• Volume 29,Issue 10,2012 Table of Contents
    Select All
    Display Type: |
    • >Modernization technology of traditional Chinese medicines
    • Antioxidant Activities of the Flavonoids of Gynura in Vitro and in Vivo

      2012, 29(10).

      Abstract (411) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:To separate and purify the total flavonoids in Gynura and study its antioxidant activities in vitro and in vivo. The total flavonoids were preparated by 80% alcoholic. After removing impurities, the crude extracts were purified with type AB-8 macroporous adsorption resin. The content of total flavonoids was determined by spectrophotometry. The antioxidant activities in vitro of the total flavonoids were analyzed by using different assays compared with Vc, such as DPPH radical (DPPH•) scavenging assay, hydroxyl radical (•OH) scavenging assay, superoxide radical (O2-•) scavenging assay. The antioxidant activities were tested with the purified flavonoids in vivo. The content of total crude flavonoid from Gynura was 13.928 mg/g, and the purification ratio was 32.79%. The radical scavenging effect was enhanced with increasing flavonoid concentration. The scavenging effect of the purified flavonoids was greater than the crude extracts. The level of superoxide dismutase (SOD) activity of mice brain and liver was higher significantly in low doses groups than in normal control groups (p < 0.05), so was the level of catalase (CAT) activity of liver.The brain malondialdehyde (MDA) content was obviously lower than normal control groups(p < 0.05).

    • >Catalysis,separation and purification technology
    • Synthesis of lactonic crown ethers by ethoxylation of γ-butyrolactone

      2012, 29(10).

      Abstract (378) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Lactonic crown ethers were synthesized by a novel insertion reaction of ethylene oxides into γ-butyrolactone (GBL) catalyzed by Al-Mg composite oxide, and the molecular structures of the target products were confirmed by FT-IR and ESI-MS. The process was optimized with respect to Al/Mg molar ratio of catalysts, reaction temperature and pressure. The conversion of GBL was 75.2% when the insertion reaction was catalyzed by 1 %(w/w) of LE-4 catalyst based on the target products and run in 5 times molar ratio of EO to GBL at160oC under 0.65 MPa.

    • Reverse micelle -mediated synthesis of silicalite-1 zeolites with different morphology

      2012, 29(10).

      Abstract (576) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The synthesis and characterization of silicalite-1 made in reverse micelle at 433k are reported. Silicalite-1 materials formed in reverse micelle synthesis possessed different shapes compared to those formed by conventional methods. Syntheses were also performed to ascertain how the content of surfactant and heptane, silica source and NaOH content influence material properties. The current work showed that the morphology of the crystals obtained was highly sensitive to surfactant and heptane content and silica source, but insensitive to the NaOH content. Silicalite-1 materials that were coffin, hexagonal prismatic and rod shapes could be obtained in the present of reverse micelle.

    • Preparation of D-Serine by enzymatic resolution of D,L-Serine using Tryptophanase

      2012, 29(10).

      Abstract (499) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A practical method was established to resolute L-Serine into L-Tryptophan via Tryptophanase, using D,L-Serine as the substrate. D-Serine could be obtained after isolation and purification. Response surface methodology was used to optimize the conditions of the enzymatic resolution. And the optimum conditions were: 45℃, pH 8.0, 18 hours, 30 g/L of substrate concentration and 6 g/L of Tryptophanase concentration. After twice similar reactions, the total conversion rate of L-Serine could be up to 95.4% .The products were separated and purified on NKA-II macroporous absorption resin, 001×7 ion-exchange resin and recrystallized at the end. The purity of the products was 99.4%.The optical rotation of D-Serine was -15.3°(C=10,2N HCl) and the total separation recovery of the products was 66.6 % .

    • The Baeyer-Villiger oxidation of ketons catalyzed by AlPO4-5

      2012, 29(10).

      Abstract (466) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:AlPO4-5 molecular sieves was prepared by hydrothermal reaction using triethylamine as template, aluminum isopropoxide, orthophosphate as the aluminum and phosphorus resource. Via chemical tailoring method with different concentrations of hydrobromic acid, AlPO4-5-AlBr3 catalysts were obtained. Several techniques such as high-resolution field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption techniques were employed to investigate their morphology, structures as well as component. The characterization showed that AlPO4-5 was hexagonal crystal with microporous structur, after chemical tailored, AlPO4-5-AlBr3 still maintained the structure. The catalytic test was performed using 30 H2O2 as oxidant and ethyl acetate as solvent. It was revealed that the catalyst had good performances for some ketons, and could be reused several times.

    • >Perfumes and essences
    • volatile compounds of Yueshengzhai Fragrant Beef extracted

      2012, 29(10).

      Abstract (438) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The volatile compounds of Yueshengzhai fragrant beef were extracted by solid phase microextraction with three different solid phase microextraction fibers:65um PDMS/DVB,75um CAR/PDMS and 50/30um DVB/CAR/PDMS. Volatile compounds were identified by gas chromatography-mass spectrometry. Comparison the difference of volatile compounds extracted with different solid phase microextraction fibers, and then found the fit solid phase microextraction fiber. 53 volatile compounds were extracted by them. Comparison with the extracted outcome, 75um CAR/PDMS was the best solid phase microextraction fibers for extracting volatile compounds of Yueshengzhai fragrant beef.

    • Preparative resolution of stereoisomers of 3-methyl-γ-octalactone by packed column supercritical fluid chromatography

      2012, 29(10).

      Abstract (576) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Packed column supercritical fluid chromatography (pSFC) was used to resolve preparatively the four optical stereoisomers of the flavor substance of 3-methyl-γ-octalactone. First, cis-, and trans- isomers were prepared by pSFC resolution of the synthetic molecule of 3-methyl-γ-octalactone on a silica gel column. Then, the effects of kind of chiral column, type of modifier solvent and content of modifier solvent in mobile phase, column temperature, column pressure, and flow rate on the resolution of the cis-, and trans- isomers were investigated in an analytical scale. The optimum resolution conditions for cis-isomers found were chiralpak AD-H, column temperature 30 ℃, column pressure 9 MPa, 4.0 % (v/v) methanol in mobile phase, and flow rate of mobile phase 1.5 ml/min, in which the resolution factor (Rs) achieved was 1.45; while those for trans-isomers found were chiralpak AD-H, column temperature 30 ℃,column pressure 10 MPa, 4.5% (v/v) methanol in mobile phase, and flow rate of mobile phase 1.5 ml/min, in which the resolution factor (Rs) achieved was 2.24. Following the optimum chromatographic conditions, preparative resolution of cis-, and trans- isomers of 3-methyl-γ-octalactone were performed further by pSFC, and four stereoisomers of several milligrams were obtained all in an optical purity of 100 % e. e.

    • >Drug and cosmetic materials
    • Synthesis of hydroxypropyl methylcellulose acetate succinate

      2012, 29(10).

      Abstract (665) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: Hydroxypropyl methylcellulose acetate succinate (HPMCAS) was successfully synthesized from hydroxypropyl methylcellulose (HPMC), which was used succinic anhydride and acetic anhydride as esterifying agent, acetic acid as organic solvent. By varying the amount of factors, HPMCAS with the different content of succinyl groups and acetyl groups were prepared. The contents were determined by titration, and then the structure of the product was characterized and tested. The results show that the reaction system was heated at 105oC for 6.5 h, after reaction we use deionized water for the precipitation agent, make products precipitated in 750 rpm speed. We can obtain that the succinyl groups and acetyl groups were about 13% and 8% respectively. The obtained HPMCAS products have the polydispersity index of 1.06 and the molecular weight distribution is narrow. The product has a good solubility in acetone, methanol and other solvents and the thermal stability is very good before 200 oC.

    • Synthetic of Hydroxytyrosol

      2012, 29(10).

      Abstract (731) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The 3,4-dihydroxyphenylacetic acid was directly given from the starting material 3,4-dimethoxyphenylacetic acid. Methyl 3,4-dihydroxyphenylacetate was obtained by reacting 3,4-dihydroxyphenylacetic acid with SOCl2 in methanol。It is the first time that the important natural product hydroxytyrosol was obtained by using sodium/ethanol reduction which on the basis of the Bouveault-Blanc classic reaction and the resulting product was characterized by 1H NMR,IR and MS。A novel synthetic method for hydroxytyrosol was provided. In addition, the influences of the molar ratio of methyl 3,4-dihydroxyphenylacetate to sodium,the reaction time,the reaction temperature on the yield of hydroxytyrosol were investigated。The mechanism for the reductive reaction of methyl 3,4-dihydroxyphenylacetate with sodium/reduction was discussed.

    • Microwave-assisted synthesis of 7,3,4'-trihydroxylflavone

      2012, 29(10).

      Abstract (317) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: 3,4–dimethoxybenzoic acid and 2-hydroxyl-4-methoxyacetophenone as the starting material, 7,3',4'-trihydroxylflavone were synthesized by acylation,esterification, Baker-Venkataraman rearrangement,cyclization and demethylation,the overall yield was 47.3%. Microwave irradiation was applied in cyclization which was the key step. Comparing with traditional heating method, the use of microwaves was found to significantly improve product yields and shorten the reaction time. The appropriate microwave reaction time was 15 min and the yield was 92.1%. HOAc/40%HBr being used as the catalyst, the demethylation was performed under the conditions of 110℃ for 36h. Finally, The structures of the compounds were confirmed by IR, 1HNMR and MS. This method is simple, eco-friendly, high selectivity and has a wide range of applications.

    • Preparation of salicylic acid-loaded lecithin/chitosan nanoparticles

      2012, 29(10).

      Abstract (630) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: The salicylic acid-loaded lecithin/chitosan nanoparticles were prepared by Solvent injection method. The structure, morphology, size distribution as well as surface potential of nanoparticles were investigated. Finally the effects of preparation technology on drug entrapment efficiency by using the dialysis technique were also studied. The preparation process adapted to the formulation was as follows:the concentration of lecithin was 20mg/mL, lecithin-chitosan and SA-carriers weight ratios were 3:1(w/w) and 1:6(w/w) respectively, the pH of Water phase reaches 4. The average diameter of optimized spherical nanoparticles was 150nm with good encapsulation efficiency and drug loading up to 55% and 8.07% respectively, the Zeta potential was 18.7mV. The preparation method of salicylic acid-loaded lecithin/chitosan nanoparticles may provide a new approach for the development of fat-soluble whitening active ingredients-loaded delivery.

    • >Starch chemicals
    • Synthesis and Viscosity Properties of 2,4-bis(3- sulfonic aniline ) -1,3,5- triazine -6- starch ether

      2012, 29(10).

      Abstract (627) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A novel starch derivative of 2,4-bis(3- sulfonic aniline ) -1,3,5- triazine -6- starch ether (BSTSS) containing sulfonic acid groups was prepared in dimethylsulfoxide (DMSO) using 2,4-bis(3- sulfonic aniline)-6-chloro-[1,3,5]-triazine (BSTS) as etherifying agent. Effect of reaction conditions on the preparation of BSTSS was studied in detail and the optimized conditions were proved as follows: n (BSTS) : n (AGU) = 0.4 : 1, n (NaOH) : n (AGU) = 0.6 : 1, reaction time 4 h. The structure of BSTSS was determined by IR and NMR and the molecular weight of the product was measured by GPC . Effect of pH on the solution viscosities was studied and the results showed that the BSTSS had good acid and base resistance.

    • >Water treatment technology and environmental protection
    • Synthesis of 2,4,6-tri[(4,- carboxyl-1,-carboxypropyl)amino]-1,3,5-trizine and Its Performance on Scale Inhibition

      2012, 29(10).

      Abstract (455) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A kind of cyanuric chloride derivatives with sale inhibition effect was prepared by cyanuric chloride and glutamic acid. The effects of the reactant ratio,the reaction time , the temperature used on the reaction were discussed. The structure was characterized by infrared spectrum. The results of scale inhibition experiment of product which were used as scale inhibitors show that the type of scale inhibitor has good scale inhibition on calcium carbonate. the study on the change of crystal form of the scale inhibitor calcium carbonate was carried out by means of scanning electron microscope analysis, the results thereof show that the crystal form of calcium carbonate can be completely distorted to form a vaterite crystal to realize the purpose of scale inhibition through 2,4,6-tri[(4,- carboxyl-1,-carboxypropyl)amino]-1,3,5-trizine.

    • >Papermaking chemicals
    • Preparation and Research on the Low Melt Viscosity C-5 Petroleum Resin Water-based Emulsion

      2012, 29(10).

      Abstract (813) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A O/W type C-5 petroleum resin emulsion was prepared with paraffin wax as viscosity regulator and blend of nonionic emulsifier. Effect of HLB value and concentration of emulsifier on stability, droplet size, viscosity and surface tension of the petroleum resin emulsion were examined. The results showed that when the paraffin added with 30% percentage composition, the C-5 petroleum resin melt viscosity decreased obviously and the material in the low temperature mixing uniformly. The suitable HLB value is about 10.75 and emulsifier concentration is 16%. The orthogonal experiment results showed that optimum conditions were, emulsifying temperature 98℃, emulsifying time 20 minutes, stirring rate 5000 rpm and emulsifying water quantity 1/3. The O/W type C-5 petroleum resin emulsion which solid content is 40% was prepared under this condition; it showed excellent stability, small droplet size and low viscosity.

    • >Acrylic series chemicals
    • The study on synthesis and properties of coal-water slurry dispersant

      2012, 29(10):0-0.

      Abstract (522) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Through the radical polymerization, IA/AA/AMPS terpolymer coal-water slurry (CWS) dispersant was prepared by acrylic acid (AA), itaconic acid (IA), 2-acrylamide-2-methylc sulfonic acid (AMPS), using water as solvent, potassium sulfate and sodium sulfite as the redox initiation system and sodium hypophosphite as chain transfer agent. Also, the slurry properties of the dispersant were investigated through IR, rheometer. The results showed sulfonic group and carboxylic acid group were successfully introduced into copolymer;The results showed that the optimal dispersant effect appeared when concentration of coal-water slurry was 68% and adding amount of was 0.6% of the total amount of monomers.

    • >Special dyes and pigments
    • Preparation of nanoscale encapsulated carbon black with branched styrene-maleic anhydride copolymer

      2012, 29(10).

      Abstract (434) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Nanoscale encapsulated carbon black was prepared by phase separation method using branched styrene-maleic anhydride copolymer. The effects of dropping speed of phase separation agent, amounts of BPSMA, pH, mass ratio of carbon black and dispersing time on particle size of carbon black were investigated. FTIR、TEM and Cantact angle analysis confirmed that BPSMA was successfully encapsulated on the surface of carbon black. The optimal preparation conditions of nanoscale encapsulated carbon black were as follows: the dropping speed of phase separation was 3mL/min, amount of BPSMA was 20%, pH was 10, mass ratio of carbon black was 8% and dispersing time was 10min. It could be found that the particle size was smaller and stability was higher, the K/S value and rubbing fastness of the printed fabric with dispersion which was prepared by BPSMA was higher than that of by linear styrene-maleic anhydride polymer.

    • >Adhesives
    • Preparation of Fluorinated Ploystyrene-acrylate Soap-free Emulsion and Its Application in Fluorocarbon Coating

      2012, 29(10).

      Abstract (426) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:A fluorinated polystyrene-acrylate emulsion (BSAD) was prepared by soap-free emulsion polymerization from dodecafluoroheptyl methacrylate (DFMA), butyl acrylate(BA)、styrene(ST) and acrylic acid(AA), with (NH4)2S2O8(APS) as an initiator. And the chemical structure, morphology of latex grain,size distribution and Zeta potential of BSLD were characterized by Infrared spectrum (IR) ,Transition electron microscopy (TEM), particle analyzer and Zeta potential analyzer. The effects of temperature and dosages of sodium acrylate、APS and DFMA on properties of emulsion were discussed. And the emulsion was employed with nano-TiO2 to prepare the fluorocarbon coating. The results showed that: when dosage of sodium acrylate was 12%, APS was 1%, and reaction temperature was 78℃,the emulsion displayed the best properties and its gel rate was 0.8%, time of water tolerance was longer than 168 hours, percent conversion was 97.1%; when dosages of DFMA was 25% of monomers ,the coating displays the best hydrophobicity and water contact angle on its surface was 113°, water absorption rate was 6.4%; and the fluorocarbon coating won satisfied effect about its properties such as the adhesion, hardness and water resistance.

    • Synthesis and Characterization of Alcohol-soluble Polyurethane Modified by Castor Oil and Nano-SiO2

      2012, 29(10).

      Abstract (419) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Hydrophobic nano-SiO2 particles were prepared from reacting coupling agent KH-550 and nano SiO2 particles in the ultrasound, and dispersed in polyurethane solution modified by castor oil (CO). The performances of polyurethane were characterized by Fourier transform infrared (FT-IR) spectroscopy, thermal gravimetric analysis (TGA) and scanning electron microscopy (SEM). The FT-IR analysis indicates the formation of chemical bond between PU and nano-SiO2, and formed the Si-O-Si particle structure. As m(CO):m(N210)=1:9 the tensile strength o f the films increased from 6.8 MPa to 16.2 MPa. The water absorption also increased two times. As the mass fraction of nano-SiO2 increased from 0 to 2%, the initial weight loss temperature of the PU films increased from 255 e to 272 e. The films performance is better, greatly improve the mechanical properties, water resistance and heat resistance.

    • Synthesis of a Lactose-Biuret resin adhesive

      2012, 29(10).

      Abstract (501) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract:In this paper,An environmental friendly lactose-biuret resin adhesive was prepared using lactose instead of formaldehyde in acid condition. The viscosity was used as an index to investigate and optimize the reactive conditions by the single factor experiment and response surface methodology(RSM).By analyzing and comparing the experimental result,the optimum conditions of the reaction process were gained: the molar ratio of lactose and biuret was 6.03:1,the reaction temperature was 198.9℃,the reaction time was 45.3min,and the catalyst amount was 1.47%. Under these conditions,the theoretical viscosity of the products was 175.6 mPa·S and the measured values was173.8 mPa·s.

    • >Fine chemical intermediates
    • A Novel Approach to the Synthesis of trans-5-Propyl-2-(4′-Bromine-Phenyl)-Tetrahydropyran

      2012, 29(10).

      Abstract (623) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract:4-Bromobenzene carboxylic acid as the starting material,which was acylated to generate acyl chloride.Firstly acyl chloride and N,O-dimethylhydroxylamine hydrochloride reacted to synthesize the amides,which reacted with chlorovinylmagnesium to synthesize alpha, beta unsaturated ketone. At the moment allyl amine was synthesized with pentanal and di-n-propylamine.By Michael addition reaction, alpha, beta unsaturated ketone and allyl amine reacted to synthesize intramolecular aldehyde and ketone,which reacted to synthesize more than 99.5% purity of trans-5-propyl-2-(4′-bromine-phenyl)-tetrahydropyran (3PyPBr)with closed loop reaction and recrystallization with ethanol.

    • Synthesis of glycerol carbonate by transesterification of glycerol with dimethyl carbonate over KF/γ- Al2O3 catalyst

      2012, 29(10).

      Abstract (494) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Series of Alumina supported alkali metal fluoride solid base catalysts were prepared by an impregnation method and applied to the synthesis of glycerol carbonate (GC) via transesterification of glycerol with dimethyl carbonate(DMC). Among these catalysts, KF/γ-Al2O3 could promote the transformation of glycerol into GC more efficiently than other catalysts. The effects of preparation conditions of KF/γ-Al2O3 and reaction conditions on transesterification of glycerol with DMC were investigated. The results proved that the loading amount of KF over KF/γ-Al2O3, calcination temperature and time of catalysts and reaction conditions had significant impacts on the conversion of glycerol and the selectivity of GC. With the molar ratio of DMC to glycerol 3:1, reacted at 80℃ for 1.5h, the conversion of glycerol, selectivity and yield of GC attained 96.1%, 98.1% and 94.3%, respectively, over KF/γ-Al2O3 catalyst with 15wt.% KF loading amount and calcined at 400℃ for 5h.

    • Synthesis of trans-4-(trans-4′-n-propylcyclohexyl)cyclohexyl -ethylene

      2012, 29(10):0-0.

      Abstract (458) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract:With cis/trans-4-(trans-4'-n-propylcyclohexyl)cyclohexyl carboxylic acid as the starting material, more than 99.9% purity of trans-4-(trans-4′-n-propylcyclohexyl)cyclohexyl-ethylene was synthesized via acylation, reduction, isomerization and Wittig reaction.The total yield was 73.2%, The structure of the target compound was confirmed by IR, GC-MS and 1HNMR.