• Volume 27,Issue 4,2010 Table of Contents
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    • >Review and monographs
    • Modification of organic pigments via coating method

      2010, 27(4).

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      Abstract:The recent developments in the modification of organic pigments by coating technology with inorganic particles are reviewed. The preparation mechanism of the encapsulated organic pigments is summarized and some examples of the organic pigments coated on the inorganic core or encapsulated with inorganic compounds such as silica, titania and some other inorganic pigments are introduced. The applied prospect of the organic coating pigments is also discussed.

    • >Modernization technology of traditional Chinese medicines
    • Study on Synthesis of 4-methoxy-3-halogenated biphenyl

      2010, 27(4).

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      Abstract:4-methoxy-3-halogenated biphenyl was synthesized from p-dimethoxybenzidine via diazotization at -5~0℃ and Sandmeyer reaction with Cuprous Bromide or Cuprous chloride at 90℃, Some factors affected the reaction,such as the mw material rate,the reaction time and the reaction temperature were also discussed. The structure of the product was confirmed by melting point, IR and 1H NMR .The results show that the total yield of 3-Chloro-4-methoxybiphenyl synthesized by this preparation procedure was 63% and 3-Bromo-4-methoxybiphenyl was 51%.

    • Study on the Synthesis of Diallyl phthalate

      2010, 27(4).

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      Abstract:Diallyl phthalate, whose structure was identified by IR and 1H-NMR, was obtained by allyl alcohol and phthalic anhydride. A series of influential factors to the reaction, such as the mole ratio of allyl alcohol to phthalic anhydride, amount of tosic acid, different kinds and amount of inhibitors and volume of methylbenzene were investigated. The appropriate reaction condition are as follows(based on 0.1 mol phthalic anhydride), n(allyl alcohol):n(phthalic anhydride)= 2.4:1, amount of tosic acid 0.8 g and 4-hydroxyl-2,2,6,6-tetramethyl piperidinyloxy nitroxide radical 0.32 g, volume of methylbenzene 35 mL, ,reacted under reflux condition until no water generated, the yield of diallyl phthalate is about 96.5%.

    • Hepatoprotective effect and antioxidant activity of Cultivate Cistanche deserticola Y. C. Ma

      2010, 27(4).

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      Abstract:The antioxidant activity of the extracts of Cultivate Cistanche deserticola was assayed by the method of DPPH, ABTS and FRAP in vitro. Mouse model of acute hepatic injury was established by giving CCl 4 abdominally. The activities of ALT and AST in serum and the levels of MDA and SOD in liver tissue were examined to evaluate the hepatoprotective and antioxidant activity of ethanol extract of Cultivate C. deserticola. The ethanol extract was the highest antioxidant activity in four extracts which the values of RACT50 were 3534.32 祄ol/g, 2726.39 祄ol/g and 2621.68 祄ol/g in DPPH, ABTS and FRAP assay respectively. It was slightly lower than that of BHA as positive control, and higher than that of BHT. The ethanol extract of Cultivate C. deserticola significantly reduced the activities of ALT and AST in serum and the levels of MDA in liver tissue, and significantly raised the levels of SOD in liver tissue. The results showed that the ethanol extract of Cultivate C. deserticola had a significant hepatoprotective effect in CCl4-induce acute liver injury. The mechanisms may be related to its effects of reducing lipid peroxidation product.

    • >Catalysis,separation and purification technology
    • Study on decoloration process of Crude glycerol as biodiesel by-product

      2010, 27(4).

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      Abstract:Crude glycerol can be obtained by distillation of biodiesel by-product. Its decoloration process by absorption of active carbon prepared by coconut shell was investigated and analyzed. The results indicated that LY-725B active carbon was selected as the optimal decolorant. In addition, decoloration temperature, decoloration time and active carbon dosage were chosen as the three main factors of response surface optimization model. After experiment and analysis with Minitab Program, the optimal process conditions were found as follows: m(activated carbon): m(crude glycerol)=2.2%, decoloration temperature 48℃ and decoloration time 31min. Under those optimal conditions, the transmittance and once through yield of discolored glycerol reached 96.1%, and 72.6%, respectively.

    • The effects of the precipitators on the low-temperature oxidative coupling of methane over SrCO3/La2O2CO3 catalysts and the thermal effects in the reaction

      2010, 27(4).

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      Abstract:A series of SrCO3/La2O2CO3 catalysts prepared by thermal decomposition and co-precipitation method were tested in low-temperature OCM (oxidative coupling of methane). The choice of precipitators played great role on the catalytic performance, and the catalysts obtained by the multiple precipitators NaOH/Na2CO3 showed better activity and stability than the catalysts obtained by single precipitator. Both tetragonal (I-) and hexagonal (II)-La2O2CO3 was detected in the catalysts, and their coexistence provided two types of active sites for OCM to produce C2 and deep oxidation of methane to produce COx, respectively. The later reaction was high exothermic, which provided the hot spot for the ignition of the OCM reaction, and great energy to maintain the reaction. The catalyst with 25 mol.% of SrCO3 could hold the reaction for at least 24 h at Tex=100 oC (external furnace temperature) with CH4 conversion of 25.6% and C2 selectivity of 43.4%.

    • Synthesis, Characterization and Catalytic Phenol Hydroxylation Performance of Iron-modified Hexagonal Mesoporous Silica

      2010, 27(4).

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      Abstract:An iron-modified hexagonal mesoporous silica(Fe-HMS) was prepared by sol–gel method with tetraethyl orthosilicate(TEOS), iron trichloride and template reagent of dodecyl amine(DDA) as the raw materials, and the physicochemical properties of the synthesized Fe-HMS were characterized by XRD, FT-IR, UV-Vis, ESR, TG–DTA, ESEM, TEM and nitrogen adsorption–desorption testing technology. Additionally, the catalytic performance of the Fe-HMS on the reaction of phenol hydroxylation was also investigated. The results showed that the Fe-HMS prepared was spherical small particles with stable hexagonal mesoporous structure, and the irons were embedded into the frameworks of the HMS. Furthermore, the Fe-HMS exhibited a higher catalytic activity in the hydroxylation reactions of phenol, and the highest conversion ratio of phenol reached 46.9%. The catalyst could be regenerated after calcined at 450℃ for two hours. The conversion of phenol still could reach 36.4% even after seventh cycle.

    • Synthesis of Ethyl Ferulate Catalyzed by Strong Acidic Cationic Exchange Resin

      2010, 27(4).

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      Abstract:Ethyl ferulate was synthesized from ethanol and ferulic acid by direct esterification using cation exchange resin as catalyst.The effects of resin type,amount of catalyst,reaction time,materials ratio and repeatability of catalyst on the synthesis were studied.The optimal reaction conditions were given as follows:m(resin)∶m(ferulic acid)=12%,n(ethanol)∶n(ferulic acid)= 6∶1, reflux reaction time 7 h.The yield of product was 83.4% and 78.1% respectively under above conditions. The conversion rate of ferulic acid and yield of product keep greater than 81% and 75% respectively after the 732# resin was used four times.

    • >Perfumes and essences
    • Preparation of Optically Active Flavors 3-Methylthio Hexanol and Its Acetate

      2010, 27(4).

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      Abstract:The syntheses of optically active 3-methylthio hexanol and 3-methylthio hexyl actetate were studied starting from (E)-2-hexenal through reduction, the Sharpless asymmetric epoxidation, regioselective reduction and SN2 nucleophilic substitution. (E)-2-hexenal was reduced by NaBH4 to give (E)-2-hexenol in about 91% yield. The optically active 2, 3-epoxy hexanol was obtained through the Sharpless asymmetric epoxidation of (E)-2-hexenol with about 94% e.e. in about 86% yield. 2, 3-Epoxy hexanol was regioselectively reduced with Red-Al to give optically active 1, 3-hexanediol in about 82% yield. After the primary hydroxy group of 1, 3-hexanediol was transformed to acetate and 3-hydroxy was transformed to mesylate, an SN2 nucleophilic substitution by the reaction with self-made sodium thiomethoxide was carried out to form 3-methylthio hexanol. The overall yield of these three steps was about 59%. 3-Methylthio hexanol was esterified with acetic anhydride to give 3-methylthio hexyl acetate in about 87% yield. The final products 3-methylthio hexanol and 3-methylthio hexyl actate were obtained with about 94% e.e..

    • Study on ozonolysis of anethole in single solvent with carbonyl group

      2010, 27(4).

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      Abstract:Anisaldehyde was prepared by the ozonolysis of anethole. By experiment, a single solvent system with carbonyl group was fond in which anisaldehyde had a good yield. Meanwhile, the species and mass of solvent and flow of ozone and time of the reactivity were investigated. The optimum conditions are as follows: acetic ether or acetone as solvent, the mass ratio of anethole and solvent is 1:3, the flow of ozone is 0.06 m3/h, the time of the reactivity is 80min. In this condition, the percent conversion of anethole is 100% and the yield of anisaldehyde is 74.54% in ethyl acetate and 73.61% in acetone.