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    28 December 2014, Volume 34 Issue 6 Previous Issue    Next Issue
    Synthesis and Characterization of Castor Oil Based Initiator Used for Living Polymerization
    LIU Yu-peng, YU Juan, HUANG Hai-zhou, WANG Chun-peng, JI Yong-xin, LIU Mei-hong, WANG Ji-fu, CHU Fu-xiang
    2014, 34 (6):  1-7.  doi: 10.3969/j.issn.0253-2417.2014.06.001
    Abstract ( 663 )   PDF (1586KB) ( 597 )   Save
    Castor oil based atom transfer radical polymerization (ATRP) initiator was synthesized by one-pot reaction of 2-bromoisobutyryl bromide with hydroxyl group in castor oil under hydroxyl-to-bromide molar ratio of 1:1 and characterized by means of FT-IR, 1H NMR and 13C NMR. The results showed that the esterification for the synthesis of castor oil based ATRP initiator is prompt and highly efficient. In FT-IR spectrum, the conversion of hydroxyl group to ester group resulted in the decrease in the intensity of peak at 3500 cm-1 corresponding to hydroxyl group and increase of peak at 1740 cm-1 corresponding to ester group. This indicated that 2-bromoisobutyryl group was grafted on castor oil successfully. Subsequently, the castor oil based ATRP initiator was used to trigger the ATRP of methyl methacrylate (MMA) and styrene (St) under the condition of feeding molar ratio (monomer/initiator/CuBr/ligand) of 100:1:0.5:1 and reaction temperature 60 ℃ for MMA and 80 ℃ for St, respectively. GPC curves and spectra of 1H NMR and 13C NMR showed that polymerization process of MMA, as well as St, was highly efficient and well controlled.
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    Adsorption Property of Organically Modified Kieselguhr on Polyvinylacetate
    MAO Cui-ping, WU Shu-bin
    2014, 34 (6):  8-12.  doi: 10.3969/j.issn.0253-2417.2014.06.002
    Abstract ( 490 )   PDF (679KB) ( 463 )   Save
    The kieselguhr was modified by lignin-based cationic surfactant which was obtained from the Mannich reaction. Modified organic kieselguhr exhibited an excellent adsorption of dissolved and colloidal substances (DCS). In this paper, polyvinylacetate (PVAc) was chosen as the simulacrum of stickies. The effects of PVAc dosages, adsorption time and temperature on adsorption were discussed. Meanwhile, kinetic and thermodynamic parameters were obtained. Correlation coefficient of kinetic model, R2 were all beyond 0.99; the thermodynamic parameters ΔS, ΔH were -61.39 J/mol and -12.03 kJ/mol, respectively. The adsorption of PVAc on organic kieselguhr matched with the Langmuir model. The higher temperature was positive for the adsorption process. The adsorption process obeyed the pseudo-second-order kinetic model, and belonged to physical type.
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    The Catalytic Effects of Two-step Pretreatment Actived Carbon Loaded Pd by HNO3-H2O2 on Alkali Lignin
    LIU Liang, ZHANG Sheng-ming, FANG Gui-zhen
    2014, 34 (6):  13-20.  doi: 10.3969/j.issn.0253-2417.2014.06.003
    Abstract ( 675 )   PDF (1412KB) ( 515 )   Save
    The Pd/C catalyst was prepared using impregnation method, acidizing pretreatment activated carbon as the carrier, formaldehyde as reducing agent. The catalysts was characterized and its performance on alkali lignin was examined. Finally, the oxidation resistance was explored. That showed that the content of carboxyl functional groups on the surface of activated carbon was 1.31 mmol/g after pretreatment by HNO3 and H2O2. Pd/C catalyst was characterized by AAS, SEM, XRD and XPS. The AAS showed that the content of Pd was 2.9%, and the SEM photos showed that Pd was evenly and globularly distributed on the surface of the active carbon. The XRD and XPS data analysis indicated that Pd existed in the form of face-centered cubic structure, which is the main active species in the reaction. The hydroxyl groups of alkali lignin had significantly been improved after reaction. The content of hydroxy, phenolic hydroxyl and alcoholic hydroxyl increased by 158.74%, 4.21% and 255.96%, respectively. The GPC showed that the Mw of alkali lignin increased while the Mn and Mw/Mn reduced. The antioxidant properties of the lignin increased with concentration increased. It was lower than BHT at the same conditions.
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    Effect of Starch Esterification Performed by Dry Method on UV Aging Properties of Starch/Polylactic Acid Composite
    ZUO Ying-feng, GU Ji-you, YANG Long, TAN Hai-yan, ZHANG Yan-hua
    2014, 34 (6):  21-28.  doi: 10.3969/j.issn.0253-2417.2014.06.004
    Abstract ( 581 )   PDF (1829KB) ( 513 )   Save
    Maleic anhydride esterified starch was synthesized by using dry method with corn starch as raw material and maleic anhydride (MAH) as esterifying agent. FT-IR test results confirmed the successful esterification reaction between the maleic anhydride and corn starch. The maleic anhydride esterified starch was then blended with polylactic acid (PLA), and the mixture was melted and extruded to produce the esterified starch/polylactic acid (ES/PLA) composite. The composite was accelerated aging with UV aging box in order to study the effect of this process on aging properties of composites. FT-IR and SEM results showed that prolonging the aging time led to gradually decrease in the absorption peak strength of C—O, C—H and C=O and gradually increase in the extent of damage to the composite. In the same aging time, the group absorption peak strength of ES/PLA was higher than that of native starch/PLA (NS/PLA), and the extent of damage was less. XRD and DSC results showed that the crystallization peak of 2θ=21° disappeared and the crystallization peak of PLA at 16.5° appeared. This indicated that the hydrolysis of starch was faster than that of PLA. With the increase of the aging time, the crystallization of PLA in composites increased first, then decreased. It suggested that amorphous of PLA was first hydrolyzed. Influenced by the crystallinity, thermal decomposition temperature of composites increased first, and then decreased. The thermal stability of ES/PLA was better than that of NS/PLA. Besides, when the aging time was same, ES/PLA performed better mechanical properties compared with NS/PLA. And with the aging time prolonged, the mechanical strength of NS/PLA and ES/PLA gradually decreased.
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    Vacuum Pyrolysis of Camphorwood Sawdust Optimized by Response Surface Methodology and Bio-oil Composition Analysis
    FAN Yong-sheng, CAI Yi-xi, LI Xiao-hua, YU Ning, ZHANG Rong-xian, YIN Hai-yun
    2014, 34 (6):  29-36.  doi: 10.3969/j.issn.0253-2417.2014.06.005
    Abstract ( 533 )   PDF (3462KB) ( 656 )   Save
    Camphorwood sawdust from industrial processing was treated by vacuum pyrolysis for bio-oil preparation. The response surface methodology (RSM) was employed to optimize the process for maximum yield of bio-oil. All factors that affected bio-oil yield, including pyrolysis temperature, reaction pressure and heating rate, were investigated. Furthermore, the physicochemical properties of the bio-oil obtained from vacuum pyrolysis at the optimal conditions were evaluated. The chemical composition was also examined using Fourier transform infrared (FT-IR) and gas chromatograph/mass spectroscopy (GC-MS). The results showed that these three factors had obvious effects on bio-oil yield. However, the interaction between them was not remarkable. The optimal conditions for bio-oil yield were pyrolysis temperature 474.0 ℃, reaction pressure 7.5 kPa and heating rate 20.0 ℃/min. At this condition, the bio-oil yield could reach 50.25% close to 50.41%—the predicted value. Water content and high heat value of bio-oil was 21.35% and 26.82 MJ/kg, and its dynamic viscosity at room temperature, density, pH value and carbon residue content were 3.85 mm2/s, 1.08 g/cm3, 3.24 and 5.54%, respectively. Bio-oil from camphorwood sawdust was a complex mixture, which involve aromatics (26.30%), alcohols (12.14%), carboxylic acids (8.45%), aldehydes (26.17%), ketones (14.24%) and esters (1.18%). It also contained some specific organic compounds, which could be further extracted for industrial raw materials. Further study on enhancing the properties of bio-oil should be performed to ensure economic feasibility in future.
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    Preparation and Application of Curcumin Magnetic Molecularly Imprinted Solid-phase Extraction Material
    LIU Yu-nan, ZHANG Zhao-hui, HUANG Xiao-hua, RAO Wei
    2014, 34 (6):  37-43.  doi: 10.3969/j.issn.0253-2417.2014.06.006
    Abstract ( 704 )   PDF (1148KB) ( 538 )   Save
    Magnetic molecularly imprinted polymer(MIP)was prepared by using magnetic iron oxide as the carrier, curcumin as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linker. The Fe3O4@SiO2@MIP was characterized by scanning electron microscope, thermogravimetric analysis, vibrating sample magnetometer and infrared spectroscopy. The results showed that the Fe3O4@SiO2@MIP was prepared on magnetic iron oxide surface successfully. The adsorption properties were investigated by high performance liquid chromatography. The results demonstrated that the Fe3O4@SiO2@MIP exhibited specific selectivity toward curcumin. The maximum adsorption capacity on Fe3O4@SiO2@MIP was 36.2 mg/g, and the selectivity factors of curcumin toward rhein and emodin were 2.0 and 2.2, respectively. Combined with magnetic solid phase extraction and high-performance liquid chromatography technology, the Fe3O4@SiO2@MIP was used to separate, enrich and detect curcumin in ginger powder, sample solution successfully with the recoveries of 99.2%-107%.
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    A Micro Water Solid Phase Method for Oxidation of Gleditsia sinensis Lam.Galactomannan Gum
    ZHANG Wei-an, DUAN Jiu-fang, SUN Da-feng, ZHANG Wei-ming, JIANG Jian-xin
    2014, 34 (6):  44-48.  doi: 10.3969/j.issn.0253-2417.2014.06.007
    Abstract ( 614 )   PDF (887KB) ( 434 )   Save
    In this study, A micro-water solid phase method was used in the oxidation of Gleditsia sinensis Lam. Galactomannan (GSG) with H2O2 as the oxidizing reagents to prepare the oxidated G. sinensis Lam.Galactomannan(OGSG).The degree of substitution (Ds), relative molar mass and viscosity of OGSG treated with different concentrations of H2O2 were investigated by gel permeation chromatography (GPC), and viscometer detectors. The result showed that with the increasing of concentration of H2O2, molar-mass values and the intrinsic viscosity decreased and degree of substitution and polydispersity increased. With the dosage of GSG and 30% H2O2 20 g and 18 g, the reaction temperature 65 ℃ and reaction time 1 h, the Ds of product reached 1.22.The oxidation of GSG can be achieved by the method of micro-water solid phase oxidation modification under the condition of using fewer reaction reagent.
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    Comparison of Morphology and Fast Characterization Methods of Nanocellulose
    WANG Qian-qian, ZHU Qian-qian, SUN Jian-zhong, LIU Yu, ZHAN Huai-yu
    2014, 34 (6):  49-55.  doi: 10.3969/j.issn.0253-2417.2014.06.008
    Abstract ( 974 )   PDF (5605KB) ( 567 )   Save
    In this study, nanocellulose was prepared by acid hydrolysis, cellulase enzyme pretreatment, TEMPO oxidation and mechanical fibrillation techniques using commercial southern pine dissolving pulp and bleached eucalyptus pulp as raw materials, respectively. This study intended to provide relatively complete morphological pictures of several kinds of wood nanocellulose including cellulose nanocrystals (CNC) and cellulose nanofibrils (CNF) produced by most commonly used processes. TEM and AFM were applied to provide visual examinations of several nanocellulose samples. Commercial particle sizing instruments were evaluated for quick particle sizing the samples. It was found that CNC were mainly rodlike nano-whiskers with diameter of approximately 20 nm and length ranging from 10 to 200 nm as expected, and CNF were fibril network particles with a diameter ranging from several nanometers to several hundred nanometers, respectively. The instruments based on the centrifuge and a Brownian motion showed good repeatability in particle sizing. Both instruments were well suited to semi-quantitative characterize non network particles even with large aspect ratios such as CNC, but further study is required before they can be used for characterizing network particles such as CNF.
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    Chromatographic Separation of Single Glucosyl Flavonoid Glycosides Using Collagenous Fiber as Adsorbent
    LI Xin-xin, ZHANG Qi-xian, ZHANG Wen-hua, LIAO Xue-pin, SHI Bi
    2014, 34 (6):  56-60.  doi: 10.3969/j.issn.0253-2417.2014.06.009
    Abstract ( 618 )   PDF (757KB) ( 465 )   Save
    The collagenous fiber cross-linked by glutaraldehyde was used as an adsorbent (CFA) for chromatographic separation of single glucosyl flavonoid glycosides. Genistin and baicalin with similar molecular structure were chosen as the representatives of flavonoid glycosides in the experiments is this paper. It was found that the adsorptive affinity and selectivity of CFA to genistin and baicalin could be adjusted by ethanol concentration in aqueous solution. In column chromatographic separation, where the CFA dosage was 6 g and the ratio of column height to diameter was 10:1, genistin and baicalin were well separated by stepwise elution of 100%-90%-70% ethanol aqueous solutions. The purities of the obtained genistin and baicalin were 98% and 97%, and their recovery rates were 99.35% and 96.52%, respectively.
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    Separation and Utilization of Classification Products in Liquefied Oil of Biomass
    FENG Jun-feng, JIANG Jian-chun, XU Jun-ming, HE Xiao-liang, YANG Zhong-zhi, XU Le
    2014, 34 (6):  61-68.  doi: 10.3969/j.issn.0253-2417.2014.06.010
    Abstract ( 840 )   PDF (1039KB) ( 550 )   Save
    Liquefaction of biomass using concentrated sulfuric acid as catalyst and methanol-glycerol complex as solvent was investigated. The liquefied products from bamboo shavings, poplar, eucalyptus and pine were neutralized, filtrated and followed by rotary evaporation. The results show that the product from liquefaction of bamboo shaving are mixture of phenolics and acetyl methyl glucoside. Polyglycoside phase mainly contains about 41.81% of polyglycosides which were mainly pyranoside, and 47.27% of unreacted glycerin and glycerin polymers. On the other hand, polyphenol phase mainly contains levulinate, polyphenols, and glycerol, and the content of glycerine and its polymers is 38.04%. Polyphenols mainly contain phenols and levulinic acid esters, and the average molecular weight of phenolics is approximate 990.
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    Production Practice of Total Chlorine Free Clean Bleaching Bagasse Pulp
    HE Shui-lin, LI Jun, LI Zhi, XU Jun, MO Li-huan
    2014, 34 (6):  69-74.  doi: 10.3969/j.issn.0253-2417.2014.06.011
    Abstract ( 695 )   PDF (1074KB) ( 430 )   Save
    The experimental research, process design and production practice of total chlorine free OpQPo bleaching bagasse pulp were introduced in this paper. The results showed that Kappa number decreased from 14.0-15.0 to 7.0-7.3 with a 50%-51% removal of residual lignin, and pulp brightness increased from 42%-45%(ISO) to 58%-60%(ISO) after a strengthened oxygen delignification. The production practice showed a better performance than that in lab. After subsequent pretreatment and pressurized hydrogen peroxide bleaching, the final pulp brightness was beyond 80% and the viscosity was over 800 mL/g. The pulp quality was much better than traditional Chlorine-Alkali Extraction-Hypochlorite(CEH) bleached pulp. Moreover, adsorbable organic halides (AOX) was not generated any more in the bleaching process. The wastewater was only discharged in chelating pretreatment (Q) stage and easily treated to meet the critical discharge standard due to its lower chromaticity and lower pollution load. In contrast to the traditional bleaching, no additional investment was needed in this new technology. Besides, the production procedure was flexible and the operation was stable. The investment of main equipments was about ¥13.55 million yuan.
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    Synthesis, Characterization and Properties of Rosin Ester Hydroxylpropyl Quaternary Ammonium Surfactants
    HUANG Xiu-zhi, RAO Xiao-ping, XUE Zhi-ge, CUI Yan-jie
    2014, 34 (6):  75-80.  doi: 10.3969/j.issn.0253-2417.2014.06.012
    Abstract ( 567 )   PDF (822KB) ( 498 )   Save
    Three rosin ester hydroxlpropoyl quaternary ammonium surfactants (Ⅰ, Ⅱ and Ⅲ), were synthesized from dehydroabietic acid, acrylopimaric acid, maleopimaric acid and 2, 3-epoxy propyl trimethyl ammonium chloride (GTMAC). Their structures were characterized by IR, 1H NMR and 13C NMR spectra, respectively. The critical micelle concentration (Ccmc), surface tension (γcmc), emulsifying ability, foaming ability and bactericidal activity of three quaternary ammonium surfactants were evaluated. The results showed that their Ccmc values are 3.58×10-4, 2.53×10-4 and 3.25×10-4 mol/L, their γcmc were 38.9, 28.9 and 33.5 mN/m, their emulsifying abilities were 31, 33 and 38 min, respectively. The foaming ability of Ⅰ was better than the others, foaming ability was 115 mm, and 85 mm after 5 min. With the increase in the number of quaternary ammonium salt, HLB value was increased, and the hydrophilic of surfactant was enhanced. Compound Ⅰexhibited excellent antibacterial activity against Staphyloccocus aureus, and the minimum inhibition concentration was 4 mg/L.
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    Preparation of Porous Biological Carrier with Gingko LCC and Application in Culture of Human Hepatocytes
    LI Jin-ling, WANG Peng, YANG Jing, CHEN Fan-geng, XIE Zhi-jie, XIE Yi-min
    2014, 34 (6):  81-87.  doi: 10.3969/j.issn.0253-2417.2014.06.013
    Abstract ( 573 )   PDF (1185KB) ( 466 )   Save
    A porous biological carrier was prepared by the method of eluting stent with lignin-carbohydrate complexes (LCC) isolated from ginkgo wood. Fourier transform infrared spectrometer(FT-IR), high performance liquid chromatograph(HPLC), nuclear magnetic resonance (NMR) spectroscopy and scanning electron microscope (SEM) were applied to elucidate the composition, chemical structure and morphology of the biological carrier. The results indicate that a biological carrier with excellent performance can be prepared with gingko LCC as raw material. Not only the guaiacyl lignin subunits existe in this biological carrier, but also the galactose and mannose with high biological compatibility to human hepatocytes are found to be 3.30% and 21.94%, respectively. The porosity of prepared porous scaffold is more than 60% with average pore size of 130 μm. The carriers were used to culture human hepatocytes. The results show that human hepatocytes can grow successfully on carriers. Furthermore, the human hepatocytes on carriers proliferate rapidly and show a high metabolic activity by determination of human albumin and glucose metabolism. These interesting results indicate that porous biological carrier prepared with gingko LCC have an excellent biocompatibility.
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    Purification of Lignans and Pinoresinol Diglucoside from Eucommia ulmoides Oliv.
    PENG Mi-jun, LÜ Qiang, PENG Sheng, ZHANG Chang-wei, ZHANG Lin-jie, WANG Zhi-hong, ZHOU Yun-lei
    2014, 34 (6):  88-92.  doi: 10.3969/j.issn.0253-2417.2014.06.014
    Abstract ( 607 )   PDF (1451KB) ( 418 )   Save
    Purification of lignans and pinoresinol diglucoside(PDG) from Eucommia bark extract was studied by a combined method of macroporous adsorption resin-C18 column chromatography and silica gel column chromatography. The results indicated that AB-8 resin was the best one on the adsorption and desorption rates by comparing with the other 3 kinds of resins. The purity of effective part of lignans and the crude product of PDG were respectively from 23.33% to 71.61% and 0.960 5% to 8.070% through AB-8 resin once. Then the purity of PDG increased to 53.12% after C18 purification and finally reached 91.50% after purifying by normal phase silica gel column chromatography.
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    Design and Experiments Study on Combustion Engine of Straw Briquettes Fuel
    SUN Kang, CHEN Chao, XU Yu, LIU Yong, ZHU Guang-zhen, Ying Hao
    2014, 34 (6):  93-99.  doi: 10.3969/j.issn.0253-2417.2014.06.015
    Abstract ( 543 )   PDF (1158KB) ( 476 )   Save
    In order to solve the problems in biomass briquette combustion including low efficiency, exhausting gas and smoke, slagging easily and difficulty to remove, we designed a new type of combustion machine which adopt staged combustion mode. The steam boiler heating experiments were conducted and the results showed that the output of boiler was 5 300 MJ and combustion efficiency was 99.36%. The combustion gas contained CO with 0.001 45% and the contents of SO2 and NOX were 0.01% and 0.06%, respectively. Slag could be automatically broken and slagging-off under the help of automatic slag broken & clean device.
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    Effect of Cardanol Based Plasticizers on Properties of Acetylated Wood Flour Composites
    XIE Zhen-hua XIE Zhen-hua, JIN Li-wei
    2014, 34 (6):  100-104.  doi: 10.3969/j.issn.0253-2417.2014.06.016
    Abstract ( 946 )   PDF (488KB) ( 539 )   Save
    Composites of acetylated wood flour (AWF)/low-density polyethylene (LDPE) were prepared by extrusion-injection molding process, and cardanol acetate (CA) and epoxy cardanol acetate (ECA) were added respectively. Properties such as tensile strength and hydrophobic as well as surface energy, migration of plasticizers and thermal mechanical properties (TMA) were studied. The results showed that the tensile strength of composites decreased with the increasing content of plasticizers, but tensile strength of all composites with CA were higher than that of composites with ECA. Composites with 5% plasticizers showed similar hydrophobicity, but composites with 15% CA was more hydrophobic, and contact angle test showed the similar results. The migration test of plasticizers revealed ECA had lower transfer constant (4.35×10-4) than that of CA (5.48×10-4) at 85 ℃ in 100 min, and ECA retained more in the composites after 3 700 min. The result of TMA exhibited the inflation of composites intensified with increasing temperature, and composites with 15% ECA showed higher coefficient of linear expansion (3 758 μm/(m·℃)) than that of composites with CA (3 182 μm/(m·℃)).
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    Cellulase Pretreatment on Poplar APMP and Its Impact on Papermaking
    SHEN Li-hong, YANG Gui-hua, CHEN Jia-chuan
    2014, 34 (6):  105-110.  doi: 10.3969/j.issn.0253-2417.2014.06.017
    Abstract ( 600 )   PDF (2638KB) ( 454 )   Save
    Cellulase pretreatment was utilized to treat the poplar alkaline peroxide mechanical pulp (APMP) in present study to improve its papermaking performance and expand the application. The results showed that the beating energy consumption of the pretreated APMP decreased by 19% maximum and water retention value increased by 12.6%, compared to the virgin APMP. Meanwhile, the breaking length, bursting index and tearing index of the papersheets, which were furnished by pretreated APMP and blended with different ratio of softwood bleached kraft pulp (BKP), increased maximum by 6.1%,44.6% and 30.3% respectively. However, the bulk, brightness and the opacity were decreased slightly. The fiber quality analysis(FQA), scanning electron microscope(SEM) and X-ray diffraction(XRD) were employed to characterize. The analysis results indicated that the fiber length increased by 7.0%, the fines content decreased by 10.0%, and the curl index decreased by 22.4% compared with the pretreated APMP with the virgin APMP. Beside, a 0.7% increase of the crystallinity was observed. Cellulose pretreatment can improve the fiber quality of poplar APMP. The resulted in a better physical strength property.
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    Synthesis and Properties of Rosin-based Quaternary Ammonium Salt Heterogemini Surfactant
    WANG Juan, WANG Dan, SHANG Shi-bin, SHEN Ming-gui, QI Fan
    2014, 34 (6):  111-116.  doi: 10.3969/j.issn.0253-2417.2014.06.018
    Abstract ( 617 )   PDF (827KB) ( 562 )   Save
    Four rosin-based quaternary ammonium heterogemini surfactants were synthesized from dehydroabietic acid via the reactions of amidation, reduction and quaternarization, which were named N,N,N',N'-tetramethyl- N-dehydroabietyl-1,3-propylene diammonium bromide, N,N,N',N'-tetramethyl-N-dehydroabietyl-1,4-butane diammonium bromide, N,N,N',N'- tetramethyl-N-dehydroabietyl-1,5-pentane diammonium bromide, and N,N,N',N'-tetramethyl-N-dehydroabietyl-1,6-hexane diammonium bromide. The structures of these compounds were confirmed by FT-IR and 1H NMR. The surface activities, e.g. surface tension (γcmc),critical micelle concentration(Ccmc) and Krafft points, ect.. Their antibacterial activities were investigated and analyzed. The results showed that the Ccmc values of the heterogemini surfactants were 3.32×10-5, 2.86×10-5, 2.54×10-5, 2.28×10-5 mol/L, and the γcmc values were 24.7, 26.5, 28.9, 32.3 mN/m, the Krafft points 12, 17, 20, 23 ℃, respectively. Separating 10 mL water from the turpentine/water emulsion spent 42, 45, 53 and 48 h, respectively. The initial foam heights were 137, 128, 131 and 135 mm, and after 5 minutes, the heights reached 125, 121, 127 and 131 mm, respectively. Through the test, the minimal inhibitory concentration on escherichia coil were 4,< 2, < 2 and 2 mg/L and the antibacterial activities were superior to the commercial bacteriostatic agent bromogeramine (64 mg/L).
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    Synthesis and Properties of Organic Gelator Based on Dehydroabietate Derivative
    TONG Bi-hai, ZHANG Man, LI Jian-fei, MA Peng, WANG Heng-shan, ZHANG Qian-feng
    2014, 34 (6):  117-123.  doi: 10.3969/j.issn.0253-2417.2014.06.019
    Abstract ( 663 )   PDF (1082KB) ( 497 )   Save
    A novel low-molecular-mass organic gelator (DBNPM) was synthesized from 12-bromine-13, 14-dinitro dehydroabietic acid methyl ester. The title compound was characterized by 1H NMR, 13C NMR, IR and MS techniques. The assembly behavior of the prepared organogelator in solution was investigated. The organogelator induced gelation in a wide variety of organic solvents. With methanol as solvent, the critical gelation concentration (CGC) of the prepared gelator was the minimum, 0.5 g/L. But the gelatination property was the most stable in 1, 4-dioxane. Scanning eletron microscope (SEM) images indicated that the xerogels from methanol solution presented flaky structure and the xerogels from 1, 4-dioxane solution were net-like structure. Infrared spectra (FT-IR) and XRD showed that hydrogen bond was the main driving force for the formation of organogels.
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    Optimization of Synthesis of Hydroxyl Citronella Aldehyde-1,2-propanediol Acetal Using Response Surface Method
    CAI Mei-ping, FAN Guo-rong, CHEN Shang-xing, CHEN Jin-zhu, WANG Zong-de
    2014, 34 (6):  124-128.  doi: 10.3969/j.issn.0253-2417.2014.06.020
    Abstract ( 812 )   PDF (725KB) ( 533 )   Save
    On the basis of single factor experiments, the synthesis conditions of hydroxyl citronella aldehyde-1,2-propanediol acetal from hydroxycitronellal and 1,2-propylene glycol were optimized using response surface method (RSM). The results of the single factor experiments showed that the most significant factors were the substance ratio of hydroxycitronellal to 1,2-propylene glycol, the reaction temperature and the reaction time. According to the experiment design principle of Central Composite Design, the response surface method of three factors with three levels were employed, and the yield of target compound in the reaction system were taken as the response value to analyze the significance and interaction of the various factors. The optimal synthesis conditions were substance ratio of hydroxycitronellal to 1,2-propylene glycol 1:3.5, reaction temperature 38 ℃, reaction time 4.4 h, and substance ratio of hydroxycitronellal to toluene 1:2-1:2.5. Under the optimal conditions, the yield of target compound was 89.76%.
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    Adsorption Kinetics and Isotherm of Methylene Blue on Activated Carbon from Sandlive Willow
    ZHANG Gui-lan, BAO Yong-ze, MIAO Ya-wen
    2014, 34 (6):  129-134.  doi: 10.3969/j.issn.0253-2417.2014.06.021
    Abstract ( 700 )   PDF (697KB) ( 614 )   Save
    The activated carbon with low cost and high performance was prepared by chemical activation of salix psammophila in order to improve utilization value of the biomass. Three kinds of activators were employed and their adsorption performance of methylene blue (MB) were investigated. The effects of temperature and pH value on adsorption, adsorption isotherms and adsorption kinetics studied. The experimental results indicated that activated carbon from different activators had different ability in methylene blue adsorption. When using KOH, H3PO4 and ZnCl2 as activators, adsorption capacities were 519.63, 347.13 and 323.45 mg/g, respectively. Adsorption behavior of activated carbon conformed to the pseudo-second-order kinetics with good correlation and fitted well with the Langmuir isotherm model. The increasing of pH value and temperature was beneficial for adsorption process.
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    Expression Purification and Directed Evolution of Cytochrome P450 from Bacillus megaterium
    LI Xun, WANG Ting, WANG Liang-liang, WANG Fei
    2014, 34 (6):  135-140.  doi: 10.3969/j.issn.0253-2417.2014.06.022
    Abstract ( 608 )   PDF (1266KB) ( 503 )   Save
    In order to express the cytochrome P450 enzyme (CYPs) from Bacillus megaterium ALA2 effectively, the CYPs genes (cyp) were cloned into pET20b (T7 promoter) and pTrc99A (Trc promoter) to yield pET20b-cyp and pTrc99A-cyp. Then they were transferred into the Escherichia coli BL21 (DE3) and Top10. The pTrc99A-cyp produced more recombinant CYPs than pET20b-cyp. The Ni-NTA purification of CYPs was optimized. The recombinant CYPs were eluted by 60 mmol/L imidazole at pH 8.1. The enzyme activity of purified recombinant CYPs was 2 095 U/mg and recovery rate reached 31%, and the recovery ratio was 2.32. The mutation positions of the threonine (T) and phenylalanine (F) were measured as 269 loci and 394 loci by reasonable experimental design. The activities of mutant enzyme T269S and T269R were increased by 32.0% and 29.0% respectively with palmitic acid as substrate, and 11.6% and 9.1% with oleic acid as substrate.
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    Process of Producing Organic Fertilizer by Solid-state Fermentation of Leaves Residual of Eucommia ulmoides Oliv.
    ZHANG Chang-wei, PENG Sheng, ZHANG Lin-jie, WANG Zhi-hong, ZHOU Yun-lei, PENG Mi-jun
    2014, 34 (6):  141-145.  doi: 10.3969/j.issn.0253-2417.2014.06.023
    Abstract ( 666 )   PDF (849KB) ( 460 )   Save
    The preparation process of organic fertilizer by solid-state fermentation of leaves residual of Eucommia ulmoides Oliv. was studied. Effects of four main factors, including bacteria combination, ratio of liquor to material, additive amount of glucose and fermentation time on the mass fraction of humic acid, were analyzed by using single factor method. Based on the single factor test, the process conditions of solid-state fermentation of Eucommia unmolds Oliv. were optimized by the orthogonal experiments method, and toxicity of the vested organic fertilizer was tested. The results showed that the optimum condition were the ratio of liquor to material 2.0:1, additive amount of glucose 1.5%, and inoculating the composite bacteria of white rot fungus and Trichoderma koningii to the Eucommia ulmoides Oliv., and fermentation time 6 days. In this experimental condition, the mass fraction of humic acid in the leaves residual of Eucommia ulmoides Oliv. could reach 38.31%. The results of toxicity test showed that the germination rate of brassica chinensis were all higher than 90%. It proved that the organic fertilizer prepared by leaves residual of Eucommia ulmoides Oliv. was nontoxic.
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    Research Progress on the Microscopy and Micro-spectroscopy in Biomass Pretreatment
    MA Jian-feng, ZHANG Xun, MA Jing, JI Zhe, ZHOU Xia, XU Feng
    2014, 34 (6):  146-154.  doi: 10.3969/j.issn.0253-2417.2014.06.024
    Abstract ( 748 )   PDF (2613KB) ( 565 )   Save
    This paper reviewed the applications of light microscopy (LM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), confocal laser scanning microscopy (CLSM), FT-IR microscopy, confocal Raman microscopy (CRM) and micro-UV spectrometer (UMSP) on chemical, biological and physical-chemical pretreatment in detail. The established approaches provided alternatives to the scientific research and industrialization development related to biomass conversion.
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    Research Status Analysis of Acid Catalyzed Hydrolysis of Biomass to Levulinic Acid
    WANG Qiong, ZHUANG Xin-shu, YUAN Zhen-hong, XU Jing-liang, QI Wei, YU Qiang
    2014, 34 (6):  155-164.  doi: 10.3969/j.issn.0253-2417.2014.06.025
    Abstract ( 870 )   PDF (1626KB) ( 525 )   Save
    This paper discussed the research status of acid catalyzed hydrolysis of biomass to levulinic acid (LA) with three aspects i.e. sources of raw materials, processes and reactors, and catalytic mechanism. Especially in the field of catalytic mechanism, it gradually analyzed the mechanism of LA production from cellulose to sugars, sugars to 5-hydroxymethylfurfural(5-HMF), and 5-HMF to LA, and the mechanism of LA production directly from glucose, as well as the demonstration of the kinetics of LA production from microcrystalline cellulose under dilute hydrochloric acid and dilute sulfuric acid environments, followed by the kinetics and mechanism analysis of degradation of typical biomass in the dilute acid. This paper aims to provide sufficient information for relative scholars to carry out researches on LA production from biomass, and help scholars to conduct selective research.
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