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    31 July 2016, Volume 50 Issue 4 Previous Issue    Next Issue
    Synthesis and Characterization of Fenchyl Oxalate
    YUAN Xiao-min, ZHAO Zhen-dong, XU Shi-chao, LU Yan-ju, ZHU Shou-ji
    2016, 50 (4):  1-5.  doi: 10.3969/j.issn.1673-5854.2016.04.001
    Abstract ( 752 )   PDF (710KB) ( 697 )   Save
    Fenchyl oxalate was synthesized by the reaction of α-fenchyl alcohol and oxalyl chloride.The influences of reaction conditions on the esterification were studied.The optimum conditions of the esterification were the molar ratio of oxalyl chloride and fenchyl alcohol 0.6:1.0, reaction temperature 55℃ and reaction time 10h.Under these conditions, the yield of fenchyl oxalate was 93.9%.After recrystallization, the purity could be 99.9%.And the structure of fenchyl oxalate was characterized by GC-MS, IR, 1H NMR and 13C NMR.
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    Electrochemical Catalytic Steam Reforming of m-Cresol with Ni-CeO2/γ-Al2O3 Catalyst
    RAN Ze-peng, LU Qiang, WANG Xin, HU Bin, DONG Chang-qing
    2016, 50 (4):  6-12.  doi: 10.3969/j.issn.1673-5854.2016.04.002
    Abstract ( 516 )   PDF (835KB) ( 612 )   Save
    m-Cresol was selected as the oxygenated model compound of biomass gasification tar to study the electrochemical catalytic steam reforming using the Ni-CeO2/γ-Al2O3 as catalyst. Experiments were carried out to reveal the effects of electric current intensity and reforming temperature on the m-cresol conversion, product gas composition and carbon deposition of the catalyst. In addition, the stability tests at 600℃ were conducted to evaluate the stability of the catalyst and the improving effect of the electric current on the catalyst stability.The results indicated that the electrochemical catalytic method significantly improved the reforming efficiency of the m-cresol.The conversion rate reached ashigh as 99.7% at 700 ℃ and electric current of 3A with 2.4g catalyst in the vertical tube furnace.The elevation of the temperature and current intensity could increase the CO volume fraction, and decrease the concentrations of CO2 and H2.Furthermore, the presence of the electric current also reduced the carbon deposition on the catalyst and enhanced the stability of the catalyst.
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    Synthesis and Characterization of γ-Acrylpimaric Acid
    LU Yan-ju, ZHANG Hai-bo, ZHAO Zhen-dong, WANG Mi-xia, WANG Jing, CHEN Yu-xiang
    2016, 50 (4):  13-20.  doi: 10.3969/j.issn.1673-5854.2016.04.003
    Abstract ( 567 )   PDF (1765KB) ( 623 )   Save
    Acrylic-modified rosin was synthesized by Diels-Alder reaction using resin acid and acrylic acid as raw materials.The gas chromatography(GC) was employed in analyzing the content of acrylpimaric acid which was the main constituent of acrylic-modified rosin.And the optimum reaction conditions were resin acid 10g, reaction temperature 230℃, microwave energy 400W, reaction time 90min, and n(acrylpimaric acid):n (resin acid) 2:1.Under the optimum conditions, the GC content of acrylpimaric acid was 78.4%, and the conversion rate of abietic-type acid was up to 98.6%. γ-Acrylpimaric acid was isolated by controling pH value and silica gel column, and the GC content of the purified product was 95.7%.The structure of the γ-acrylpimaric acid was characterized by GC, GC-MS, FT-IR, 1H NMR, and 13C NMR.The glass transition temperature and the thermal decomposition temperature of γ-acrylpimaric acid were 79.78℃ and 335.9℃ by DSC and TG analysis, respectively.
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    Preparation and Characterization of Carboxyl Modification Cellulose Gel Beads
    LI Jing, LIU Zhi-ming, YU Hui, ZHANG Xue
    2016, 50 (4):  21-25.  doi: 10.3969/j.issn.1673-5854.2016.04.004
    Abstract ( 748 )   PDF (1202KB) ( 871 )   Save
    Regenerated cellulose solution was obtained by NaOH/urea system using microcrystalline cellulose as raw materials.Cellulose hydrogel bead was prepared by titration suspension method.Carboxyl modified cellulose hydrogel bead was obtained by oxidation treatment of TEMPO/NaBr/NaClO selective oxidation system and carboxyl modified cellulose aerogel bead was obtained by freeze drying.The results showed that water content of carboxyl modified cellulose hydrogel bead was 95.64%.After adsorption for 4 hours, the adsorption capacity of methylene blue was 6.97mg/g.The characterization analysis results of Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy(SEM) of carboxyl modified cellulose aerogel bead showed that CO stretching vibration absorption peak was appeared at 1600cm-1, and TEMPO selective oxidation played a carboxyl modification role in the samples.The surface permeability of spherical aerogel was increased by carboxyl modification and the interior still presented network structure.The density of carboxyl modified cellulose aerogel bead was 0.038g/cm3.
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    Synthesis of Tributyl Citrate Catalyzed by Heteropolyacid Salt
    JIANG Guang-ping, WANG Hong-bo, LUO Feng
    2016, 50 (4):  26-30.  doi: 10.3969/j.issn.1673-5854.2016.04.005
    Abstract ( 605 )   PDF (527KB) ( 617 )   Save
    Three kinds of heteropolyacid salts, i.e., 1-(3-sulfonic group) propyl-3-methyl imidazolium phosphomolybdate ([MIMPS]3PMo12O40), 1-(3-sulfonic group) propyl-3-methyl imidazolium phosphotungstate ([MIMPS]3PW12O40) and 1-(3-sulfonic group) propyl-3-methyl pyridine phosphotungstate ([PyPS]3PW12O40), were synthesized.And the tributyl citrate (TBC) was synthesized with these three kinds of heteropolyacid salts as catalyst, in which [MIMPS]3PMo12O40 performed the best catalytic property.The effects of various reaction conditions were investigated with [MIMPS]3PMo12O40 as catalyst.The results showed that the esterification rate 98.3% was obtained under the optimum esterification conditions as follows: n(butanol):n(citric acid)=4.5:1.0, reaction temperature 130℃, reaction time 3.5h and the weight of catalyst 5%.The catalysis could be reused five times with the esterification rate still above 94%.
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    Process Resrarch of Multi-stage Enzymatic Hydrolysis of NaOH-Fenton Pretreated Mulberry Wood
    WANG Yan-yun, WU Kai, LEI Fu-hou, YANG Jing
    2016, 50 (4):  31-36.  doi: 10.3969/j.issn.1673-5854.2016.04.006
    Abstract ( 660 )   PDF (709KB) ( 717 )   Save
    During the multi-stage enzymatic hydrolysis of lignocellulosic materials, the product inhibitions were reduced by the removal of end products at each stage to enhance the hydrolysis efficiency and shorten the hydrolysis time with NaOH-Fenton pretreated mulberry as raw material. During the three-stage (8+8+8h) hydrolysis, as the enzymatic dosage was 15FPIU/g(calculated by the mass of cellulose, similarly here in after), enzymatic average reaction rate increased from 1.25 to 2.21g/(L·h) at the first stage, and after the second stage, it reached 1.54g/(L·h) and increased rapidly by 73% comparing with that of unsegmented hydrolysis.When enzymatic dosage was 40FPIU/g, the three-stage (8+8+8h) hydrolysis could reach 88.08%.Multi-stage hydrolysis made full use of the absorbed cellulase on substrate.The classical Langmuir adsorption isotherm was used to fit the cellulase enzyme adsorption on substrates.The adsorption capacity of cellulase on NaOH-Fenton pretreated mulberry was studied with the maximum adsorption capacity of 8.08mg/g substrate.The adsorbed sites were enhanced in the pretreatment process.
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    Pretreatment of Waste Paper Pulp and Enzymatic Hydrolysis Properties
    YANG Shu-juan, YOU Yan-zhi, BU Ling-xi, LI Xiao-li, JIANG Jian-xin
    2016, 50 (4):  37-41.  doi: 10.3969/j.issn.1673-5854.2016.04.007
    Abstract ( 635 )   PDF (640KB) ( 801 )   Save
    In order to study the effects of various pretreatments(Na2SO3, H2O2 and HCl) on enzymatic hydrolysis of deinking waste paper pulp, the hydrolyses were carried out with the pretreated pulp as substrate and cellulase and cellobiase as hydrolytic enzyme.It was concluded that three pretreatment methods could increase glucose yield by improving the content of cellulose, inceasing the specific area and disrupting its structure.Compared with the yield of raw pulp, the highest yield was achieved with the hydrolysis of hydrogen peroxide pretreated deinking waste paper pulp (91.67%), closely followed by sodium sulfite (87.57%) and dilute acid pretreatment (82.49%).
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    Purification of Polyphenols from Koelreuteria paniculata Laxm. Leaves by Macroporous Resin
    LI Yan-fang, GAO Cai-xia, HAN Xiang-en
    2016, 50 (4):  42-46.  doi: 10.3969/j.issn.1673-5854.2016.04.008
    Abstract ( 490 )   PDF (508KB) ( 1006 )   Save
    The absorption and desorption behaviors of seven macroporous resins for polyphenols from Koelreuteria paniculata Laxm. were investigated. The 24h static adsorption capacity and desorption rate of AB-8 resin was 13.74mg/g and 98.35%, respectively. The static adsorption and desorption equilibrium time of AB-8 resin was both less than 3h. The optimum conditions of dynamic absorption and desorption by AB-8 were sample mass concentration 4g/L, sample pH value 6, and volume fraction of ethanol 60%, elution speed 1mL/min, respectively.Under these conditions, the adsorption rate was 88.21% and desorption rate was 89.91%.The purity of polyphenols from Koelreuteria paniculata Laxm. increased from 50.36% to 72.37% after purification using AB-8 resin and the recovery rate was 86.83%.
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    Research Progress of Cellulose Catalytic Conversion for Preparation of 5-HMF in Different Solvents
    YANG Yan-ping, SHEN Ming-gui, SHANG Shi-bin, SONG Zhan-qian
    2016, 50 (4):  47-52.  doi: 10.3969/j.issn.1673-5854.2016.04.009
    Abstract ( 638 )   PDF (469KB) ( 831 )   Save
    Cellulose could be converted into the platform compound 5-hydroxymethylfurfural(5-HMF) directly through chemical conversion. Effective dissolution of cellulose was a long and difficult task in the process of preparing 5-HMF from cellulose through catalytic conversion. In this paper, the research progress of catalytic conversion of cellulose to 5-HMF in different solvents was reviewed, and the future research was prospected.
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    Process of Conversion of 5-Hydroxymethylfurfural and Levulinic Acid to Biomass-based Chemicals
    ZHU Shi-lin, LI Jing-dan, JIANG Xiao-xiang, YANG Hong-min, JIANG Jian-chun, ZHANG Ai-ling
    2016, 50 (4):  53-59.  doi: 10.3969/j.issn.1673-5854.2016.04.010
    Abstract ( 854 )   PDF (642KB) ( 869 )   Save
    The processes of the conversion of biomass-based platforms molecules 5-hydroxymethylfurfural(HMF) and levulinic acid(LA) to chemicals were reviewed.This paper mainly included HMF to 2, 5-furandicarboxylic acid, 2, 5-diformylfuran and 2, 5-dimethylfuran and LA to esters, acids, pyrrolidione and diphenolic acid.The use, producing process and the existing problems were briefly introduced.The object of this paper aimed to provide the guiding significance for developing the industrial production process of bio based chemicals from biomass platform molecules.
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    Combustion Characteristics and Pollutants Emission of Biomass Pellet Fuels
    SONG Jiao, YANG Bo
    2016, 50 (4):  60-64.  doi: 10.3969/j.issn.1673-5854.2016.04.011
    Abstract ( 943 )   PDF (442KB) ( 976 )   Save
    The combustion characteristics and pollutants emission of biomass pellet fuels were reviewed.The combustion process, ignition, burnout and slagging characteristics were summarized.The emissions of nitrogen oxide, sulfur dioxide, and particulate matter, together with chloride, dioxins, polycyclic aromatic hydrocarbons, etc. in the combustion process were discussed.And the feasible methods to reduce the pollutant emissions were proposed.According to the nature of biomass pellet fuels in China, the future research directions were prospected.
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    Research Progress of Catalyst for Esterification and Polymerization of Rosin
    MIAO Shou-ling, YU Shi-tao
    2016, 50 (4):  65-68.  doi: 10.3969/j.issn.1673-5854.2016.04.012
    Abstract ( 1014 )   PDF (393KB) ( 953 )   Save
    In this paper, a comprehensive overview of the catalysts in the esterification and polymerization of rosin was made.The advantages and disadvantages of the catalysts were discussed at the same time.The applications of the modified rosin were prospected. According to the aim of green technology for esterification and polymerization of rosin, the future development of inexpensive, environmentally friendly, highly active catalyst was considered as research focus of the above of reactions.
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