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    28 August 2014, Volume 34 Issue 4 Previous Issue    Next Issue
    Interaction during the Pyrolysis Process of Cellulose and Hemicellulose
    HU Yi-ming, JIANG Jian-chun, SUN Yun-juan, YANG Zhong-zhi
    2014, 34 (4):  1-8.  doi: 10.3969/j.issn.0253-2417.2014.04.001
    Abstract ( 935 )   PDF (2363KB) ( 1310 )   Save
    Simultaneous thermal analyzer (STA) and Thermogravimetric analyzer coupled with a Fourier transform infrared spectroscopy (TG-FT-IR) were used to investigate the pyrolysis characteristics of microcrystalline cellulose(MCC), xylan and their mixtures. The results showed that both MCC and xylan were fast pyrolysis in a narrow temperature ranges with separated pyrolysis ranges. An obvious endothermic peak has been observed from MCC pyrolysis. The temperature area was corresponded to the peak of DTG curve and the absorbed heat was indicated as 547.98 J/g. When xylan was pyrolyzed, there was a small endothermic peak in DSC curve later than DTG peak. This indicated the absorbed heat was 45.01 J/g. There are two weight loss peaks found in different ratios of xylan and MCC mixture. They were induced by MCC and xylan respectively. These two weight loss peaks were inversely proportional according to the ratio of the two conponents. There are two independent endothermic peaks existing in DSC curve, which are caused by pyrolysis reaction of xylan and MCC. The peak of xylan did not influence by ratio of xylan, but the peak of MCC decreases largely with the ratio of MCC decreasing either in DTG or in DSC curves. In addition, the peaks of MCC are shifting to higher temperature. The FT-IR observed that H2O、CH4、CO2 and CO are the mainly gas products from biomass components and mixed components pyrolysis. During xylan-MCC mixtures pyrolysis, the products released from pyrolysis reaction is approximately sum of the pyrolysis reaction of xylan and MCC pyrolysis individually. it was found that pyrolysis of mixture has benefit to generate CH4 and CO, while CO2 yield decreases drastically at the same time.
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    Adsorption Performance of Heavy Metal Ions by Fir Bark and Its Kinetic
    SU Wen-peng, YANG Yi-qin, JIANG Ling-yu, ZHOU Hao, ZHOU Yong-hong
    2014, 34 (4):  9-15.  doi: 10.3969/j.issn.0253-2417.2014.04.002
    Abstract ( 736 )   PDF (1791KB) ( 873 )   Save
    The adsorption of copper, lead and cadmium ions (heavy metal ions, HMI) from aqueous solution by the powder of fir bark was investigated by using batch techniques.The effects of pH value, contact time and initial metal ions concentration and particle size of fir bark powder on the metal ions adsorption capacity have been studied. Fir bark was found to be a low cost and promising adsorbent for absorbing heavy metal ions from aqueous solution. The results showed that the suitable size of bark powder used as adsorbent is 250-830 μm. Under the condition with pH of 5.0 and a contact time of 30 min, 0.6 g bark powder in 100 mL initial ions concentration of 150 mg/L resulted in the maximum adsorption capacity of 6.83, 13.56 and 23.17 mg/g for Cu2+, Cd2+ and Pb2+, respectively. Kinetics fitted with Lagergren pseudo second-order models. Hence adsorption kinetic parameters were calculated, and the correlation coefficient R2>0.997 was obtained. The adsorption data of metal ions at 45℃ has been described by the Freundlich and Langmuir isothermal absorption models, and Langmuir isothermal adsorption model was more satisfied. Ion exchange was probably one of the major adsorption mechanisms for binding divalent metal ions to the bark powder. From these results, it can be concluded that the powder of the fir bark could be a good adsorbent for extracting the metal ions from aqueous solution.
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    Comparation on UV Curing Reactivity of Allyl Abietate and Allyl Isopimarate
    LU Yan-ju, ZHAO Zhen-dong, CHEN Yu-xiang, BI Liang-wu, LI Dong-mei, WANG Jing
    2014, 34 (4):  16-20.  doi: 10.3969/j.issn.0253-2417.2014.04.003
    Abstract ( 721 )   PDF (1393KB) ( 679 )   Save
    The UV curing reaction of the difference between allyl abietate(AA) and allyl isopimarate(AI) was studied. The conversion rate of the vinyl double bond was characterized and detected by FT-IR analysis. Results showed that conversion of double bonds are firstly increased then decreased with the increases of the dosage of initiators. Conversion of double bonds firstly increased and then leveling off with the increases of the illumination time, and AA is higher before the 200 s. AA is higher then AI under the same illumination intensity. Surface drying time of AA is shorter than AI, and relative curing speed become faster at the same conditions. Under the conditions of 2-hydroxy-2-methylpropiophenone(Darocure-1173)as photo initiator and dosage 6%,illumination time 200 s,illumination distance 4.5 cm and illumination intensity 100%,number average molecular weight of cure products of AA and AI are 4 176 and 9 407 with polymerisation degrees of 12 and 28, respectively. The obtained UV cured coating all have smooth and transparent appearance. It represented some superior properties in flexibility, mechanical impact strength, adhesive power, hardness, acid resistance, alkali resistance, salt resistance, water resistance, etc.. The hardness of AA and AI cured products are H and HB, respectively.
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    A New Synthetic Method of 2,3,4,4’-Tetrahydroxybenzophenone by Boron Trifluoride Catalysis
    OUYANG Wen, CAO Yong, CHEN Xue-xiang, DU Fang-lu
    2014, 34 (4):  21-24.  doi: 10.3969/j.issn.0253-2417.2014.04.004
    Abstract ( 776 )   PDF (1078KB) ( 677 )   Save
    A new synthesis of 2,3,4,4'-tetrahydroxybenzophenone by boron trifluoride etherate catalysis was proposed in this paper. In the new method, high boiling-point petroleum ether was used as the reaction solvent to replace the poisonous and expensive 1,1,2,2-tetrachloroethane. Although p-hydroxybenzoic acid, pyrogallic acid, boron trifluoride and petroleum ether were immiscible at room temperature, the reaction system could be gradually turned into brown oily solution in the heating and rapid mixing conditions. After a period of time, a large amount of yellow crystalline products were precipitated. According to the results of orthogonal experiments, the optimum reaction conditions were as follows:pyrogallic acid 0.05 mol, p-hydroxybenzoic acid 0.055 mol, catalyst 0.16 mol (20 mL), reaction temperature 110℃ and reaction time 1 h. Under this condition, the yield reached 83.24% and product purity 97.83%. The new method possessed many advantages, e.g., low toxicity, low cost, short reaction time, easy operation and the recycled catalyst. The product with 99.53% purity by recrystallization in water was identified as 2,3,4,4'-tetrahydroxybenzophenone by the combination of IR, NMR and EI-MS techniques.
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    Promotion of in Situ Enzymatic Degradation on Natural Plant Fiber by Ionic Liquid
    LIU Xian-hong, LI Lu, YU Shi-tao, LIU Shi-wei, LIU Fu-sheng, XIE Cong-xia
    2014, 34 (4):  25-29.  doi: 10.3969/j.issn.0253-2417.2014.04.005
    Abstract ( 684 )   PDF (1785KB) ( 657 )   Save
    An ionic liquid, i.e., 1-ethyl-3-methylimidazolium ([EMIM] OAc), was used to treat two natural plant fiber (Salix psammophila and cotton). The effects of this pretreatment on the enzymatic degradation of these two materials were investigated in present study. The optimum condition for degradation was obtained as 3.64 mL pH 5 citric acid-sodium citrate buffer solution was added to 5g 4% natural plant fiber[EMIM] OAc solution. A reaction system with 55 g/L fiber substrate was obtained. The optimal ratio of enzyme to substrate was 0.5:1(mL:g), and the optimal reaction temperature and reaction time were 55℃ and 25 h, respectively. Under the optimal condition, the enzymatic degradation of the two natural plant fiber was beyond 90%. The FT-IR showed that the hydrogen bondings of fiber were broken by [EMIM] OAc in the process of dissolution. It resulted in a fiber material with more amorphous pattern. These changes would increase the accessibility between fiber and cellulase. This led to more enzymatic degradation of cellulose.
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    Effects of Combination of Thermo-mechanical and Liquid Hot Water Pretreatment on the Efficiency of the Enzymatic Hydrolysis of Eucalyptus and Its Process Optimization
    XU Shao-hua, WU Shu-bin, LI Xiao-hong
    2014, 34 (4):  30-36.  doi: 10.3969/j.issn.0253-2417.2014.04.006
    Abstract ( 714 )   PDF (3202KB) ( 693 )   Save
    Combination of thermo-mechanical pulping (TMP) process and liquid hot water pretreatment method had been adopted to improve the enzymatic saccharification efficiency and reduce the processing costs of eucalyptus. The pretreated sample was then hydrolyzed by cellulase. The pretreatment conditions on the influence of sugars yield had been discussed by measuring the yield of xylose and glucose in the pretreated hydrolyzate and enzymatic hydrolyzate. The optimal pretreatment condition was 180℃(cooking temperature), 40 min(residence time) and 5%(substrate concentration). It was obtained by using the total sugars in the pretreated hydrolyzate and enzymatic hydrolyzate as the evaluation index. Under this pretreatment condition, the conversion of xylose and glucose reached 82.70% and 78.90%, respectively. The physics and chemical properties of pretreated residue were characterized using FT-IR, SEM so as to analyse effect of two pretreatment methods. The results showed that the particle of raw eucalyptus was diminished, the shape was filiform, but the fibre morphology was maintained. However, the structure of fibre was loose and smashed after the hot water pretreatment, and this improved the accessibility of cellulase and efficiency of enzymolysis.
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    Optimization of the HPLC Condition of Ursolic Acid and Oleanolic Acid by Central Composite Design
    XING Ya-li, BI Liang-wu, ZHAO Zhen-dong, HAN Lu-lu, XIA Tian-juan
    2014, 34 (4):  37-41.  doi: 10.3969/j.issn.0253-2417.2014.04.007
    Abstract ( 828 )   PDF (1380KB) ( 685 )   Save
    Effects of HPLC mobile phase and column on the separation and determination of ursolic acid and oleanolic acid were in vestigated. By using the resolution and the analysis time as response values, the main influencing factors of HPLC(the volumetric ratio of methanol and aqueous phase in the mobile phase, the volume fraction of phosphoric acid in the aqueous phase, as well as the flow rate of the mobile phase and the column temperature) were optimized by central composite design. An effective and fast method for the separation and determination of ursolic acid and oleanolic acid by HPLC was established. The results showed that oleanolic acid and ursolic acid were effectively separated within 23 min with the resolution of 1.739, when the chromatographic separation was performed on a Shim-pack ODS-CLC (M) column kept at 21℃, using the methanol and aqueous phase containing 0.05% phosphoric acid with the volumetric ratio of 91.7:8.3 as the mobile phase at a flow rate of 0.6 mL/min, and the detection wavelength was set at 210 nm.
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    Synthesis and Property of Dimethyl-butyl-sulfonated Lignin Ammonium Chloride
    TIAN Jin-ling, REN Shi-xue, FANG Gui-zhen, AI Qing
    2014, 34 (4):  42-50.  doi: 10.3969/j.issn.0253-2417.2014.04.008
    Abstract ( 692 )   PDF (2587KB) ( 793 )   Save
    Dimethyl-butyl-sulfonated lignin ammonium chloride (DBSLAC) amphoteric surfactant was synthesized through Mannich and Sulfonating reaction using wheat straw alkali lignin as a raw material. Its structure was characterized by FT-IR, and the solubility in different pH solutions was evaluated. The effects of dimethyl-butyl-sulfonated lignin ammonium chloride on the adsorption performance was investigated with copper ions as simulate wastewater, while its flocculation performance was investigated with acid black ATT and methylene blue wastewater as the simulation dyes. The results showed that sulfonic group and quaternary amine group were successfully grafed, and nitrogen content of DBSLAC was 2.34%. DBSLAC amphoteric surfactant on the adsorption isotherms of copper ions could be fitted well by Freundlich equation, when the optimum adsorption conditions for Cu2+ were the dosage of 0.002 g(the initial mass concentration of Cu2+ 100 mg/L, solution volume 20 mL), pH 5.5 and adsorption time of 2 h. Under this condition, the maximum adsorption capacity was 262.34 mg/g. The maximum removal rate of 20 mL Acid black ATT (anionic dye) was 75.41% when the optimum flocculation conditions were the dosage of 0.03 g, pH 2 and mass concentration of dye of 0.1 g/L. The maximum removal rate of 20 mL methylene blue (cationic dye) was 97.87%, when the optimum flocculation conditions were the dosage of 0.3 g, pH 9 and mass concentration of dye of 0.1 g/L. The result shows that DBSLAC amphoteric surfactant will be expected to a novel adsorbent for heavy metal ion and flocculants of dyes.
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    Removal of Ca2+ from Papermaking Whitewater by Polyampholyte P (DMDAAC-AM-AA)
    SUN Xuan, DAI Hong-qi, QIAN Hui-wen, MAO Sheng-tao, WANG Jing-jing
    2014, 34 (4):  51-58.  doi: 10.3969/j.issn.0253-2417.2014.04.009
    Abstract ( 695 )   PDF (2369KB) ( 632 )   Save
    A polyamoholyte, P(DMDAAC-AM-AA) which was composed of acrylamide (AM), acrylic acid (AA) and dimethyl diallyl ammonium chloride (DMDAAC) was prepared in the lab. Its property, mechanism and affecting factors for Ca2+ adsorption from papermaking whitewater were studied. The results indicated that, alkaline environment was beneficial to the adsorption process under the optimum pH range 9 to 11. Besides, along with the increasing of the initial concentration of Ca2+, the adsorption increased firstly and then leveled off, and the optimum molecular weight range was 600 000 to 800 000. Moreover, the adsorption kinetic curve of Ca2+ was represented as a chemisorption process and was quite fit for Lagrange pseudo-second-order model. The adsorption isotherm was accordance with a Langmuir model. It was a monomolecular layer and easy adsorption process. The values of RL at different temperatures were below 0.5. Besides, the adsorption of P(DMDAAC-AM-AA) onto fibers was characterized by FT-IR. The adsorption equilibrium was achieved at 60min as the whitewater was stirred at 120 r/min and 20-30℃, and the equilibrium absorption capacity was ca.2.4 mg/g oven dry fiber. The adsorption of the polymers on the fiber surface was confirmed by the FT-IR analysis.
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    Purification of Anthocyanin in Blueberry by Macroporous Resin
    ZHENG Hong-yan, YU Hua-zhong, LIU Jian-lan, GAO Meng, LIU Tong-fang, CHEN Yan-mei
    2014, 34 (4):  59-65.  doi: 10.3969/j.issn.0253-2417.2014.04.010
    Abstract ( 897 )   PDF (1958KB) ( 624 )   Save
    With extracts of blueberry as material, purification of anthocyanin in blueberry by macroporous resins was studied in this paper. The absorption capacity and desorption effect of 12 kinds of macroporous, and the static optimum resin adsorption isotherms for five kinds of macroporous resin which is better on anthocyanin separation effect was investigated. The processing parameters were optimized based on the adsorption and desorption results. The results indicated that XDA-7 resin had best efficacy in separating and purifying the anthocyanins from blueberry. The optimum conditions of adsorption process were pH 3.0, mass concentration 0.94 g/L and flow rate 30 mL/h (2 bed volume). The maximum adsorption capacity is 15.41 g/L wet resin. The optimum elution conditions were room temperature, pH 3.0, velocity of 80% methanol taken as eluent 60 mL/h, and volume of 80% methanol 75 mL. The optimum desorption rate is 92.65%. The anthocyanin produced by this technological process was purplish dark powder after freeze-drying, and the yield of anthocyanin was 70.2%. The anthocyanin's purity increased from 2.20% to 24.54%, and the color value was 121.
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    Synthesis of Castor Oil-based Flame Retardant Polyols and Its Applicaition in Polyurethane Foams
    ZHANG Li-qiang, ZHANG Meng, ZHOU Yong-hong, HU Li-hong, YANG Xiao-hui
    2014, 34 (4):  66-70.  doi: 10.3969/j.issn.0253-2417.2014.04.011
    Abstract ( 1184 )   PDF (1462KB) ( 853 )   Save
    In this paper, castor oil-based flame retardant polyols were synthesized using castor oil as raw material pretreated through glycerol alcoholysis, hydrogen peroxide epoxidation and ring-opening reaction between diethyl phosphate and epoxy group. The castor oil-based flame retardant polyols were than reacted with MDI to produce polyurethane foam (PUF). The structure of castor oil-based flame retardant polyols was characterized by FT-IR and 1H NMR. The mechanical behavior and flame resistance of PUF was studied by universal testing machine and limiting oxygen index (LOI) and thermogravimetric analysis, respectively. The results showed that the castor oil-based flame retardant polyols were prepared by a series of reactions and the hydroxyl value was increased to 420 mg/g. The value of PUF's LOI could reach about 23.8% from 20.1% compared with PUF prepared by alcoholisis castor oil, although the content of phosphorus in PUF is merely 1% and without any fire retardant. The compressive strength of polyurethane foam is increased from 0.118 MPa to 0.128 MPa and thermal stability of polyurethane foam increase with castor oil-based flame retardant polyols content increasing.
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    Chemical Constituents of Ginkgo Biloba L. Leaves Lipids
    TAO Ran, WANG Cheng-zhang, KONG Zhen-wu
    2014, 34 (4):  71-76.  doi: 10.3969/j.issn.0253-2417.2014.04.012
    Abstract ( 809 )   PDF (1398KB) ( 645 )   Save
    In this paper, lipids separated from Ginkgo biloba leaves were prepared by extraction with solvent and saponification. Fifteen known compounds were separated from Ginkgo biloba leaves by molecular distillation and chromatographic isolation. They were identified by physical and chemical properties and spectral data. The isolated compounds are β-sitosterol acetate, ethylpalmitate, β-sitostero1, stigmasterol, ergosterol, palmitamide, glycerol tripalmtate, daucosterol, hendecane, β-caryophyllene, isophytol, nerolidol, linalool, terpineol and β-carotene, respectively. The separated and identified compounds, i.e., palmitamide, glycerol tripalmtate, hendecane, β-caryophyllene and terpineol,are reported for the first time in Ginkgo biloba leaves.
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    Preparation of N-doped Activated Carbon and Effects of N-doping on Formaldehyde Adsorption
    SUN Kang, JIANG Jian-chun, LU Xin-cheng, CHEN Chao, JIA Yu-jie
    2014, 34 (4):  77-82.  doi: 10.3969/j.issn.0253-2417.2014.04.013
    Abstract ( 871 )   PDF (2018KB) ( 677 )   Save
    Aniline (An) as nitrogen source, N-doped activated carbon was prepared by in-situ polymerization and carbonization. Effects of added aniline on pore structure, external nitrogen-containing groups and formaldehyde equilibrium adsorption capacity of the modified activated carbon (AC) were investigated. Results showed that N-doping activated carbon (AC2) prepared by the mass ratio of mAn:mAC with 10:2 had very high gas adsorption capacity. The sample AC2 has nitrogen content of 2.05%, and its total pore volume and mesoporous volume decrease, whereas microporous volume increases slightly. AC2 has gotten formaldehyde equilibrium adsorption capacity 379 mg/g, which is 3-6 times high than commercial activated carbon and bamboo charcoal. Doping element N on the surface of activated carbon can increase the electron cloud density around the porosity and the attractiveness of carbonyl carbocation from formaldehyde. The present modification method is a promising convenient way to obtain the N-doped activated carbon with high removal capacity of formaldehyde.
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    Pyrolysis Characteristics of Main Organic Components in Eucalypt APMP Pulping Spent Liquor
    LI Xiao-hong, WU Shu-bin, ZHAO Yu-shuang
    2014, 34 (4):  83-89.  doi: 10.3969/j.issn.0253-2417.2014.04.014
    Abstract ( 718 )   PDF (2807KB) ( 649 )   Save
    The eucalypt alkaline peroxide mechanical pulp (APMP) spent liquor solid (ASLS) and its three major organic components, i.e., alkali lignin(AL), polysaccharide(PLS) and lignin-carbohydrate complexes(LCC), were rapidly pyrolyzed at the temperature from 400℃ to 800℃ through a tubular furnace. The composition and distribution of the pyrolysis products were determined by gas chromatography (GC), gas chromatography coupled with mass spectrometry (GC/MS), Fourier transforms infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM), respectively. It was found that AL showed a significant effect on the yield of liquid products while PLS exhibited a remarkable influence on the yield of solid and gas products as ASLS was pyrolyzed. The yield of H2 was as high as ASLS was pyrolyzed. It indicated no relation with the contents of AL, LCC and PLS. A large amount of CO was generated as PLS was pyrolyzed at high temperature. In contrast to ASLS, LCC and PLS, more hydrocarbon was generated as AL was pyrolyzed. Aromatics of ASLS pyrolysis liquid products were mainly from AL. And the pyrolysis of AL and LCC should be responsible for the generation of phenols and PAHs. Ketones, furans and acids were attributed to the pyrolysis of AL, LCC and PLS. The surface morphologies of ASLS, AL, LCC and PLS pyrolysis char were significantly different.
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    Surface Chemical Structure of Alkali Lignin Modified by the Synergistic Process of Laccase and Ultrasound
    LIAN Hai-lan, CHENG Ming-juan, HONG Shu, ZHAN Xian-xu
    2014, 34 (4):  90-96.  doi: 10.3969/j.issn.0253-2417.2014.04.015
    Abstract ( 846 )   PDF (3590KB) ( 671 )   Save
    Wheat alkali lignin was treated by ultrasound, laccase, and the synergistic process of ultrasound and lassase, respectively. The chemical structure of wheat alkali lignin after treatment was then characterized by the content of phenolic hydroxyl, infrared spectroscopy, X-ray photoelectron spectroscopy (XPS) and electron spin resonance (ESR). The result showed that comparing with the untreated lignin, the total phenolic hydroxyl content increased after ultrasonic treatment. However, it decreased after laccase treatment. The number of spin decreased by 38% after ultrasonic treatment, but it increased significantly after laccase treatment. Particularly, the number of spin increased by 112% after the single treatment by laccase. Then ultrasonic wave and laccase were applied to treat the sample in sequence. This resulted in the increase of the number of spin by 193%. In these cases, ultrasonic cavitation can induce the demethylation and cleavage of some linkages in lignin. Laccase was able to promote depolymerization. At the same time, phenolic hydroxyl in lignin was oxidized and generated phenoxy radicals for free radical polymerization during the process of laccase-catalyzed oxidation. Small molecule lignin obtained after ultrasonic treatment was prone to react with laccase and C-O was oxidated in this case.
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    Analysis and Determination of Nutrient Compositions of Olive Leaves
    XIE Pu-jun, HUANG Li-xin, ZHANG Cai-hong, YOU Feng, ZHANG Yao-lei
    2014, 34 (4):  97-101.  doi: 10.3969/j.issn.0253-2417.2014.04.016
    Abstract ( 732 )   PDF (1458KB) ( 635 )   Save
    The aim of this work is to analyze and determine nutrient compositions, i.e., fat-soluble ingredient, mineral elements, crude protein, crude fiber and amino acid (AA) in Frantoio olive leaves (OL). GC-MS, ICP-AES, Dumas combustion and ion chromatography-integrated pulsed amperometric detection were used to detect the nutrient ingredients. The results showed that crude fat content was 3.0%, which esters accounted for 26.81%, fat acid 18.46%, 1-nonadecene and squalene 1.62%, (Z)-9-octade cenamide 2.00%, vitamin E 2.68%, theobromine 6.88%, (Z)-9,17-octadecadienoic aldehyde 5.53% in its total volatile compositions. The ash content of OL was 4.9%. Among them, Ca content was the most with 30.5% in the ash, and followed by K, Mg and P. Meanwhile, it did't have toxic heavy metal elements, e.g., As, Hg and Pb. The protein and fiber content of olive leaves was 11.46% and 15.8%, respectively. It was also found that AA was rich in OL and the total AA was 0.991% in dry matter of OL. Especially, it was rich in glycine, histidine and valine, and short of arginine. Therefore, OL is possible to be made as animal fodder after some treatments due to its rich nutrient compositons.
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    Synthesis and Characterization of Isobornyl Acrylate Modified Waterborne Polyurethane
    XU Xu, XU Xiao-wei, XING Ying-ying, WANG Shi-fa
    2014, 34 (4):  102-106.  doi: 10.3969/j.issn.0253-2417.2014.04.017
    Abstract ( 910 )   PDF (7735KB) ( 503 )   Save
    The composite emulsion of waterborne polyurethane (WPU) modified by isobornyl acrylate (IBOA) was prepared by emulsion polymerization method. The effects of the dosage of initiator, mass ratio of IBOA to WPU, reaction temperature and holding time on the mass ratio of solid content, monomer conversion rate, water absorption and tensile strength of film were investigated. The optimum conditions were obtained by orthogonal test. Eventually, it was determined that the best preparation conditions of WPU modified by acrylate (WPUA) were: m(IBOA):m(WPU)=1:3, 0.5% APS as the initiator (based on the mass of monomer), reaction temperature 80℃ and holding time 3 h. The chemical structure, mechanical property, water resistance, and other properties of the composite were characterized by FT-IR, TEM and TG, respectively. The structure- property relationship was also discussed. It showed that the average monomer conversion was 97.35%, the average water absorption of WPU modified by IBOA was 5.94%, and its average tensile strength was 27.17 MPa. Moreover, the morphology of emulsion was core-shell structure, and its stability was good. Thermal degradation of the film was caused by two stages including hard segments degradation and soft segments degradation, respectively.
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    Extraction and Purification of Flavonoids from Poplar Buds with Subcritical Water Extraction Coordinated with Macroporous Resin Adsorption
    BO Cai-ying, ZHENG Guang-yao, GAO Li-ping, ZHANG Jian-hua, DAI Hai-jing
    2014, 34 (4):  107-112.  doi: 10.3969/j.issn.0253-2417.2014.04.018
    Abstract ( 772 )   PDF (5859KB) ( 693 )   Save
    Subcritical water extraction coupled with macroporous adsorption resin technology was applied to extract and purify flavonoids from poplar buds. Based on the yield of flavonoids, the factors of extraction technology including extraction temperature, liquid-feed ratio was optimized through orthogonal tests. By comparison of four macroporous resins in the adsorption of flavonoids, the optimal macroporous of resin was selected, then adsorption and desorption effects were investigated. The results showed that the optimum process of subcritical water extraction were extraction temperature 180℃, liquid-feed ratio 30:1, extraction time 10 min. The yield of crude flavonoids was 11.83% and the purity of the product is 13.16%. The HP-20 macroporous adsorption resin was selected to separate and purify flavonoids from poplar buds. The optimal technological conditions were solution concentration 4 g/L, flow rate 60 mL/h, solution pH 2-3, and eluting solvent 90% ethanol. The purity of flavonoids can reach 49.28%.
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    The Preparation of Urushiol Acetal from Lacquer Sap and Its Hydrogenation Process Mechanism
    HE Yuan-feng, LU li, WANG Cheng-zhang, YANG Zhi-bin, ZHOU Hao, CHEN Hong-xia, YE Jian-zhong
    2014, 34 (4):  113-117.  doi: 10.3969/j.issn.0253-2417.2014.04.019
    Abstract ( 764 )   PDF (1688KB) ( 701 )   Save
    Urushiol acetal was prepared from the acetone extracted lacquer sap by acetalation which decreased the polarity of urushiol. Thus it is easy to be separated from dimmer and oglimer of urushiol. The tri-unsaturated urushiol were obtained through silica gel column. The rushiol acetal products were analysed by IR and NMR. IR absorptance at 3100-3650 cm-1 indicates phenol to disappear while ether 1049 cm-1 was found after acetalation. The absorption of 5.92 in 1H NMR represents methylene ether group in rushiol acetal. The tri-unsaturated urushiol acetal was hydrogenised. Its hydrogenation process was detected by HPLC. It was found that tri-unsaturated urushiol acetal gradually became di-unsaturate and mono-unsaturate, and turned into saturate state after 8 h.
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    A New Benzophenone from Ranunculus ternatus
    DENG Ke-zhong DENG Ke-zhong, LUO Yong-ming, ZHOU Bin, CHEN Hong, XIONG Ying
    2014, 34 (4):  118-120.  doi: 10.3969/j.issn.0253-2417.2014.04.020
    Abstract ( 641 )   PDF (562KB) ( 642 )   Save
    A new benzophenone, i.e. (R)-3-(2-(3,4-dihydroxybenzoyl)-4,5-dihydroxyphenyl)-2-hydroxypropanoic acid, was isolated from the roots of Ranunculus ternatus by alcoholic extraction, silica gel, ODS column chromatography and PHPLC. Its structure was elucidated by HRESI MS, 1H NMR, 13C NMR, HMBC and CD. This compound is a new benzophenone which has not been reported before, and named as ternatic acid.
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    Effect of Different Dyes on Rattan and Its Dyeing Mechanism
    WANG Chuan-gui, PEI Yun-wen, ZHANG Shuang-yan, WANG Xiang, CHEN Mei-ling
    2014, 34 (4):  121-125.  doi: 10.3969/j.issn.0253-2417.2014.04.021
    Abstract ( 610 )   PDF (1361KB) ( 577 )   Save
    Calamus simplicifolius and Daemonorops margaritae are dyed with 8 kinds of dyes. Analyzsis of influence of different structure dyes on dye uptake with two kinds of rattan.The result shows that acid scarlet-GR is the biggest permeability of dye on C.simplicifolius and D.margaritae. The -SO3- of its -SO3H and hydrophilic group of wood fiber compounded covalent bond with hydrogen bond and VDW. The influence of different structure of the dye penetration on C.simplicifolius has the order of acidic dye > reactive dye > direct dye > alkaline dye;it's reactive dye > acidic dye > direct dye > alkaline with D.margaritae.
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    Chemical Constituents in the Fruit of Rosa davurica Pall.
    ZHONG Fang-li, WANG Xiao-lin, XUE Jian-fei, CHEN Shuai
    2014, 34 (4):  126-130.  doi: 10.3969/j.issn.0253-2417.2014.04.022
    Abstract ( 728 )   PDF (1142KB) ( 809 )   Save
    The chemical constituents in the fruit of Rosa davurica Pall. were studied. The silica gel column and thin layer chromatography methods were applied to isolate and purify the fruit of R.davurica cultivated in Jilin. The structure of the chemical constituents obtained were identified by modern spectrum analysis techniques and their physico-chemical properties. Seven compounds were isolated from the fruit of R.davurica. They were identified as α-D-(6-O-sinapoyl)-glucopyranosyl-β-D-(3-O-sinapoyl)-fructo-furanose(1), luteolin-7-O-rutinoside(2), hyperin(3), quercetin(4), isoliquiritigenin(5), β-daucosterol(6), β-sitosterol(7). Compounds 1, 2 and 5 were obtained in the fruit of R. davurica for the first time.
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    Microwave-assisted Extraction and Bioavailability of Flavonoids from Ginkgo Leaves
    XU Chun-ming, WANG Ying-ying, LI Ting, PANG Gao-yang, LI Dan
    2014, 34 (4):  131-136.  doi: 10.3969/j.issn.0253-2417.2014.04.023
    Abstract ( 883 )   PDF (4157KB) ( 1356 )   Save
    On the basis of single factor test, the orthogonal design was employed to optimize microwave-assisted extraction of total flavonoids from ginkgo leaves. The bioavailability of flavonoids from ginkgo leaves was analyzed using gastrointestinal digestive process imitated in vitro. Ginkgo leaves and digested ginkgo leaves were compared using IR spectra and scanning electron microscopy. The results indicated that the highest extraction yield of flavonoids by microwave-assisted extraction could reach 2.698% using liquid to ethanol concentration of 70% as solvent, ratio of liquid to solid 25:1 (mL:g) and microwave power of 300 W for 60 s. During gastrointestinal digestion, the flavonoids in ginkgo were released, and can be digested and decomposed, then absorbed by human body. Infrared spectrum analysis showed that flavonoids from ginkgo leaves were digested during gastrointestinal digestion process, and its content was decreased. Scanning electron microscopy (SEM) results showed that the structure of samples before and after digestion was very different, and the gastrointestinal digestion changed the cell wall structure of sample.
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    Research Progress on Mechanism of Wood Liquefaction Reaction in Phenol and Polyhydric Alcohols
    ZHANG Qiu-hui, ZHAO Guang-jie
    2014, 34 (4):  137-143.  doi: 10.3969/j.issn.0253-2417.2014.04.024
    Abstract ( 834 )   PDF (1777KB) ( 810 )   Save
    The research progress of reaction mechanism on wood liquefaction by phenol or polyhydric alcohols was reviewed domestically and internationally. This paper suggested that the mechanism of wood liquefaction needs be further explored. The trend of the development of wood liquefaction mechanism research was summarized. It is helpful to reveal the essence of wood liquefaction, and supplement and improve the corresponding theoretical system on wood liquefaction mechanism. Meanwhile, it is also beneficial to realize the green liquefaction process, reduce the cost of liquefaction reaction, establish the nature of the product between the regulatory mechanism of wood liquefaction technology and finally accelerate the industrialization process.
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    Present Situation and Prospect on the Industrial Development of Cellulosic Fuel Ethanol
    WANG Wen, ZHUANG Xin-shu, YUAN Zhen-hong, XU Jing-liang, QI Wei, YU Qiang, TAN Xue-song
    2014, 34 (4):  144-150.  doi: 10.3969/j.issn.0253-2417.2014.04.025
    Abstract ( 1098 )   PDF (1777KB) ( 971 )   Save
    Fuel ethanol is a kind of clean and renewable energy. It has been considered as an alternative to oil or was blended with oil to reduce the CO2 emission. To develop fuel ethanol industry can alleviate the crisis on excessive consumption of fossil fuels, sustain the energy security, and achieve the sustainable development. The current industrial development of fuel ethanol in the USA, Brazil, European Union and China was summarized according to the productive capacity, the raw materials, and so on. The industrial development of cellulosic ethanol was mainly stated in this paper. The thermo-chemical and biochemical technologies applied in the conversion of cellulose to ethanol were described, and the bottlenecks of these two technologies were pointed out. Several ways were suggested to push the development of cellulosic ethanol industry, such as improvement of industrial technology, complementation of advanced technology, production of high value-added by-products, integration of manufacturing and marketing, and so on. Finally, it made an outlook for the future of cellulosic ethanol industry.
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    Biomass to Energy in China:Development Status and Strategic Consideration
    YAN Jin-ding
    2014, 34 (4):  151-158.  doi: 10.3969/j.issn.0253-2417.2014.04.026
    Abstract ( 1026 )   PDF (2467KB) ( 1362 )   Save
    This paper overviews the current situation of bio-energy development in China. The development tendency and industry prospect of the renewable energy originated from biomass was introduced both in China and worldwide. The existing main problem were mentioned and prospect of this research field is pointed out. This paper provide important reference for the bio-energy theory research, technology development and industry applications.
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