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Table of Content

    28 February 2009, Volume 29 Issue 1 Previous Issue    Next Issue
    研究报告
    Study on Preparation of Biodiesel by Whole-cell Biocatalysis——Preparation and Catalytic Capability of Immobilized Cells
    LI Zhi-lin;LI Xun;WANG Fei;JIANG Jian-chun
    2009, 29 (1):  18-22. 
    Abstract ( 612 )   PDF (1112KB) ( 822 )   Save
    Rhizopus oryzae cells were immobilized respectively with 4 different supports, including diatomite, polyurethane foam resin (PUF), alumina and sodium alginate, and the immobilized cells were used to catalyze methylation of soybean oil with methanol. The results showed that PUF was the most suitable immobilizing support for R. oryzae cells. When 0.6gPUF was added into 80mLculture medium, the obtained immobilized cells biocatalyst had optimal performance, in which immobilized dry weight of cells and lipase activity of the culture fluid were 0.5560g and 17.4U/mL, respectively. The yield of methyl esters (ME) from the methylation of soybean with methanol catalyzed by PUF immobilized cells could reach 94%when m(methanol):m(soybean oil) was 5:1 and methanol was added in 5 batches (12h for each batch). The whole-cell biocatalyst of PUF immobilized cells can be simply prepared and separated, and it is environment-friendly and reusable.
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    Extraction, Separation, Purification and Structural Analysis of Polysaccharide from Stenoloma chusanum(Linn.)Ching
    LUO Ya-jun;XIAO Xin-feng;WANG Zhao-li
    2009, 29 (1):  68-72. 
    Abstract ( 664 )   PDF (966KB) ( 925 )   Save
    Water-soluble polysaccharide in Stenoloma chusanum(Linn.)Ching is extracted by means of hot water. Polysaccharide is purified by enzyme treatment and Seveg method to remove protein, then decolorized by 10% H2O2 to remove pigment, followed by DEAE-cellulose column chromatography. Polysaccharide is shown to be a single homogeneous component by PC and Sephadex G-100 column chromatography, and their structural composition was studied by means of permeation chromatography (GPC),TLC, GC-MS, UV, IR, etc.. The average molecular mass of polysaccharide is 8.6×104u. Polysaccharide is composed of glucose, arabinose and uronic acid. There is no absorption peak of protein and nucleic acid at 280 and 260nm. Polysaccharide of this plant is a non-proteinous single polysaccharide containing β-glucopyranose.
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    Comparison of Structure Formation of Phenol-urea-formaldehyde Resin
    LEI Hong;DU Guan-ben;PIZZI Antonio;LI Qin;ZHAO Wei-gang;FANG Qun
    2009, 29 (1):  73-78. 
    Abstract ( 656 )   PDF (943KB) ( 731 )   Save
    The progresses of structure formation of phenol-urea-formaldehyde (PUF) resin prepared in two different routes were followed by 13CNMR which allowed quantitative analysis of the main function groups in the PUF prepolymers. The structures of three different PUF resins were compared too. The results showed that the medium condition at the initial stage of the preparation had decisive effects on the formation of phenol methylol. Acidic condition caused the increase of urea-formaldehyde prepolymer and co-condensed PUF resin. The final structures of PUF resins were different when acidic condition was in different stage during the preparation.
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    Study on Quality of Tea-tree Oil Produced by Different Production Processes
    LIANG Zhong-yun;LIU Hong;CHEN Hai-yan;CHEN Zu-hong;
    2009, 29 (1):  107-110. 
    Abstract ( 508 )   PDF (713KB) ( 1123 )   Save
    Contents of main chemical constituents and physico-chemical indexes of oil of Melaleuca alternifolia L. of terpinen-4-ol type(tea-tree oil) produced by different production processes were analyzed according to ISO 4730-1996 standard. It was found that content of heavy constituent of tea-tree oil produced by small-scale perfumer oil production device was below 5%, which indicated that boiling point of heavy constituents in the oil is too high to be distilled under normal pressure.
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    Study on Chemical Constituents of Ilex rotunda Thunb.
    SUN Hui;ZHANG Xiao-qi;CAI Yan;HAN Wei-li;WANG Ying;YE Wen-cai;
    2009, 29 (1):  111-114. 
    Abstract ( 746 )   PDF (555KB) ( 772 )   Save
    Chemical constituents of the cortex of iron holly (Ilex rotunda Thunb.) were studied. Twelve compounds were isolated, and their structures were identified as rotundic acid (Ⅰ), pomolic acid (Ⅱ), pedunculoside(Ⅲ), kudinoside H (Ⅳ), 3β--19α-hydroxyolean-12-en-28-oic acid 28-O-β-D-glucopyranosyl ester (Ⅴ), syringaresinol 4'-O-β-D-glucopyranoside (Ⅵ), caffeic acid 4-O-β-D-glucopyranoside (Ⅶ), vanillic acid 4-O-β-D-glucopyranoside (Ⅷ), syringin (Ⅸ), sinapaldehyde glucoside (Ⅹ), β-sitosterol (Ⅺ) and β-daucosterol (Ⅻ). Among them, compounds Ⅱ, Ⅳ-Ⅷ were isolated from this plant for the first time.
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    综述评论
    Research Progress on Liquefaction of Waste Biomass and Utilization of Products in China
    ZHANG Qiu-hui;ZHAO Guang-jie
    2009, 29 (1):  120-126. 
    Abstract ( 546 )   PDF (1288KB) ( 845 )   Save
    The research progress on liquefaction of waste biomass and the utilization of products in China are systematically described in this review.The importance of studying waste biomass liquefaction for renewable resource utilization was pointed out, and main factors affecting liquefaction of different biomasses under different conditions were discussed, also some examples of utilization of liquefied products were illustrated in detail. The constituent characteristics of several typical liquefied products from waste biomass are analyzed. The existing problems in research and industrialization development of waste biomass liquefaction are studied, and the proposals for further investigations are suggested.
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    研究报告
    Study on Chemical Constituents of Root-bark of Cunninghamia lanceolata(Lamb.)Hook.
    LIU Chao-xiang;GAO Xue-qin;JIANG Ji-hong;FENG You-jian
    2009, 29 (1):  100-102. 
    Abstract ( 602 )   PDF (615KB) ( 789 )   Save
    To study the constituents of root-bark from Cunninghamia lanceolata(Lamb.)Hook., compounds were separated and purified by column chromatographic methods, and their structures were established by physico-chemical properties and spectral analyses. Six compounds were isolated and their structures were established as octacosan-1-ol(Ⅰ), dibutyl phthalate(Ⅱ), diisobutyl phthalate(Ⅲ), β-sitosterol(Ⅳ), β-sitosterol-3-O-β-D-glucoside(Ⅴ), kaempferol(Ⅵ). All these compounds are isolated from C.lanceolata for the first time.
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    Study on Activation of Bamboo Charcoal by KOH-microwave Method
    GAO Long-lan;LIU Yu-huan;LUO Ai-xiang;LUO Jie;RUAN Rong-sheng
    2009, 29 (1):  91-94. 
    Abstract ( 994 )   PDF (703KB) ( 744 )   Save
    The preparation of activated carbon from bamboo charcoal by fast pyrolysis using KOH-microwave irradiation method was researched. The effects of different conditions on the properties of bamboo-based activated carbon were systematically studied via orthogonal experiments. The optimum conditions were as follows: mass fraction of KOH solution 25%, impregnating time 24h, microwave power 800W and activating time 7min. Under the above conditions, iodine adsorption value of activated carbon was 1239.08mg/g, methylene blue adsorption value was 274.95mg/g, which was 2.04 times of the level specified for the first grade in GB/T 13803.2-1999 standard, and specific surface area was 1394.16m2/g. Meanwhile, FT-IR spectra of bamboo charcoal before/after activating were tested. The results showed that surface structure of bamboo charcoal was modified greatly after activation, more surface chemical functional groups were created and specific surface area and adsorption properties of bamboo charcoal were also raised.
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    Co-liquefaction of Biomass with Plastic in Sub- and Supercritical Water
    CAO Hong-ta;YUAN Xing-zhong;ZENG Guang-ming;TONG Jing-yi;LI Hui;WANG Li-hua
    2009, 29 (1):  95-99. 
    Abstract ( 746 )   PDF (914KB) ( 939 )   Save
    Co-liquefaction of biomass(sawdust and rice straw) with plastic(high density polyethylene,HDPE) in sub-and supercritical water(SCW)was investigated using a 500mL stainless-steel autoclave. A series of liquefaction experiments were carried out with biomass and plastic individually and in combination. To obtain basic knowledge about degradation of biomass and plastic into oil, the effects of reaction temperature, reaction time, ratio of water to biomass and polyethylene(PE) and degradation pressure were investigated. At 653K the maximum yield of oil was achieved. At this temperature, the most important parameter for oil yield was biomass/plastic ratio in the feedstock. Yield of oil up to 60% was obtained using 1:4 weight ratio of biomass/PE mixture. Co-liquefaction of biomass with plastic increased the yield of oils. Results showed that addition of biomass to plastic could decrease the degradation temperature of plastic to supply hydrogen, and the synergistic effects of biomass and plastic,could enhance oil yield and ease the requirement of reaction condition.
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    Spectroscopic Analysis of Cotton Stalk Lignin
    WANG Jian;WANG Yan
    2009, 29 (1):  115-119. 
    Abstract ( 624 )   PDF (751KB) ( 728 )   Save
    Milled-wood lignins from whole cotton stalk and cotton stalk core respectively were isolated and purified through ball-milling,etc.These lignins were analyzed by means of ultraviolet spectroscopy, infrared spectroscopy and 13CNMR. The results indicated that lignins of cotton stalk are of guaiacyl-syringyl-parahydroxy phenylpropane(GSH) type. There are less parahydroxy phenylpropane and more syringyl units in lignin of cotton stalk bark and more syringyl and guaiacyl units in lignin of cotton stalk core.
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    Production of 2,3-Butanediol from Fermentation of Xylose by Klebsiella oxytoca ZU-03
    FENG Yan-qing;XIA Li-ming
    2009, 29 (1):  103-106. 
    Abstract ( 541 )   PDF (668KB) ( 697 )   Save
    The production of 2,3-butanediol was carried out from fermentation of xylose by Klebsiella oxytoca ZU-03, in which xylose was the main reducing sugar in hemicellulosic hydrolysate. Under optimized conditions: xylose mass concentration 90g/L, corn liquor mass concentration 6g/L, inoculum 10% (volume fraction), initial pH value 5.5 and 30℃, concentration of 2,3-butanediol reached 36.22g/L and yield of 2,3-butanediol from xylose was 0.45g/g.
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    Effect of Aluminate Coupling Agent on Interfacial Properties of Bamboo-plastic Composites
    CHEN Qin-hui;LI Xue-fang;LIN Jin-huo
    2009, 29 (1):  83-86. 
    Abstract ( 624 )   PDF (1148KB) ( 852 )   Save
    The effect of aluminate coupling agent on interfacial properties between bamboo powder and polycaprolactone was studied in this paper. The interaction between coupling agent and bamboo powder and the best treatment time were determined by IR, XRD,etc.. The effect of coupling agent on compatability between bamboo powder and polycaprolactone was displayed by torque-rheometer and DSC. Results showed that both high-speed stirring and coupling agent destructed the ordered structure of bamboo fibre and the composite poccessed the best proccessing performance when the dosage of coupling agent was 1.6% of bamboo powder.
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    Synthesis of 3,28-Di-O-glutaryl-betulin and Analysis of Its Solubility Properties
    LÜKun;TIAN Shui-qing;FANG Gui-zhen
    2009, 29 (1):  87-90. 
    Abstract ( 698 )   PDF (792KB) ( 637 )   Save
    To improve water solubility of betulin, two acyl groups were introduced at C-3 and C-28 hydroxy groups of betulin. 3,28-di-O-glutaryl-betulin was synthesized with pyridine as solvent and DMAP as catalyst from betulin and glutaryl anhydride. Its structure was characterized by FT-IR,1HNMR and MS. Solubility data of betulin and 3,28-di-O-glutaryl-betulin in acetone, ethanol, water and phosphate-buffered saline (PBS, pH value 7.4) were determined by equilibrium method. The results showed that in acetone and ethanol, solubilities of 3,28-di-O-glutaryl-betulin were 33.52 and 22.65 times of those of betulin respectively; In water, solubility of 3,28-di-O-glutaryl-betulin was 0.0021g(100mL water), and in PBS, solubility of 3,28-di-O-glutary-betulin was 0.0015g (100mL PBS), the hydrophilicity of 3,28-di-O-glutaryl-betulin was significantly increase.
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    Study on Preparation and Properties of Cellulose-acrylic Ester Molded Plastic
    CHEN Ri-qing;JIN Li-wei;DUAN Li-yan;CHU Fu-xiang;WANG Chun-peng;QIU Mei-qin
    2009, 29 (1):  63-67. 
    Abstract ( 620 )   PDF (1354KB) ( 769 )   Save
    High-quality cellulose-acrylic ester molded plastic (CAEMP) was prepared by controlling molding temperature at 140℃, under molding pressure 39.2MPa for 12min. The effects of cellulose particle size, mold discharging agent, polymethyl methacrylate (PMMA) types and the mass ratio of cellulose to PMMA on properties of molded plastics were compared. High performance of molded plastics with 49MPa flexural strength, 2708MPa flexural modulus,1.98kJ/m2 impact strength and 0.78% water absorption was obtained under the conditions of cellulose diameter 19μm, the use of PMMA-7 powder, mass ratio of cellulose fiber to PMMA of 75:25 and the use of organosilicon as mold discharging agent.
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    Study on Chemical Constituents and Antioxidant Activity of Anthocyanins from Ipomoea batatas L.(purple sweet potato)
    ZHU Hong-mei ZHU Hong-mei;ZHAO Meng
    2009, 29 (1):  39-45. 
    Abstract ( 609 )   PDF (541KB) ( 841 )   Save
    Anthocyanins extracted from purple sweet potatoes (Ipomoea batatas L.) were purified through AB-8 resin column. The extract contains 11 kinds of anthocyanins by HPLC-DAD analysis. The majority of the anthocyanins are acylated cyanidin and peonidin. The objective of this study was to investigate the antioxidant activities of anthocyanins from purple sweet potatoes by different analytical methods: the α,α-diphenyl-β-picrylhydrazyl (DPPH) radical-scavenging effect and superoxide anions radical-scavenging effect, reducing power and antioxidant effect on lipid peroxidation in a linoleic acid model system. At a concentration of 0.5g/L, the reducing power of anthocyanins, L-ascorbic acid (L-AA) and butylated hydroxytoluene (BHT) reached 0.572, 0.460 and 0.121, respectively. The result displayed that anthocyanins possessed excellent reducing power. The fact that half inhibition concentrations (IC50) of anthocyanins scavenging DPPH radical and superoxide anions radical were 6.94 and 3.68mg/Lrespectively indicates that anthocyanins were effective in scavenging DPPH and superoxide anions radical. In addition, anthocyanins could significantly inhibit the peroxidation of lipid.
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    Homogenated Extraction of Camptothecine from Camptotheca acuminata Decne. Seeds and Leaves
    SHI Wei-guo;ZU Yuan-gang;ZHAO Chun-jian;YANG Lei;LI Jia-hui
    2009, 29 (1):  79-82. 
    Abstract ( 709 )   PDF (821KB) ( 881 )   Save
    The method of homogenated extraction and HPLC determination of camptothecine in seed and leaf of common campto-theca(Camptotheca acuminata) were studied,and comparisons of this extraction method with other methods such as ultra sonic extraction,refluxing, soaking and shaking in water bath were conducted.For the homogenated extraction,the optimum technology parameters were found as following: homogenation for 8 min with 55% ethanol at a ratio of material to liquid of 1:15 (g:mL).By using the optimized parameters,the extraction yields of camptothecine from C. acuminata seeds and leaves were 0.0801% and 0.0679%,respectively.Moreover,homogenated extraction required less extraction time and had high yield,which was an efficient method for extracting camptothecine.
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    Degradation of Milled-wood Lignin and Its Condensation with Xylose during Kraft Cooking
    SHAO Zhen-yu;XIE Yi-min;ZHOU Yan;YANG Zhi-yong
    2009, 29 (1):  29-32. 
    Abstract ( 627 )   PDF (941KB) ( 593 )   Save
    Degradation and condensation of milled-wood lignin(MWL) from Jacaranda copaia Aubl.D.Don during kraft cooking in the presence of xylose was investigated. FT-IR and 13CNMRwere used to analyze the structure of the products from kraft cooking. The results indicated that lignin linkages were cleaved easily by kraft cooking, especially α-aryl ether linkages and β-O-4 linkages. New lignin-carbohydrate complexes(LCC) structures were found simultaneously during the breaking of lignin linkages. The newly formed LCC was originated from condensation between lignin intermediates and xylose,mainly from β-O-4 and 5-5' lignin structures, which were connected with xylose through benzyl ether linkage. In addition, this newly formed LCC was very stable against alkali.
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    Study on Cyclization of Pseudoionone Catalyzed by Aluminium Chloride
    BAI Yang;LIU Liu-jun;JIANG Jian-xin;LI Jian-zhang
    2009, 29 (1):  55-58. 
    Abstract ( 620 )   PDF (736KB) ( 621 )   Save
    The Lewis acid catalyst——aluminium chloride was first used as catalyst for cyclization of pseudoionone in this study. Catalyst can effectively promote cyclization of pseudoionone. The process had characters of mild condition,simple post-processing and easy operation. The optimum conditions were determined as follows:temperature 0℃,mass ratio of AlCl3 to pseudoionone 3:4,reaction time 3h.The constituents of product were determined by GC-MS. Using AlCl3 as catalyst,pseudoionone was synthesized into β-ionone and dihydro-α-ionone.The yields of β-ionone and dihydro-α-ionone were 45.54%and 43.55%,respectively. The conversion rate of pseudoionone was 96.00%.In addition,the catalyst of high activity could be reused repeatedly. The process gives no pollution and has characters of green synthesis.
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    Study on Preparation of PVC/PEW-g-MAH/Bamboo Flour Composites
    ZHU De-qin;SHENG Yu;LIU Xi-rong;XU Yan-rong
    2009, 29 (1):  51-54. 
    Abstract ( 689 )   PDF (670KB) ( 701 )   Save
    Polyethylene wax grafted maleic anhydride (PEW-g-MAH) was applied to modify bamboo flour and the composites of poly(vinyl chloride) (PVC) filled with the modified bamboo flour were prepared. The effects of bamboo flour particle size and its dosage, grafting ratio of PEW-g-MAH and its dosage on the mechanical properties of PVC/PEW-g-MAH/bamboo flour composites were studied in detail by orthogonal-design experiments. Results show that the best condition for optimal mechanical property of PVC/PEW-g-MAH/bamboo flour composite is the following: grafting ratio of PEW-g-MAH 1.16% and its dosage 0.3g,particle size of bamboo flour 0.425mm and its dosage 30g. When modified bamboo flour was added, tensile strength and Charpy impact strength of the composite increased from respectively 28.6MPaand 3.05kJ/m2 of the composite filled with equal amount of unmodified bamboo flour to 30.01MPa and 3.86kJ/m2respectively.
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    Influences of Betulonic Acid on HepG-2 Cell and Mice Bearing H22 Tumor Cells
    ZHANG Xiu-juan;LI Guo-yuan;JI Yu-bin;FANG Gui-Zhen
    2009, 29 (1):  46-50. 
    Abstract ( 645 )   PDF (1113KB) ( 616 )   Save
    The anti-tumor effect of betulonic acid in vivo and in vitro and the preliminary mechanism of action were studied.The survival time of mice bearing H22 was used to observe the potency in vitro and the effect of betulonic acid on human hepatoma cell line(HepG-2) in vitro was studied. The morphology of H22 tumor cells treated with betulonic acid was observed by transmission electron microscopy.The effect of betulonic acid on the cell cycle was adopted by flow cytometry. The results showed that betulonic acid had certain effect on survival time of mice in vitro and HepG-2 in vitro. In the experiments of tumor transplantation in vivo, it could be observed that betulonic acid had some therapeutic effect on H22, it could significantly extend the survival time of the mice vaccinated by H22. This showed that betulonic acid also showed good tumor inhibition in vivo experiments. The values of IC50 and TC50 are 110.77 and 683.57μmol/L, respectively.The apoptosis of tumour cells can be observed by electronmicroscopy. Therefore, betulonic acid had anti-tumor effect by promoting tumor cellapoptosis.Increasing the dosage of betulonic acid, H22 cells in S phase and G2 phase gradually increased. It can be speculated that when betulonic acid acted on cells, the cells were blocked in S and G2 phases.
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    Bromination of Acrylic Rosin and Fire-retardant Property of the Product
    HUANG Huo-yang;HA Cheng-yong;MA Yi-jing;SHEN Min-min;LI Yin-wen;
    2009, 29 (1):  59-62. 
    Abstract ( 738 )   PDF (772KB) ( 639 )   Save
    Bromination of acrylic rosin with bromine was carried out. The influences of reaction parameters were discussed respectively, such as reaction temperature, mole ratio of material, reaction time etc.. FT-IR,1HNMR and TG of the brominated acrylic rosin were discussed. The result showed that, reaction temperature -2-4℃, reaction time 5-6h and mole ratio of material 1.2:1(Br:rosin), the product yield could be up to 93%. Brominated acrylic rosin had not only better fire-retardant property, but also widened the application of rosin and increased its worth.
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    Preparation of Bamboo Charcoal-ZnO Composite and Its Effect on Photocatalytic Degradation of Phenol
    ZHANG Li-min;CHEN Qing-song;LI Xiao-yan;DING Fu-chuan
    2009, 29 (1):  33-38. 
    Abstract ( 574 )   PDF (1454KB) ( 684 )   Save
    Bamboo charcoal-ZnO composite was prepared via dipping method by using sodium silicate as binder. The bamboo charcoal-ZnO composite was characterized by FT-IR and scanning electron microscopy (SEM), and the removal effects of the composite for photocatalytic degradation of phenol in aqueous solution were investigated. The experimental results showed that in the preparing process of composite the optimum mass ratio of bamboo charcoal-ZnO-Na2SiO3·9H2O was 5:2:1. It was favorable to the removal of phenol in acidic aqueous solution and when H2O2 was added. Under optimum condition of phenol concentration 50mg/L, composite mass concentration 2g/L and H2O2 concentration 1.95mmol/L, reaction time 4h under UV and sunlight irradiations respectively, the phenol removal rates were 92.3% and 76.4%, respectively. The phenol removal rate of the composite after reused for three times could still reach more than 80%.
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    Study on Preparation of β-Glucosidase and Its Application in Enzymatic Hydrolysis of Cellulose
    QU Li-li;ZHU Jun-jun;LIU Min;YONG Qiang;YU Shi-yuan
    2009, 29 (1):  13-17. 
    Abstract ( 563 )   PDF (992KB) ( 995 )   Save
    Preparation of β-glucosidase by solid-state fermentation and its application in enzymatic hydrolysis of cellulose were investigated. The maximal β-glucosidase activity was 225.43IU/g dry base (based on koji) when Aspergillus niger NL02 was employed using corn cob and wheat bran as carbon sources for 5 days cultivation. β-Glucosidase was purified to homogeneity by ammonium sulfate precipitation, anion-exchange chromatography and gel filtration chromatography. The recovery of enzyme acti-vity and specific activity were 69.34% and 133.88IU/mg, respectively. Corn stalk pretreated by dilute sulfuric acid was hydrolyzed by the dosages of 20FPIU/g (based on cellulose) Trichoderma reesei cellulase and 4IU/g(based on cellulose) β-glucosidase at the substrate concentration of 100g/L for 48h, the concentration of cellobiose and glucose in hydrolysate were 1.12 and 42.68g/L, respectively, the yield of enzymatic hydrolysis and the ratio of fermentable sugar were 62.85% and 97.44%, respectively.
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    Study on Co-polymerization of Coniferin with Model Compound of Lignin
    ZHAO Fang;XIE Yi-min;WANG Song;WANG Peng
    2009, 29 (1):  1-6. 
    Abstract ( 659 )   PDF (1525KB) ( 789 )   Save
    In order to explore the mechanism of polymerization between lignin from effluent of pulping process and lignin precursors, the method and mechanism of co-polymerization of coniferin with model compound of β-O-4 type lignin were investigated. The characteristics of polymerization product were analyzed by FT-IR, 13CNMRand gel permeation chromatography(GPC). Polarized microscopy was applied to observe the products. Moreover, GPC was used to determine mumber-average molecular mass (Mn) of the polymerization product. The results showed that coniferin could completely polymerize with model compound of β-O-4 type lignin to form lignin macromolecule. The Mn of the polymerized product was much higher than the starting materials. There was no crystalline starting material in the obtained polymer. These results could be the basis of waste-water treatment using coniferin and enzymes.
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    Kinetics of Curing Reaction of Novolak-type Phenol Formaldehyde Resin from Phenolated Wood
    LI Gai-yun;QIN Te-fu;REN Hai-qing;JIANG Ze-hui
    2009, 29 (1):  7-12. 
    Abstract ( 563 )   PDF (1363KB) ( 808 )   Save
    The curing behaviors and kinetics of novolak-type phenolic resin from phenolated wood (PWF) were investigated with DSC. Thermal degradation properties and structure of cured PWF were analyzed by means of TG and FTIR, respectively. The curing reaction of PWF was compared with that of traditional novolak-type phenol formaldehyde resin (PF). The results showed that the amount of curing agent——hexamethylene tetramine (HMTA) had great influence on curing of PWF. When the mass ratio of HMTA and resin was 100:10, apparent activation energy of curing reaction of PWF was 107.76kJ/mol, which was lower than 141.35kJ/mol of PF. There was little effect of curing agent content on the order of curing reaction of PWF, and the order of PWF curing reaction was constantly 0.95, the same as PF's. Curing temperature of PWF was from 135 to 137℃ by extrapolating Tp-β. TG curve of cured PWF followed the similar trend as that of cured PF during the range of 30 to 291℃. Both were thermal stable and had no weight loss before 200℃ and they began to loss weight with further increasing of temperature. The temperatures of thermal degradation of cured PWF and PF were 291 and 296℃, respectively. The structure of cured PWF was nearly similar to that of cured PF confirmed by IR.
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    Study on Synthesis and Crystalline Structure of Substituted Benzylidene-3,4,5-trimethoxybenzohydrazide
    WANG Yu-min;ZHAO Zhen-dong;BI Liang-wu;LI Dong-mei
    2009, 29 (1):  23-28. 
    Abstract ( 574 )   PDF (919KB) ( 673 )   Save
    Three titled compounds namely (E)-N'-(2-hydroxybenzylidene)-3,4,5-trimethoxybenzohydrazide (1), (E)-N'- (5-bromo-2-hydroxybenzylidene)-3,4,5-trimethoxybenzohydrazide (2) and (E)-N'-(4-cholobenzylidene)-3,4,5- trimethoxybenzohydrazide (3) have been synthesized, and characterized by IR and 1HNMR.Their crystalline and molecular structures have been determined by single crystal X-ray diffraction. Both compounds 1 and 2 belong to monoclinic system, space group P2(1)/c, with a=1.5348(12)nm, b=1.3330(11)nm, c=0.8299(7)nm,α=90.00°,β=99.854(16)°,γ=90.00°, V=1.6730(2)nm3, Z=4, Dc=1.312g/cm3,F(000)=696,R=0.1016, wR=0.1936, for compound 1; a=1.14157(19)nm, b=1.6279(3)nm, c=0.9738(16)nm,α=90.00°, β=100.210(16)°,γ=90.00°,V=1.7144(4)nm3,Z=4, Dc=1.586g/cm3, F(000)=832,R=0.0669,wR=0.0969 for compound 2. Compound 3 belongs to triclinic system, space group P-1, with a=0.5119(2)nm, b=0.8210(4)nm, c=2.0276(9)nm, α=101.055(7)°,β=92.362(7)°,γ=101.459(7)°, V=0.8169(7)nm3,Z=2, Dc=1.418g/cm3,F(000)=364, R=0.0516, wR=0.1276. In the crystals there exist several intermolecular hydrogen bonds, through which one-dimensional infinite-chain structures were formed.
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