and Characterization of the PEO-terminated Groups Poly(amidoamine) Dendrimers

      2010, 27(6).

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      Abstract:Abstract: A series of polyoxyethylene macromonomer (PEO-A) with terminal acryloyl-groups have been synthesized from different molecular weight of polyethylene glycol and acrylchloride as raw materials via acyl-chloride method. Results show a better molar ratio n(PEG) : n(CH2CHCOCl) : n((CH3CH2)3N) is 2:1:1. Then the PEO-terminated groups non-ionic PAMAM dendrimers were prepared via Michael addition reaction of 96 h using PEO-A as the modifier for exterior terminal groups of PAMAM G1.0 ~ G4.0 dendrimers in the N2 atmosphere, 50 ℃ THF solution, respectively. The composition and structure of the modified dendrimers have been identified via FTIR, 1H NMR and 13C NMR.

    • Size-controlled Synthesis and Characterization of Monodisperse Fe3O4 Submicrospheres

      2010, 27(6).

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      Abstract:Fe3O4 submicrospheres were synthesized by the solvothermal synthesis at 200℃, using FeCl3?6H2O and ethylene glycol as reactants. The size of as-prepared Fe3O4 submicrospheres could be controlled in the range of 115-435nm in diameter by adjusting some growth parameters. The structure, size, morphology and composition of the as-prepared Fe3O4 submicrospheres were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM). The results showed that the Fe3O4 submicrospheres were of inverse spinel structure. Magnetic propertie of 330 nm Fe3O4 submicrospheres has been detected by a vibrating sample magnetometer at room temperature. The coercive force, saturation magnetization and remanent magnetization of 330nm Fe3O4 submicrospheres are about 83.5 Oe, 81.2 emu/g and 14.6 emu/g, respectively. The influence of ethylene glycol, concentration of NaOH, and reaction time on the morphology development was experimentally investigated. It was found that ethylene glycol molecules have a significant effect on the formation of Fe3O4 submicrospheres. A possible mechanism was also proposed to account for the growth of these Fe3O4 submicrospheres.

    • >Surfactants
    • Phase Behavior and Rheology Property of LAS/AEO-9/C3H8O3/H2O System

      2010, 27(6).

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      Abstract:Abstract: Phase behavior and rheology property of LAS/AEO-9/C3H8O3/H2O were studied with polarizing microscope and RS75 rheometer. The results show that only lamellar phase could be observed on the side of the LAS/C3H8O3/H2O of the phase diagram. On the side of the AEO-9/C3H8O3/H2O, the changes of phase of the surfactant solution were different. With the increasing of surfactant concentration, the phase in the solution changed from micelle solution to hexangular phase, gradually. The patterns of lamellar phase and hexangular phase have been observed under polarizing microscope. The results of rheology corresponded to the phase behavior.

    • Synthesis and Characterization of Quaternary Ammonium Salts Methyl Carbonate

      2010, 27(6).

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      Abstract:The quaternization of long chain alkyl tertiary amine with dimethyl carbonate was studied. The effects of reaction temperature, reaction time, material mol ratio and solvent dosage on quaternization of N, N-dimethyldodecylamine were examined, and the optimized reaction condition was determined. The optimized condition was : reaction temperature 130 ℃, reaction time 5 h, n (dimetyl carbonate)︰n (alkyl tertiary amine)=5, methanol dosage (based on the materials) 10%. Under the optimized conditions, the conversions of mono-alkyl tertiary amines with different carbon chain length could reach over 98%, while the conversions of N-methyldidecadeamine and N-methyldioctadecylamine were 88.09% and 68.77% respectively. These indicated that space steric hindrance was the main factor for the quaternization process, consisting with the results of molecular space structure simulation. Through extending reaction time, the conversion of N-methyldidecadeamine can reach to 98.96% after 7 h and N-methyldioctadecylamine can reach to 95.68% after 12 h. The quaternary ammonium salts were characterized by 1H-NMR and IR. The results showed that quaternary methyl carbonates were synthesized successfully.

    • >Modernization technology of traditional Chinese medicines
    • α-Glucosidase inhibitory activity in vivo and vitro of Lindera glauca (Sieb1et Zucc) Blume

      2010, 27(6).

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      Abstract:To investigate the yeast and rat intestinal α-glucosidase inhibitory activity of Lindera glauca (Sieb1et Zucc) Blume. in vitro and vivo. Its α-glucosidase inhibitory activity was assayed by the method of 96-microplates. The results showed that yeast α-glucosidase inhibitory activity of petroleum ether extracts (IC50 = 229.70 μg/mL), ethyl acetate extracts (IC50 =259.10 μg/mL) and n-butanol extracts was lower than that of Acarbose (IC50=1081.27 μg/mL) as positive control, and only ethyl acetate extracts (IC50 =418.17 μg/mL) showed rat intestinal α-glucosidase inhibitory activity. The IC50 value of Acarbose did not be detected. The results indicate that all the extracts of L. glauca showed a better yeast α-glucosidase inhibitory activity and only ethyl acetate extracts showed a better rat intestinal α-glucosidase inhibitory activity.

    • >Catalysis,separation and purification technology
    • Ultrasound-surfactant extraction of total dioscin from Dioscorea zingiberensis. C. H. Wright

      2010, 27(6).

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      Abstract:Effects of ultrasonic frequency, the processing time as well as the solid-liquid ratio on the extraction of dioscin were investigated, also selected proper surfactant and usage for ethanol extraction, and using electrical conductivity method determinate the critical micelle concentration, finally obtained an optimization process by orthogonal experiments. The results showed that the best extraction conditions were: ethanol volume fraction was 30%, ultrasonic frequency was 25.8kHz, ultrasonic time was 40min, solid-liquid ratio was 1:10, sodium lauryl sulfate(SDS) usage was 17.408?0-3mol/L. The process can significantly increase yield, saving time and energy, reduce pollution, has a great feasibility in industry promoting.

    • Synthesis of Diethyl 2-(2-cyanoethyl) malonate Catalyzed by L-Proline

      2010, 27(6).

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      Abstract:Diethyl 2-(2-cyanoethyl)malonate was synthesized from diethyl malonate and acrylonitrile by Michael addition reaction using L-proline as catalyst. The effects of the reaction condition on the yield and the enantiomeric excess value of Diethyl 2-(2-cyanoethyl)malonate were investigated.A 74.10% yield ( the yield is higher than 67.6% in the literature which was reported.)with 79% enantiomeric excess was obtained under the optimal reaction conditions: pyridine as solvent; the dosage of diethyl malonate, 0.1mol; the mole ratio of diethyl malonate to acrylonitrile, 1:1.2; the dosage of L-proline, 0.04mol; reaction time, 48 h; and temperature, 35℃, respectively.

    • Study on the extraction of Collagen with enzyme under supersonic from the skin of Monopterus albus

      2010, 27(6).

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      Abstract:The extraction conditions of the collagen in the skin of Monopterus albus are studied in this paper. The extraction conditions are optimized by experiment to five factors of extraction time of supersonic,the addition of trypsin, temperature, pH and the decomposition time of enzyme. The result shows that the optimum conditions are supersonic extraction time 3min, the amount of 150U/g ftrypsin, pH7.2, temperature of 35℃, the decomposition time of enzyme 7 hours ,and the extraction rate of collagen is 92.4%. Collagen are analyzed by UV and IR. The result shows that the λmax of product is 226 nm and the functional groups of collagen have peptide bond, carbonyl, carboxyl etc.

    • Preparation of 1-Hydroxyethylidenediphosphonic acid (HEDPA)with low low concentration of arsenic

      2010, 27(6).

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      Abstract:With sodium sulfide as a reducing reagent and a precipitant in acidic condition, the removal of arsenic (As (III) and As (V)) from industrial 1-Hydroxyethylidenediphosphonic acid (HEDPA) is carried out by a reduction-precipitation method. The purpose is to obtain the effect the quantity of the sodium sulfide, pH value of the solution factors, temperature, time, and mixing speed on de-arsenic. The result shows that the optimal temperature, pH, mole ratio of sodium sulfide to arsenic species and agitation rate are 50℃, 0.5, 4:1 and 90rpm, respectively. After 2h under the selected conditions, the corresponding concentration of arsenic species in HEDPA and efficiency of arsenic removal are 0.28 mg•L-1 and 99.3%, respectively. HEDPA treated by the procedure can serve as detergent & cosmetics additives and raw materials for synthesis of drugs.

    • Study on the Catalyst and Process for the Synthesis of Butyronitriles through Catalytic Ammoniation of Butanols

      2010, 27(6).

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      Abstract:A catalyst Co20.0-Ni3.0/-Al2O3 for the synthesis of butyronitriles through the ammoniation of butanols was selected and its structure was characterized. Then, the process and the stability of the catalyst were investigated for the synthesis of butyronitriles through the ammoniation of butanols using Co20.0-Ni3.0/-Al2O3 as catalyst in a fixed-bed reactor. When the reaction was run at 410 ℃(420 ℃) under the parameters which the molar ratio of ammonia to butanol is 3 : 1, LHSV is 0.3 h-1 (0.2 h-1) and pressure is 0.1 MPa, respectively, the conversion of n-butanol (i-butanol) and the yield of n-butyronitrile (isobutyronitrile) were 100% and 81.6 % (80.6 %), respectively. The activity of the catalyst was maintained and the selectivity for butyronitrile decreased less than 1 % after the catalytic run was lasted for 100 h, which revealed that the catalyst has good performance and stability in application.

    • >Perfumes and essences
    • Advance in Synthesis of Natural Benzaldehyde

      2010, 27(6).

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      Abstract:Natural benzaldehyde is one of short-supply international spice. In this paper, several synthetic methods of natural benzaldehyde are reviewed: hydrolysis of Laetrile; synthesis of cinnamon oil and biotransformation of L-phenylalanine. Preparation of natural benzaldehyde from natural cinnamon oil, which is rich in China, is introduced in detail, including oxidation, alkaline hydrolysis and NCW (near-critical water) method, with a view to provide guided information for increasing the added value of natural cinnamon oil.

    • >Drug and cosmetic materials
    • Study on Synthesis of 6-Hydroxy-1H-quinolin-2-one in Ionic Liquid

      2010, 27(6).

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      Abstract:A method for synthesis of 6-hydroxy-1H-quinolin-2-one in ionic liquid was studied. The title compound was prepared from p-methoxyaniline via bromination, acylation and Heck reaction. The effects of reaction conditions on bromination and Heck reaction were investigated. p-Methoxyaniline was reacted with ionic liquid [bmim]Br3 to afford 2-bromo-4-methoxyaniline in 98.2% yield and 99.5% purity. N-(2-Bromo-4-methoxyphenyl)acrylamide was obtained by the acylation of 2-bromo-4-methoxyaniline with acryloyl chloride in 95.7% yield. The Heck reaction of N-(2-bromo-4-methoxyphenyl)acrylamide was effectively performed in the presence of ionic liquid [bmim]Br, Pd(OAc)2, K2CO3 and DPPP to afford 6-hydroxy-1H-quinolin-2-one in 91.5% yield. The new procedure for preparing 6-hydroxy-1H-quinolin-2-one has the advantages of good yield, simple operation and environmental benignity.

    • Synthesis and characterization of polyethylene glycol urethane prodrugs containing 5-fluorouracil

      2010, 27(6).

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      Abstract:A series of polyethylene glycol derivates was synthesized by the reaction of α-chloroacetyl isocyanate with polyethylene glycol. Owing to the good reactive activity of α-chlorin in terminal it can react with 5-fluorouracil, the prodrug could be obtained. The prodrug was characterized by FT-IR, 1H-NMR and UV spectroscopy and confirmed that the 5-fluorouracil unit was successfully connected to polyethylene glycol terminal. The maxmium loading content of prodrug was 22.6% measured by UV and it showed enhanced water solubility and longer duration of activity due to slow release compared with 5-fluorouracil. The prodrugs could release 5-fluorouracil or its derivatives in different pH solution. When the moleculare weight reaches 2000, it has the fastest hydrolyzation speed, the maximum drug release percentage was 71.5% in 20h.

    • Synthesis of lamivudine

      2010, 27(6).

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      Abstract:Abstract:The synthetic method of typical antivius agent of pyrimidine nucleoside lamivudine is reported.(1R)-(-)-Menthyl glyoxylate hydrate was synthesized from L-menthol and glyoxylic acid by a five-step way including esterification,cyclization,chlorination,condensation and reduction. In the synthesis process of MGH, the perfect molar ratio was n(L-menthol):n(glyoxylic acid)=3:1; In the synthesis process of NA, triphosgene replaced dimethyl sulfoxide and the yield was 60.3%. NA was reduced to lamivudine using sodium borohydride- methanol -THF system,which gave the 84.8% yield.The total yield reached 30.9% and the objective product was characterized with MS and IR

    • >Papermaking chemicals
    • Structure and Properties of Polyacrylate resin -b-Poly (Glycidyl Methacrylate)

      2010, 27(6).

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      Abstract:Abstract: Self-crosslinking Polyacrylate resin -b-Poly (Glycidyl Methacrylate) Copolymer was prepared by the emulsifier-free copolymerization with acrylic acid(AA)/acryl amide(AM)/vinyl cyanide (AN) / methacryloxyethyl trimethylammonium chloride(DMC) as the main materials, using GMA as crosslinking agent,polyvinyl alcohol (PVA) as dispersing agent. The particle structure and the physical properties of the copolymer were investigated by TEM、FT-IR、XRD and DSC. The microstructure of surface and cross section of paper were observed by SEM. The experimental results show that the self-crosslinking Polyacrylate resin -b-Poly (Glycidyl Methacrylate) Copolymer emulsion thus obtained is quite stable; the copolymer is amorphous polymer, and the strength of the crosslinking copolymer is highly increaseced after cross lined by GMA; When w (GMA) =0.7%, w (PVA) =0.4%, the ring crush index, bursting strength and tensile index can reached to 16.64N.m/g、440KPa、33.54N.m/g , improved by about30%.

    • >Fine chemical intermediates
    • Synthesis of Ethylene Glycol Dimethacrylate by Air Stripping

      2010, 27(6).

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      Abstract:Ethylene glycol dimethacrylate was synthesized by direct esterification of ethylene glycol and methacrylic acid. Instead of the water-carrying agent, air was used to remove the water that resulting from the esterification process. The effects of mixture gas of oxygen with nitrogen, argon and carbon dioxide respectively were studied. The results showed that nitrogen, argon and carbon dioxide have no assisted inhibit ability, and the assisted inhibit ability of the mixture of oxygen with other gases were better than pure oxygen. Air was the optimum water-carrying gas which can reduce the dosage of inhibitor. The effects of dosage of catalyst, ratio of ethylene glycol and methacrylic acid, reaction time, rate of air and dosage of inhibitor on yield were also investigated. The yield was 93.5% at the optimum conditions: dosage of tosic acid was 5% of the total weight of reactants, n(ethylene glycol):n(methacrylic acid) = 1:2.4, volume flow rate of air was 0.2L/min, dosage of hydroquinone was 0.1% of the total weight of reactants, reacting at 110℃ for 3 hours.

    • Synthesis of sodium 4-methylbenzene sulfinate

      2010, 27(6).

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      Abstract:The synthesis of sodium 4-methylbenzene sulfinate was investigated by using sodium sulfite deoxidization process from the starting material 4-methylbenzene sulfonyl chloride and the contents of product were analyzed by UV-spectrophotometric method. The aqueous sodium sulfite which used as substrate was added dichloromethane solution containing 4-methylbenzene sulfonyl chloride, at the same time , the pH was controlled by adding dropwise 10% sodium hydroxide solution in the reaction process. The optimun reaction conditions were shown as follows: n(4-methylbenzene sulfonyl chloride)/n( sodium sulfite)=1:1.09, reaction temperature 85℃, reaction time 1h, m(water)/m(4-methylbenzene sulfonyl chloride)=10, pH=7.6,with a yield of 89%.

    • Synthesis of Diphenylmethane by Alkylation Of Benzene with Benzyl Chloride by Ionic Liquid

      2010, 27(6).

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      Abstract:Diphenylmethane was prepared via Friedel–Crafts benzylation reaction over a series of ionic liquids as catalysts. The effects of the ratio of metal chloride to BmimCl or BpyCl, the amount of ionic liquids and different ionic liquids on the Friedel–Crafts benzylation were also investigated. The results showed that only the acidic ionic liquids had good catalytic activity, and the activity of ionic liquids correlated strongly with its acidity. The best yield of diphenylmethane for BmimCl-AlCl3 catalyst (97.4 %) and BpyCl-AlCl3 catalyst (92.1 %) were obtained with the mole fraction of AlCl3 66.7%, 3.3 g ionic liquid at 80 ℃ and atmospheric pressure. The ionic liquids could be reused four times without noticeable drop in activity.

    • Synthesis of L-menthylformaldehyde

      2010, 27(6).

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      Abstract:L-menthylformaldehyde was synthesized by the reaction of the Grignard reagent derived from menthyl chloride with N,N-dimethylformamide (DMF) in tetrahydrofuran by one-step process. The influence of the material ratio, reaction temperature and reaction time on the yield of the product had been investigated. The optimal reaction condition was the Grignard reagent reaction with 1.2 equivalent of DMF at 20oC for 4 hours. Under optimal reaction condition, the yield was 42.6% and no stereoisomer yielded.