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Table of Content

    28 August 2015, Volume 35 Issue 4 Previous Issue    Next Issue
    Micro Characteristics of Biomass Investigated by Scanning Thermal Microscopy
    XU De-liang, FU Xin, XU Chao-yang, WANG Si-qun, SUN Jun, ZHOU Ding-guo
    2015, 35 (4):  1-7.  doi: 10.3969/j.issn.0253-2417.2015.04.001
    Abstract ( 488 )   PDF (1645KB) ( 543 )   Save
    The application of scanning thermal microscopy(SThM) technique in the studies of bio-composites interface characteristics and the thermal conductivity characteristics in micro-scale of biomass materials was discussed using red oak and rice straw cell as research objects. The results indicated that the thermal conductivity mode of SThM could imaged the microstructure of biomass cell very well, and the thermal conductivity characteristics of these two biomass were similar. This showed that the thermal conductivity of S2 layer was higher than that of middle lamella of cell wall(CML).
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    Preparation and Characterization of Phenolic Foams Modified by Castor Oil-based Polyurethane Prepolymer
    BO Cai-ying, HU Li-hong, ZHOU Jing, ZHOU Yong-hong
    2015, 35 (4):  8-14.  doi: 10.3969/j.issn.0253-2417.2015.04.002
    Abstract ( 567 )   PDF (1158KB) ( 642 )   Save
    Castor oil-based polyurethane prepolymer(COPUP) was prepared through the reaction of castor oil(CTO) with 1,6-hexamethylene diisocyanate(HDI), then COPUP was used to modify phenolic foams(PFs). The structure of COPUP was confirmed by FT-IR and 1H NMR. Morphological properties, mechanical properties and thermal stability of the copup-filled PFs were assessed by SEM, universal test and thermogravimetric analysis(TGA). The cell shapes of the COPUP-filled PFs were approximately symmetrical, but the cell sizes were larger than that of pristine PF. Especially, when the cell sizes of PF modified with 10 % COPUP, it became obviously heterogeneous and the bubbles collapse. Compared with that of pristine PFs, the flexural strength of PFs filled with 3%-7% COPUP increased about 21.05%-26.32%; and the corresponding specific flexural strength ranged from 5.90 to 6.17 (kN·m)/kg, which were significantly higher than that of the pristine PFs, 4.96(kN·m)/kg. The addition of COPUP caused the decrease of the thermal stability of PFs.
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    Synthesis and Characterization of Myrcene Based Vinyl Ester Resin and Properties of its UV Curing Products
    YANG Xue-juan, LI Shou-hai, TANG Xiao-dong, SONG Jian, XIA Jian-ling
    2015, 35 (4):  15-20.  doi: 10.3969/j.issn.0253-2417.2015.04.003
    Abstract ( 680 )   PDF (1065KB) ( 661 )   Save
    A novel acrylic modified epoxided maleinized myrcene monomer (AE-MYM) was prepared by D-A addition reaction, polycondensation and epoxy ring opening esterification of myrcene (MY) with maleic anhydride, epichlorohydrin and acrylic. The molecular structure of the product was characterized with FT-IR and GPC. The UV curing behaviors of the resin monomer were also studied by using FT-IR. The results demonstrated that the target product was successfully synthesized. And the curing degree of the prepared myrcene based resin monomer could reach above 70 % within 50 s. Dynamic mechanical analysis(DMA) results showed that the glass transition temperature and the modulus of the prepared UV curing material were 65 ℃ and 4400 MPa respectively. Tensile properties testing results demonstrated that the tensile strength of prepared UV cured material could reach above 50 MPa. All the results showed that the curing product was an excellent rigid material.
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    Preparation of Micron-size Spherical Activated Carbon from Carboxymethyl Cellulose via Combination of Hydrothermal Carbonization and Carbon Dioxide Activation Method
    DAI Lin-lin, LI Wei, WU Qiong, ZHAO Xin, LIU Shou-xin
    2015, 35 (4):  21-27.  doi: 10.3969/j.issn.0253-2417.2015.04.004
    Abstract ( 862 )   PDF (3460KB) ( 611 )   Save
    Micron-size spherical activated carbon(SAC) was prepared via hydrothermal carbonization-CO2 activation using carboxymethyl cellulose(CMC) as starting materials. The effects of reaction parameters including carbonization temperature,reaction time,CMC dose,activation temperature,and activation time on the morphology and porous structure of spherical carbon(SC) were evaluated. Scanning electron microscopy(SEM),Fourier transform diffuse reflectance infrared spectroscopy(FT-IR),X-ray photoelectron spectroscopy(XPS),and N2(77K) adsorption-desorption isotherm were used for characterization of the synthesized products. The results indicated that the carbon sphere precursor,which mainly containing oxygenated functional groups of —COOR and —OH,were changed after hydrothermal carbonization. Regular carbon spheres with uniform sizes and good dispersity were prepared under the optimum conditions(200 ℃,10 h,1.5 g CMC,and 40 mL H2O). After the activation of carbon sphere precursor under CO2 atmosphere at 850 ℃ for 2h,micron-size spherical activated carbon with surface area of 1005.85 m2/g and average pore diameter of 2.78 nm was obtained.
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    Preparation of Reed Hemicelluloses-based Hydrogels and its Highly Effective Adsorption of Heavy Metal Ions
    ZHANG Wen-ming, HUANG Ying, ZHU Sha, LI Xiao-wei, LIU Jin-wei, ZHANG Yu-cang
    2015, 35 (4):  28-34.  doi: 10.3969/j.issn.0253-2417.2015.04.005
    Abstract ( 555 )   PDF (901KB) ( 497 )   Save
    Reed hemicelluloses-based hydrogel was prepared by free radical polymerization using acrylic acid(AA) as monomer and N, N, N', N'-tetramethylene ethylene diamine(MBA) as crosslinking agent. The chemical structure was characterized by FT-IR and the adsorption of heavy metal ions(Pd2+, Cd2+, and Zn2+) was also investigated. The effects of AA and MBA dosages, pH value, contacting time, and initial concentration of metal ion on the adsorption capacity were studied. At the same time the adsorption kinetics and adsorption mechanism of metal ions were discussed. The results showed that the adsorption capacity was influenced by AA and MBA dosages and pH value, and increased with the increase of pH value. The adsorption equilibrium time was approximately 60 min when the hemicellulose was 1.0 g, MBA was 0.1 g, and AA was 9 g. The maximum adsorption capacities of Pd2+, Cd2+, and Zn2+ were 699, 521, and 265 mg/g, respectively. The adsorption process was an ion-exchange mechanism. This suggested that the adsorption kinetics fitted the pseudo-second-order model and the adsorption followed the Langmuir model. Furthermore, reed hemicelluloses-based hydrogel also exhibited highly efficient adsorption of metal ions after 8 repeated adsorption/desorption cycles as the adsorption capacity of Pd2+, Cd2+, and Zn2+ were 616, 479 and 243 mg/g, and the recovery of Pd2+, Cd2+, and Zn2+ were 96.7%, 97.1% and 97.6%, respectively.
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    Preparation of Chitosan from Waste Biomass of Rhizopus oryzae and its Membrane Characteristics
    YANG Lei, LI Xin, YU Shi-yuan, YONG Qiang
    2015, 35 (4):  35-40.  doi: 10.3969/j.issn.0253-2417.2015.04.006
    Abstract ( 475 )   PDF (990KB) ( 578 )   Save
    Preparation of chitosan from waste biomass of lactic acid fermentation and its membrane characteristics were investigated. The results indicated that 100 g/L of glucose was fermented by R. oryzae for 48 h, then 51.59 g/L of lactic acid and 4.36 g/L of biomass were obtained, and chitosan extraction yield about 13.5 % of the cell dry weight was achieved . The deacetylation degree of R. oryzae chitosan was 89.4%, which was higher than that of commodity chitosan(86.6%). The viscosity of 20 g/L of R. oryzae chitosan solution was 5.13 mPa·s, and the molecular weight of R. oryzae chitosan(Mw=68.61 ku, Mn=48.13 ku) was similar to commodity chitosan(Mw=70.17 ku, Mn=53.53 ku), which was extracted from crab shell. The results of FT-IR proved that the R. oryzae chitosan was similar to commodity chitosan. When the thickness of membrane was (0.025±0.002)mm,the modulus of elasticity of R. oryzae chitosan membrane and commodity chitosan membrane were 42.72 and 14.64 N/mm2, respectively. The tensile strengths were 132.31 and 44.13 N/m, respectively. The water absorption rates were 52.90% and 175.80%, respectively. The temperatures at maixmum decomposition rate were 281.4 ℃ and 285.4 ℃, respectively. The onset and final temperature of decomposition were different. The film-forming performance of R. oryzae chitosan was better than that of commodity chitosan, and the R. oryzae chitosan was suitable for food packaging film preparation.
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    Synthesis Process of Epoxidized Dehydrated Castor Oil
    HUANG Xu-juan, LIU He, SHANG Shi-bin, QI Fan
    2015, 35 (4):  41-47.  doi: 10.3969/j.issn.0253-2417.2015.04.007
    Abstract ( 740 )   PDF (988KB) ( 530 )   Save
    Dehydrated castor oil(DCO) was firstly prepared by using castor oil(CTO) as raw material via dehydration reaction, and epoxidized dehydrated castor oil(EDCO) was synthesized using phosphoric acid as catalyst and acetic acid peroxide as the oxidant by epoxidation reaction afterwards. The influences of different parameters on the epoxy value of EDCO were investigated through single factor and orthogonal experiments. The results indicated that the optimal preparation conditions of EDCO were 3.5 h reaction time, 30 ℃ reaction temperature, 5.5:1 molar ratio of peracetic acid to DCO and 0.5% phosphoric acid dosage. The epoxy value of EDCO could be up to 4.82% under these conditions. In addition, the chemical structures of CTO, DCO, and EDCO were characterized by FT-IR and 1H NMR . It was confirmed that the C=C double bonds in EDCO almost disappeared and the epoxy bonds were formed during the epoxidation. The properties of the products were also studied by viscosity measurement and thermogravimetric analysis(TG). Viscosity measurement showed that the viscosities of CTO, DCO, and EDCO were 1100.0, 299.5 and 1896.0 mPa·s, respectively. TG analysis demonstrated that the descending order of thermal stability of the products was EDCO> DCO> CTO.
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    In-situ Synthesis and Catalytic Properties of Carbon-based Phosphotungstic Acid
    LU Yan-feng, WU Geng-feng, ZENG Chang-wei, LI Tao, LÜ Jian-hua, CHEN Yan-dan, HUANG Biao
    2015, 35 (4):  48-52.  doi: 10.3969/j.issn.0253-2417.2015.04.008
    Abstract ( 551 )   PDF (1088KB) ( 500 )   Save
    Carbon-based phosphotungstic acid (H3PW12O40) catalyst was prepared from sawdust of Chinese fir by in-situ synthesis. Nanocrystalline cellulose (NCC) from cellulose by catalytic hydrolysis was studied. The effects of impregnation ratio, carbonization temperature and carbonization time on the yield of NCC were also analyzed. The results showed that under the impregnation ratio of liquid to solid 2.5:1, thecarbonization temperature 350 ℃ and carbonization time 1.5 h, a comparatively high yield of NCC was observed as 25.28%. The catalysts were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, and scanning electron microscope. The results indicated that phosphotungstic acid was loaded on the carbon under good conditions, the keggin structure characteristic absorption peak of carbon-based phosphotungstic acid remains stable, and the initial decomposition temperature of keggin structure of phosphotungstic acid is 370 ℃. The morphological and crystal structures of NCC were carried out by Transmission electron microscopy and X-ray diffraction. The results showed that the NCC observed by TEM turned out to be rod-like, with the size of 9-70 nm in width and 130-830 nm in length and the average aspect ratio of 11.2:1. X-ray diffraction analysis revealed that the crystallinity of the NCC was 76.1 %, with the average particle size of 6.9 nm.
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    Preparation of High Microporosity Activated Carbon by Autogenic Pressure under High Temperature
    SUN Kang, JIANG Jian-chun, LU Xin-cheng, CHEN Chao, JIA Yu-jie
    2015, 35 (4):  53-58.  doi: 10.3969/j.issn.0253-2417.2015.04.009
    Abstract ( 573 )   PDF (770KB) ( 526 )   Save
    By using coconut shell, almond shell, camellia nutshell and Chinese fir sawdust as raw materials, high microporosity activated carbons were prepared via the activation method of autogenic pressure at elevated temperatures without activating agent. The effects of activation temperature, activation time and system pressure on the pore structure and adsorption properties of AC were studied. The results showed that coconut shell based AC was prepared with microporisty rate of 87.8%, and the yield was 13.8% under the autogenic pressure at elevated temperatures with activation 900 ℃ kept for 6 h. The surface area, total volume, iodine value, and methylene blue value were 1194.4 m2/g, 0.528 cm3/g, 1280 mg/g, and 315 mg/g, respectively. Water vapour and carbon dioxide generated from pyrolysis of woody materials formed mixed activation agent, and the autogenous pressure effectively promote the activation reaction rate of gas and solid. The activation method of autogenic pressure at elevated temperatures was a kind of new activation method which had good economic and environmental benefits, since the production process could keep clean and convenient without any pollution and the yield of product was high.
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    Effect of Different Strains on Fermented Feedstuff from Olive Leaves
    XIE Pu-jun, HUANG Li-xin, ZHANG Cai-hong, YOU Feng, ZHANG Yao-lei
    2015, 35 (4):  59-64.  doi: 10.3969/j.issn.0253-2417.2015.04.010
    Abstract ( 544 )   PDF (1046KB) ( 523 )   Save
    Olive leaves were fermented by Aspergillus niger, Geotrichum candidum, Aspergillus oryzae, Candida utilis, Candida tropicalis, and Trichoderma viride. The effects of the single and the combination of two strains on the cellulase activity(β-glucosidase, CMCase and filter paper activity), protein content, and total tannins content were investigated. The results indicated that the best fermented efficiency for single strain of olive leaves fermented feedstuff was A.niger, with a result of β-glucosidase activity 10.53 U/mL, CMCase activity 10.61 U/mL and filter paper activity 4.02 U/mL when they were fermented for 3 days. The highest protein content 14.61% for 5 days and the highest tannins degradation 84.14% for 7 days were achieved. The best fermented efficiency by mixed strains of olive leaves fermented feedstuff was the combination of A. niger and C. utilis with a ratio of 1:1(v/v). The highest cellucase activity(β-glucosidase activity 12.45 U/mL, CMCase activity 12.59 U/mL, filter paper activity 5.51 U/mL) was obtained by the mixed strains(1:1) in need of 5 days. When the fermented time reached 7 days, the protein content reached 18.63% and total tannic degradation was 86.49% in the fermented product.
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    Preparation of Hydroxytyrosol by Enzymatic Hydrolysis of Oleuropein from Olea europaea L. Leaf Extract
    YUAN Jiao-jiao, YE Jian-zhong, DAI Ming-ming, LI Wen-jun, ZHANG Hong-yu, WANG Cheng-zhang, LIU Yu-hong
    2015, 35 (4):  65-71.  doi: 10.3969/j.issn.0253-2417.2015.04.011
    Abstract ( 646 )   PDF (948KB) ( 553 )   Save
    The hydroxytyrosol(HT) was prepared from oleuropein(OE) in the olive leaves by enzymatic hydrolysis. The qualitative and quantitative determination of OE and HT from the olive leaf extract were analysed by HPLC, and the best enzyme to hydrolyze OE for HT from olive leaf extrct was selected. Moreover, the optimal technology of enzymatic process was obtained by single factor test and orthogonal test. The DPPH radical scavenging effects of HT, OE and olive leaf extract were examined, too. The results showed that hemicellulase was the best enzyme to hydrolyze OE for HT in the same enzymatic activity from 10 enzymes, and the cellulase and β-glucosidase were second. The optimal conditions were temperature 60 ℃, pH value 5.5, enzyme quantity 40 mg and time 6 h. The degradation rate of OE was 85.28 %, and HT content was 6.07 % by the best enzymatic process. Furthermore, HT was obtained by acid- and base-treatment, respectively. Acid hydrolysis performance (7.41 %) was better than enzymatic hydrolysis, and base-treatment result(4.09 %) was the worst. By comparison of the two methods, it was found that enzymatic condition was mild and could reduce the catalyst use, and it is a new hydrolysis method to further develop and utilize. The IC50 of HT was 1.07 mg/L, and the radical scavenging effect was in the order of HT> Vc> OE> BHT> olive leaf extract. Therefore, HT has a good ability of anti-oxidation compound.
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    Ultrasonic-assisted Synthesis of Cellulosic Oligosaccharide Esters Surfactant Catalyzed by K2O/C
    WANG Kui, JIANG Jian-chun, LU Xin-cheng, XU Jun-ming, LIANG Xin-yu
    2015, 35 (4):  72-78.  doi: 10.3969/j.issn.0253-2417.2015.04.012
    Abstract ( 519 )   PDF (1038KB) ( 513 )   Save
    The solid base catalyst K2O/C was prepared by the vacuum impregnation method. The orthogonal experiment was employed to optimize the preparation condition.The results indicated that the optimal reaction parameters were carbon carrier with average pore size 2.87 nm, K2CO3/C mass ratio 0.5, catalyst calcination temperature 450 ℃, and calcination time 2 h. The prepared catalyst K2O/C was adopted to catalyze the transesterification reaction of cellulosic oligosaccharide esters from cellulosic oligosaccharide and methyl oleate under ultrasonic assistance. The optimum conditions were obtained as follows: the ultrasonic frequency 20 kHz, the ultrasonic power 150 W, treatment time 15 min, the mole ratio of methyl oleate to cellulosic oligosaccharide esters 2:1, the mass fraction of K2O/C 5%, the reaction temperature 125 ℃, and the reaction time 2 h. Under these conditions, the yield of cellulosic oligosaccharide esters reached 85.6%. The synthesized product has esterification degree 18.8%, HLB 9.89, surface tension 32.1 mN/m, and the emulsifying ability 28.1%. The product showed good performance on surface tension, emulsion and stability in hard water.
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    Influence of Ionic Liquids Treatment on Enzymatic Bleaching Properties of Pulp
    LI Feng-feng, CHEN Jia-chuan, PANG Zhi-qiang, YANG Gui-hua, ZHANG Zhi-li
    2015, 35 (4):  79-84.  doi: 10.3969/j.issn.0253-2417.2015.04.013
    Abstract ( 537 )   PDF (1187KB) ( 435 )   Save
    Using aspen alkaline peroxide mechanical pulp (APMP), chemithermomechanical pulp (CTMP), kraft pulp (KP) and wheat straw CTMP as material, before enzymatic bleaching, the pulp was moderately pretreated by ionic liquids of BmimCl 1.0%(relative to the amount of dry pulp, the below was the same ) and EmimDMP 1.2%, respectively. The results showed that ionic liquids could optimize the pulp enzymatic bleaching properties, and EmimDMP gave better results. The whiteness of poplar kraft pulp(KP) increased by 4.27 %(ISO), opaqueness increased by 2.46%, and the tensile index, burst index, ring crush index, tear index as well as the folding number of wheat straw chemithermomechanical pulp(CTMP) forming paper increased by 12.21 %, 29.80 %, 22.45 %, 44.82 % and 52.50 %, respectively, after the pretreatment of EmimDMP. The fiber quality analysis(FQA), X-ray diffraction(XRD), and scanning electron microscope(SEM) were employed to characterize its properties. After pretreated with ionic liquid, there was a improvement of fiber quality with the average length increasing, the fines content reducing, and the fiber crystalline increasing. The crystalline of EmimDMP pretreated poplar KP increased by 11.21 %. The surface of pulp occured obvious fibrillation, and this phenomenon could increase the penetration of liquids.
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    Inhibitors Origination during Dilute Sulfuric Acid Pretreatment of Corn Stover for Ethanol Production by Co-fermentation
    JIANG Fa-xian, HUANG Ping, XU Yong, ZHU Jun-jun, YU Shi-yuan
    2015, 35 (4):  85-91.  doi: 10.3969/j.issn.0253-2417.2015.04.014
    Abstract ( 678 )   PDF (1172KB) ( 461 )   Save
    In order to solve the key technical bottleneck for fuel ethanol production regarding the removal of inhibitors during co-fermentation of hexose and pentose, four main non-lignin constituents of corn stover, including cellulose, hemicellulose, hot water extractives and ethanol extractives, were prepared and then treated with 0.75% dilute sulfuric acid at 180 ℃ for 40 min, respectively. 60 g/L glucose and 30 g/L xylose were added to these prehydrolyzates. 5 various ethanolic fermentation medium were fermented to produce ethanol by Candida shehatae, respectively. Thus, the influences on ethanolic co-fermentation and the origination of the key inhibitors were comparatively studied. The results showed that the degradation products formed from 133 g/L corn stover inhibited microbial glycometabolism and co-fermentation totally. During pretreatment of corn stover by dilute sulfuric acid products degraded from four non-lignin constituents reduce the ethanol yield at different extents. Additionally, the products released from the cellulose degradation can completely inhibit the xylose fermentation. Glucose and xylose could be completely inhibited by the degradation products from hemicellulose, and these products perform lethal toxicity to Candida shehatae as well. The products generated from hot water extractives and ethanol extractives exert inhibition on cell growth and sugars utilization. The key inhibitors were mainly from degradation reaction of cellulose and hemicellulose during the pretreatment of corn by stover dilute sulfuric acid. Besides formic acid, acetic acid, levulinic acid, HMF and furfural in corn stover prehydrolyzates, other unknown degradation products also presented toxicity or synergistic inhibition on ethanolic co-fermentation of hexose and pentose.
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    Fluid Characteristics and Cold State Experiment Validation of Novel Sump Type Fluidized Bed
    CHENG Yi, LIU Liu-jun, LI Rui
    2015, 35 (4):  92-96.  doi: 10.3969/j.issn.0253-2417.2015.04.015
    Abstract ( 570 )   PDF (895KB) ( 413 )   Save
    The flow equation for a novel fluidized bed reactor which contained solid particles was presented and validated by cold state experiment. The results indicated that the sump of the reactor formed by adding some relatively big particles could prolong the fluidized time effectively. Through resident rate test, its calculation was deduced as σ=-0.51lnu-0.4m/V+2.145. As the pressure drop consisted of pipe flow drop and resident drop owing to the resident effect and the resident drop, the resident rate was introduced into Ergun equation and the pressure drop equation was concluded as Δp=150(μu0/dp2)×(1-ε)2/ε3+7/4×(ρu02/dp)×((1-ε)/ε3)Le+(1-σ)(1-εb)Leρ. The experiment of cold state experiments showed that the model could match the flow state very well.
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    New Oxidation Bleaching Technology of Deresinated Montan Wax
    YUAN Cheng, ZHANG Hui-fen, ZHANG Mi, WEI Xi, LI Bao-cai
    2015, 35 (4):  97-104.  doi: 10.3969/j.issn.0253-2417.2015.04.016
    Abstract ( 755 )   PDF (940KB) ( 427 )   Save
    Using deresinated montan wax(DMW) of E'shan(ESDMW) from Yunnan province as the material, chroma value (L) as the main index, new oxidation bleaching of DMW were developed. The bleaching effects of three kinds of oxidation systems, i.e., peroxide (H2O2), peracetic acid (CH3COOOH) and H2O2/CH3COOOH system, were investigated. The results showed that H2O2/CH3COOOH system was better than the single systems of H2O2 and CH3COOOH. The main process parameters in H2O2/CH3COOOH system was optimized using the response surface method. The optimal conditions were m(CH3COOOH):m(ESDMW) 20:1, m(H2O2):m(ESDMW) 36.7:1, time 80 min and temperature 118.5 ℃. Under these conditions, the L value of the product was 62.02, which was almost consistent with the model prediction. The joint use of H2O2/CH3COOOH system with the Cr6+ was explored. The results showed that the bleaching effect of the joint use of Cr6++CH3COOOH/H2O2 was better than any other methods used before. More importantly, under the premise of better bleaching effect, the dosage of Cr6+ was significantly reduced by the optimized process.
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    Thermal Property and Migration of Polyvinyl Chloride Plasticized with Polyester Based on Soybean Oil
    JIA Pu-you, BO Cai-ying, ZHANG Meng, HU Li-hong, ZHOU Yong-hong
    2015, 35 (4):  105-111.  doi: 10.3969/j.issn.0253-2417.2015.04.017
    Abstract ( 525 )   PDF (1923KB) ( 536 )   Save
    The soybean oil based polyester was synthesized by the polycondensation of o-phthalic anhydride and the soybean oil monoglyceride obtained from the transesterification of soybean oil and glycerol at 230-240 ℃. The soybean oil polyester was characterized by gel permeation chromatography (GPC) and FT-IR. And the synthesized soybean oil polyester was then blend with polyvinyl chloride(PVC)to form a plasticized PVC. Thermodynamic properties, plasticizer migration stability and mechanical properties of soybean oil polyester plasticized PVC were investigated. The results showed that relative molecular mass of the polyester was 3 541. The thermal degradation temperature of the plasticized PVC was 256.1 ℃. And tensile strength and elongation at break for this plasticized PVC could reach 6.5 MPa and 230.3%, respectively. In addition, the combination of soybean oil polyester and dioctyl phthalate(DOP) using as complex plasticizer to plasticize PVC was also evaluated. The migration ratio of these complex plasticizers in distilled water, acetic acid solution, ethanol solution, petroleum ether and olive oil reduced to 0.18%,0.22%,0.28%,0.83% and 0.34%, which was indicative of their excellent migration property. Herein, the thermal and mechanical properties of the soybean oil polyester plasticized PVC could maintain for long time and the potential harm to human caused by plasticizer could be reduced at same time.
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    Synthesis Process of Castor Oil Glycidyl Ether
    WANG Fang, WANG Chuan-zhu, KUAI Jun-tao, LI Da-qian, ZHU Xin-bao
    2015, 35 (4):  112-116.  doi: 10.3969/j.issn.0253-2417.2015.04.018
    Abstract ( 1203 )   PDF (768KB) ( 618 )   Save
    Using castor oil and epoxy chloropropane(ECH) as the main raw materials under the alkali condition, a novel castor oil glycidyl ether (COGE) was synthesized through two steps, namely open loop and closed loop reaction. The effects of process conditions on epoxy values were investigated. The results showed that the highest epoxy value the product achieved was 1.56 mmol/g under the condition that the open loop reaction was set at 0.4% catalyst dosage,3.5 molar ratio of ECH and castor oil, and reaction temperature at 60 ℃ for 5 h, and as well as the close-loop reaction was set 0.4% catalyst dosage, 1.1 molar ratio of NaOH and ECH, and reaction temperature at 60 ℃ for 6 h. The chemical structure of the castor oil glycidyl ether was characterized by FT-IR and 1H NMR. TGA analysis showed that castor oil glycidyl ether had good thermal stability at high temperature. Viscosity test showed that the product could reduce the viscosity of epoxy resin.
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    Preparation Cochineal Dye Derivative by DDSA Esterification
    LIU Lan-xiang, ZHENG Hua, ZHANG Wen-wen, CHEN Qi, SONG Guo-bin, ZHANG Hong
    2015, 35 (4):  117-124.  doi: 10.3969/j.issn.0253-2417.2015.04.019
    Abstract ( 910 )   PDF (1182KB) ( 499 )   Save
    Oil-soluble cochineal dye derivative was obtained through molecule esterification of carminic acid with dodecyl succinicanhydride (DDSA). Based on the results of the single factor experiments, response surface methodology was applied to further optimize the pretreatment conditions. The obtained optimal conditions were raw materials 0.5 g, the quality ratio of DDSA and cochineal dye 2.3, the dosage of the catalyst triethylamine 1.8 mL, temperature 67 ℃, reaction time 6 h, and solvent N, N-dimethyl formamide 20 mL. Under these conditions, the product yield was 41.59%. The structure of the product was characterized by FT-IR and UV-Vis. The results showed that esterification reaction happened between DDSA and cochineal dye. The λmax and color of target product was strongly influenced by pH in alkaline solution. The product presented good solubility in corn oil, dyeing effect and stability with the solubility of 6.53 in oil (20 ℃). The solubility of cochineal red pigment was improved effectively.
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    Optimization of Semisynthetic Myricetin from Dihydromyricetion by Response Surface Process
    LIU Tong-fang, YU Hua-zhong, CHEN Yan-mei, WANG Ting
    2015, 35 (4):  125-130.  doi: 10.3969/j.issn.0253-2417.2015.04.020
    Abstract ( 842 )   PDF (1038KB) ( 630 )   Save
    Dihydromyricetion(DMY), which was abundant and easily extracted from the leaves of Ampelopsis grossedentata, was used as the semisynthetic sources for myricetin(MYR). The structure of MYR was characterized by IR, 1H NMR and 13C NMR. Based on the results of the single factor experiments, response surface methodology(RSM) was applied to further optimize the synthesis conditions with pyridine volume fraction, and temperature, solid-liquid-ratio as the impact factors and MYR yield as the response value. The most suitable synthesis conditions of MYR were determined as follows: pyridine volume fraction 66.6%, temperature 90.4 ℃ and solid-liquid ratio 20.88(g:L). The MYR yield was 76.63%, and the relative error with the predictive value of 76.48% was 0.19%.
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    Optimization of Medium for Production of Geraniol by the Recombinant Escherichia coli
    TIAN Ning, XIAN Mo, HU Yang-dong, LIU Wei
    2015, 35 (4):  131-137.  doi: 10.3969/j.issn.0253-2417.2015.04.021
    Abstract ( 787 )   PDF (893KB) ( 709 )   Save
    The Plackett-Burman experiment, the steepest ascent experiment and the central composite design were used to optimize the fermentation medium for the production of geraniol by the recombinant E.coli. Firstly, Plackett-Burman design was used to screen the critical factors which influenced the geraniol production from seven mediums. Secondly, the method of steepest ascent was adopted to make the key factors approach the optimal response area. Finally, the optimal concentration of key factors and regression model were obtained by central composite design. It was indicated that ammonium ferric citrate, MgSO4, and trace element solution were identified to be the significant factors and the it optimal concentrations were 0.13 g/L, 2.12 g/L, and 16.7 mL/L, respectively. The geraniol concentration increased to 223.24 mg/L under these conditions. It was about 3.26 times more than that of before.
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    Production of High Value-added Chemicals by Catalytic Fast Pyrolysis of Biomass
    YAO Qian, XU Lu-jiang, ZHANG Ying
    2015, 35 (4):  138-144.  doi: 10.3969/j.issn.0253-2417.2015.04.022
    Abstract ( 768 )   PDF (1038KB) ( 634 )   Save
    Catalytic fast pyrolysis of biomass is a technology for the conversion of biomass. It could obtain high value-added chemicals enriched in the pyrolysis products through the directional catalytic system during pyrolysis process. In this paper, reaction pathways and mechanisms of biomass fast pyrolysis are introduced.Different catalytic systems for the production of various high value-added chemicals from catalytic fast pyrolysis are reviewed. The prospect of catalytic fast pyrolysis technology is also discussed.
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    Research Progress on Catalytic Technologies for Production of Polyols from Cellulose
    LI Qiao-guang, LIU Shi-wei, YU Shi-tao
    2015, 35 (4):  145-150.  doi: 10.3969/j.issn.0253-2417.2015.04.023
    Abstract ( 561 )   PDF (811KB) ( 425 )   Save
    The recent research progress of coupling reaction of cellulose hydrolysis-hydrogenation for production of polyols was reviewed. The transformation of cellulose to polyols in different catalysis systems,i.e. three composite catalytic systems by combination of acid, hot water, and ionic liquid with the catalysis of metal hydrogenation catalyst were introduced. Their development prospects were given as well. This paper provides an important reference for the theory research and technology development of polyols generated from cellulose.
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    Research Progress on Extraction, Purification and Biological Activities of Rosmarinic Acid
    CHENG Xian, BI Liang-wu, ZHAO Zhen-dong, XIA Tian-juan
    2015, 35 (4):  151-158.  doi: 10.3969/j.issn.0253-2417.2015.04.024
    Abstract ( 709 )   PDF (1181KB) ( 725 )   Save
    Rosmarinic acid as a very strong antioxidants exists in rosemary with a high content. It has various biological activities such as anti-biotic, anti-inflammatory, anti-virus and anti-cancer activities. In order to offer more information for large-scale preparation and application, a brief review is presented on the extraction, purification methods. The biological activities of rosmarinic acid,such as antibiosis, antivirus, anti-oxidation, radical-scavenging, anti-inflammatory, immunoregulation, protecting nervous system, anti-radiation, antitumor, inhibition of xanthine oxidase and protection of livers and lungs are particularly discussed.
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