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    25 April 2019, Volume 39 Issue 2 Previous Issue    Next Issue
    Research Progress in Development and Application of Terpenoid Botanical Herbicides
    Shichao XU,Xiaojing ZENG,Huanhuan DONG,Zhendong ZHAO
    2019, 39 (2):  1-8.  doi: 10.3969/j.issn.0253-2417.2019.02.001
    Abstract ( 666 )   HTML ( 3397 )   PDF (827KB) ( 855 )   Save

    In this paper reviewed the recent research progress of terpene compounds and their derivatives in the application field of herbicides were reviewed. From the perspective of herbicidal application of natural terpenoid essential oil, pure terpenoid compounds and terpenoid derivatives, the exploration and application of terpene-based botanical herbicides in recent years were systematically induced and summarized. On this basis, the research status and achievements for the synthesis and herbicidal application of turpentine monoterpene derivatives were focused. The development direction and application prospect of terpene type botanical herbicides were also forecasted.

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    Synthesis and Electrochemical Properties of Larch-based Carbon Spheres via Spray Pyrolysis
    Yulong SONG,Wei LI,Zhou XU,Shouxin LIU
    2019, 39 (2):  9-15.  doi: 10.3969/j.issn.0253-2417.2019.02.002
    Abstract ( 602 )   HTML ( 5 )   PDF (6918KB) ( 548 )   Save

    Larch-based carbon spheres (LCSs) were prepared via spray pyrolysis with larch sawdust as raw materials. Larch-based resin obtained by liquefied larch wood powder and formaldehyde was used as carbon precursor. The effects of different carbonization temperatures and mass fractions of larch-based resin on the particle size, pore structure, specific surface area and electrochemical properties of LCSs were investigated. The surface morphology, pore structure, crystal structure and graphitization degree of LCSs were characterized by SEM, TEM, N2 adsorption-desorption, XRD and Raman. The electrochemical performance of the samples was investigated by electrochemical workstation. The results showed that the prepared LCSs were amorphous with regular spherical structures. The specific surface area of the LCSs3 fabricated at 900 ℃ was as high as 626.6 m2/g, with the pore volume 0.345 cm3/g. The specific capacitance was 309 F/g at current density of 0.2 A/g in 6 mol/L KOH electrolyte. When the current density increased to 5 A/g, its specific capacitance retention rate was 56%, indicating excellent rate performance.

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    High-efficiency Separation and Comprehensive Utilization of Deacidification and Dehydration Pyrolysis Liquid Products by Aspen Plus
    Hong CAO,Tingting QI,Rui LI
    2019, 39 (2):  16-24.  doi: 10.3969/j.issn.0253-2417.2019.02.003
    Abstract ( 559 )   HTML ( 9 )   PDF (1035KB) ( 647 )   Save

    The boiling point distribution of deacidified and dehydrated pyrolysis liquid phase product, separation process and the earnings of high value-added phenolic chemicals were analyzed. The process routes of graded distillation of the deacidified and dehydrated pyrolysis liquid phase product to prepare crude fuel oil, rich phenol oil and biological asphalt, as well as the process route for further separatmg rich phenol oil to prepare fine chemicals were put forward.Simulation results showed that the crude fuel oil, rich phenol oil and biological asphalt could be obtained by the initial separation for deacidified and dehydrated pyrolysis liquid phase product in distillation tower T-1 and T-2, and then by further distillation separation for the obtained rich phenol oil, 91.13% phenol, 94.58% o-cresol, medical raw materials (mainly including guaiacol 53.44%, 3-methylphenol 34.85%, diethyl malonate 11.56%), perfumery (2, 4-dimethylphenol 32.78%, 4-ethylphenol 26.03%, 4-methylguaiacol 31.85% and a small amount of other phenolic compounds), dye (allyl phenol 11.16%, 3-methylo-phenol 35.84%, 3-methylcyclopentane-1, 2- dione 41.56% and a small amount of other organics) and other fine phenolic chemicals are got. Calculation by the cost RMB 2 000 per ton of deacidified and dehydrated pyrolysis liquid phase product, energy consumption was RMB 497.41, total product price was RMB 5 362.20, gross profit of RMB 2 864.79 could got, which achieved the high efficient comprehensive utilization of deacidified and dehydrated pyrolysis liquid phase product.

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    pH Responsiveness and in vitro Performance of Urushiol/Amphiphilic Copolymer mPEG-PBAE Micelles
    Hao ZHOU,Zhiwen QI,Yulu MA,Chengzhang WANG
    2019, 39 (2):  25-32.  doi: 10.3969/j.issn.0253-2417.2019.02.004
    Abstract ( 821 )   HTML ( 73 )   PDF (1811KB) ( 691 )   Save

    With methoxy polyethylene glycol with terminal amino group (mPEG-NH2), tetradecyl amine, 5-amino-1-pentanol, 1, 4-butanediol diacrylate and 1, 3-pentanediamine diacrylate as raw materials, the amphiphilic polymer poly (ethylene glycol)-poly (β-amino) ester (mPEG-PBAE) was synthesized by one-pot method. The structure, molecular weight and CMC of the amphiphilic polymer (mPEG-PBAE) were characterized by FT-IR, GPC and pyrene fluorescence probe. Using urushiol as the drug model molecule, the mPEG-PBAE polymer micelles loaded with urushiol were prepared by dialysis method. The particle size, Zeta potential and morphology of the micelles loaded with urushiol were characterized by TEM and DLS. The pH responsiveness, drug release and its in vitro antitumor activity were investigated. The results showed that the amphiphilic copolymer mPEG-PBAE was successfully prepared and the weight average relative molecular mass was 11 445, which was not significantly different from the designed theoretical relative molecular mass, the CMC value of the polymer was 18.25 mg/L. The entrapment efficiency was 82.29% and drug loading capacity was 23.21%, the appearance of drug loaded micelles was regular spherical structure, the size was uniform, and the average particle size was 160.1 nm. The Zeta potential value of drug loaded micelles was 33.6 mV, its particle size in the buffer solution of pH value 5.0 was significantly higher than that in solution of pH value 6.5 and 7.4, and had obvious pH responsiveness. When pH value was 5.0, the cumulative drug release rate in 72 h was 98.7%; when pH value was 6.5 and 7.4, the cumulative drug release rates in 72 h were 61.6% and 31.5%, respectively. The median inhibitory concentrations (IC50) of the drug loaded micelles on HepG2 and A549 tumor cells were 1.38 and 0.87 mg/L, respectively; which showed better in vitro antitumor activity than that of free urushiol.

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    Isolation and Identification of Water-soluble Components from Fig Fruit
    Shuxiao FENG,Hongtao ZHANG,Shuiyong WANG,Yongxin HU,Peiwen ZHU,Weiping YIN
    2019, 39 (2):  33-38.  doi: 10.3969/j.issn.0253-2417.2019.02.005
    Abstract ( 654 )   HTML ( 33 )   PDF (537KB) ( 824 )   Save

    Several water-soluble components from fig(Ficus carica Linn.) fruit were isolated and identified by column chromatography separation and purification techniques, and the structures were verified by modern spectroscopic methods (UV, IR, HRMS, 1H NMR and 13C NMR). Seven monomer compounds were isolated from the ethanol extract of F. carica pulp, as F. carica polysaccharide(F-1), lactose(1), arabinosyl epilactose(2), rhamnosyl cellobiose(3), vitamin C(4), docosahexaenoic acid(DHA, 5) and β-carotene(6). Compounds 2 and 3 were new oligosaccharides reported for the first time. Compounds 1-5 were isolated from F. carica fruit for the first time.

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    Preparation of Monodisperse Rosin-based Polymer Microspheres by Dispersion Polymerization
    Zenghui CHENG,Daihui ZHANG,Jifu WANG,Chunpeng WANG,Fuxiang CHU,Feng XU
    2019, 39 (2):  39-45.  doi: 10.3969/j.issn.0253-2417.2019.02.006
    Abstract ( 692 )   HTML ( 12 )   PDF (9079KB) ( 507 )   Save

    A new type of monodisperse microspheres consisted of poly (2-methacryloyloxyisopropanol ester of dehydroabietic acid) PDAGMA was prepared via dispersion polymerization in the presence of isopropyl alcohol/H2O, using 2-methacryloyloxyisopropanol ester of dehydroabietic acid (DAGMA) as a monomer, polyvinylpyrrolidone(PVP) as stabilizer, 2, 2′-azobis (2-methylpropionitrile) (AIBN) as an initiator. The influences of PVP content, monomer concentration and reaction temperature on the particle size and distribution of microspheres were investigated. Then, these microspheres were crosslined and bed used as an adsorption material. And the rutin adsorption performance was also investigated. FT-IR, 1H NMR, GPC and SEM were applied to characterize the structure, morphology and size of the microspheres, respectively. The results showed that the DAGMA monomer could polymerized in the alcohol/water medium. GPC analysis showed that the relative molecular weight of the polymer was about 55 000. The average diameter of the polymer microsphere was found to decrease with the increase of the amount of PVP. The polymer microsphere particle size decreased frist and then increased as the monomer concentration increased, as the reaction temperature increased, the polymer microsphere particle size also increased. By the optimize the polymerization techmology, monodispersed microspheres with particle size 1.37 μm and PDI 1.014 were obtained. Specially, the cross-linked rosin polymer microspheres exhibited an improved thermal stability and the adsorption capacity of rutin was 12.3 mg/g.

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    Synthesis and Antiviral Activity Evaluation of Dehydroabietic Acid Amide Derived 3, 4-Dihydropyrimidinthiones
    Yunlong LUO,Minggui SHEN,Zhaosheng CAI,Shibin SHANG,Zhanqian SONG
    2019, 39 (2):  46-52.  doi: 10.3969/j.issn.0253-2417.2019.02.007
    Abstract ( 510 )   HTML ( 7 )   PDF (804KB) ( 602 )   Save

    Dehydroabietic acid chloride was prepared via the reaction of dehydroabietic acid and thionylchloride, dehydroabietic acid acylthiosemicarbazide was synthesized by thiosemicarbazone and dehydroabietic acid chloride, followed by the reaction of dehydroabietic acid acylthiosemicarbazide, aromatic aldehydes with ethyl acetate to obtain ten dehydroabietic acid amide derived 3, 4-dihydropyrimidinones: 4-phenyl-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3a), 4-(4-methoxyphenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-di-hydropyrimidine-2-thione (3b), 4-(2-methoxyphenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimi-dine-2-thione (3c), 4-(4-methylphenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3d), 4-(4-bromophenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3e), 4-(4-p-tri-fluoromethylphenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3f). 4-(4-chlorophen-yl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3g), 4-(2, 6-dichlorophenyl)- 6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3h), 4-(2-nitrophenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-dihydropyrimidine-2-thione (3i), 4-(3-nitrophenyl)-6-methyl-1-dehydroabietic acid amide-3, 4-di-hydropyrimidine-2-thione (3j).The target compounds were characterized by FT-IR, MS, 1H NMR and 13C NMR. The cytotoxicity of these 3, 4-dihydropyrimidinone derivatives (compounds 3a-3j) were tested with monkey embryonic kidney cells (MA-104 cells). The antiviral activities against the Herpes simplex virus type Ⅰ (HSV-1) of these derivatives were further evaluated with methyl thiazolyl tetrazolium(MTT) method. The results indicated that the cytotoxicity of these derivatives kept in a low level, compounds 3a, 3b, 3d, 3e, 3h, 3i and 3j showed lower cytotoxicity than the drug ribavirin; compound 3j performed better inhibitory activity of HSV-1(50% inhibitory concentration(IC50) 0.465 g/L, selective index(SI)12.18) which was similar to ribavirin (IC50=0.156 g/L, SI=12.6), and the other compounds showed weak inhibitory activity of HSV-1.

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    Preparation and Characterization of Nitrogen-containing Heterocyclic Tung Oil-based Rigid Polyurethane Foam
    Wei ZHOU,Puyou JIA,Meng ZHANG,Yonghong ZHOU
    2019, 39 (2):  53-58.  doi: 10.3969/j.issn.0253-2417.2019.02.008
    Abstract ( 519 )   HTML ( 26 )   PDF (686KB) ( 721 )   Save

    Nitrogen-containing heterocyclic tung oil-based polyol (PTOT) was synthesized by the ring opening reaction between epoxidized eleostearic acid monoglyceride (EGTO) and 1, 3, 5-tris(2-hydroxyethyl) isocyanurate (THEIC). PTOT was used to substitute part of phthalic anhydride polyester polyol (PAPP) to prepare rigid polyurethane foam(RPUF). FT-IR, 1H NMR, TG and universal testing machine were employed to characterize the chemical structure and the properties of the products. It can conclude that PTOT was obtained by the ring opening reaction, and the hydroxyl value and viscosity (25 ℃), acid value and moisture of PTOT were 378.42 mg/g and 1.84 Pa·s, respectively. The acid value was lower than 0.8 mg/g and the moisture was lower than 0.1%.With the increase of PTOT substitution amount, the limiting oxygen index (LOI) of the RPUF was increased while the compressive strength and thermal stability were decreased. When the amount of PTOT increased from 0 to 100%, the LOI increased from 19.7% to 23.0%, the compression strength decreased from 0.85 MPa to 0.59 MPa and the initial degradation temperature decreased from 276.0 ℃ to 273.5 ℃, respectively. The introduction of an appropriate amount of cellulose into RPUF could enhance the mechanical strength and retain its flame retardancy and thermal stability without lowering.

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    Extraction, Purification and Property Analysis of Polysaccharides from Quercus acutissima
    Liming ZHANG,Rongxue LI,Xihong HE,Limin HAO,Zhina HE,Yujie DAI
    2019, 39 (2):  59-66.  doi: 10.3969/j.issn.0253-2417.2019.02.009
    Abstract ( 621 )   HTML ( 106 )   PDF (714KB) ( 779 )   Save

    In order to develop and utilize the polysaccharide from Quercus acutissima, the process parameters of hot water extraction of polysaccharides were studied and the purified polysaccharide was preliminarily analyzed. The extraction conditions including extraction time, temperature, the liquid to solid ratio and times of extraction were investigated by single factor experiment and response surface method with the yield of polysaccharides as index. The optimal extraction conditions were the extraction time 3h, the extraction temperature 90 ℃, the liquid to solid ratio 25:1 (mL:g), and the times of extraction 2. Under these conditions, polysaccharide yield was 2.65%. By using DEAE-52 and Sephadex G-200 column chromatography, two purified polysaccharides (OP-1, OP-2) were obtained. The results of ultraviolet and FT-IR spactra, showed that the purified OP-1 and OP-2 from Q. acutissima had high purity and the typical groups of polysaccharide. The composition analysis by HPLC with pre-column derivatization indicated that the OP-1, a neutral heteropolysaccharide, was mainly composed of xylose and glucose with the molar ratio of 0.86:0.7; the OP-2, an acidic heteropolysaccharide, was mainly composed of ribose, glucuronic acid, and arabinose with the molar ratio of 0.42:0.21:0.56. The results of high performance gel permeation chromatography (HPGPC-ELSD) indicated that the weight average molecular weights (Mw) of OP-1 and OP-2 were about 444.8 and 121.2 ku.

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    Preparation and Performance Characterization of Sodium Alginate/Cellulose Composite Microspheres
    Yanqing LI,Zhiming LIU,Xiaokai CHENG,Mengnan CAO,Jianan WANG
    2019, 39 (2):  67-72.  doi: 10.3969/j.issn.0253-2417.2019.02.010
    Abstract ( 763 )   HTML ( 10 )   PDF (7950KB) ( 556 )   Save

    The cellulose solutions were prepared with the cotton linter pulp dissolved in NaOH/urea aqueous system at low temperature and mixed with sodium alginate for the preparation of sodium alginate/cellulose composite micropheres(SACCM) by sol-gel transition. Then a series of SACCM, which could be preserved in water phase, were prepared by turning the ratio of cellulose and sodium alginate. The structure and properties of the microspheres were characterized by scanning electron microscopy(SEM), Fourier transform infrared spectrometer(FT-IR) and laser particle size analyzer. And the adsorption ability of the sodium alginate/cellulose composite microspheres to phosphate in water phase were evaluated. The results showed that all the composite microspheres were spherical with the average diameter of about 360 μm, and the microspheres exhibited three-dimensional network porous structure. FT-IR spectra showed that cellulose and sodium alginate were physically combined through hydrogen bonding and intermolecular interaction. The results of adsorption experiments showed that these composite microspheres had a strong adsorption capacity for phosphate in aqueous phase, and the adsorption capacity of phosphate on the composite microspheres increased with the increase of sodium alginate content. Among them, SACCM20 (mass fraction of sodium alginate 20%) had the strongest adsorption capacity for phosphate, and the adsorption efficiency could reach 85.58%.

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    Preparation, Characterization and Performance for Rosin Hydrogenation of Pd/mpg-C3N4 Catalyst
    Xiaohao LI,Congxia XIE
    2019, 39 (2):  73-80.  doi: 10.3969/j.issn.0253-2417.2019.02.011
    Abstract ( 627 )   HTML ( 99 )   PDF (5381KB) ( 713 )   Save

    Using SiO2 and melamine as raw materials, mesoporous graphitic carbon nitride(mpg-C3N4) was prepared by high-temperature baking method. Pd/mpg-C3N4 was then prepared by impregnating of Pd nanoparticles and used to catalyze the hydrogenation of rosin. XRD, FT-IR, TEM, ICP-AES, XPS, nitrogen adsorption-desorption and GC were used to analyze the structure, morphology, actual loading of Pd, metal valence, specific surface area, pore size and catalytic activity of the catalyst. The results showed that nano-Pd was successfully uniformly dispersed in the layered structure of carbon nitride. Pd/mpg-C3N4 still maintained the mesoporous structure after Pd loading. However, due to Pd loading, the BET surface area, pore volume and pore diameter of mpg-C3N4 were reduced to 47.73 m2/g, 0.17 cm3/g and 3.39 nm, respectively. Hydrogenated rosin products with 5.99% dehydroabietic acid and less than 1% abietic acid were obtained under the optimized conditions for the hydrogenation of rosin (7.96% Pd loading, 5 MPa H2, 150 ℃, 4 h). After four cycles for the catalyst, the GC content of tetrahydroabietic acid decreased from 37.12% to 24.71%, and the GC content of dehydroabietic acid increased from 5.99% to 9.76%.

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    Purification and Antioxidation Activity of Polyphenol from Cyrtomium fortune
    Huifang ZHANG,Ye WANG,Weichao HU,Shu YUAN,Ming YUAN
    2019, 39 (2):  81-88.  doi: 10.3969/j.issn.0253-2417.2019.02.012
    Abstract ( 469 )   HTML ( 105 )   PDF (665KB) ( 636 )   Save

    The polyphenols were extracted from Cyrtomium fortune with 70% ethanol, and then purified with 7 macroporous resins. The results showed that HPD100 resin had the best purification effect based on the adsorption rate and desorption rate. The effect of sample mass concentration, loading speed of sample, volume fraction of desorption ethanol, desorption speed and sample pH value on the purification of HPD100 resin was further analyzed, and the optimum purification conditions were obtained as follows: mass concentration of sample solution 2.00 g/L, pH value 5, loading speed of sample 1 mL/min, volume fraction of desorption ethanol 70% and desorption speed 2 mL/min. Under these conditions, the content of polyphenols increased from 27.64% to 54.00% (the yield of polyphenols was 6.46%). The purified polyphenols showed higher antioxidant activity. For the purified polyphenols, the IC50of DPPH radical (DPPH·) and hydroxyl radical (·OH) were 0.01 and 0.49 g/L, respectively; but for the crude polyphenols, the IC50 of DPPH· and ·OH were 0.05 and 1.79 g/L, respectively. At 0.04 g/L, the DPPH· scavenging activity of the purified polyphenols was 90.82%, almost similar to that of Vc. At 0.05 g/L, ferric ion reducing power of the purified polyphenols was 0.47, but the crude polyphenols was only 0.25. Furthermore, the purified polyphenols exhibited better DPPH· scavenging activity and ferric ion reduction ability under acidic conditions and the hydroxyl radical scavenging activity under alkaline condition.

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    Preparation of Micro-nanocellulose from Low Quality Fiber
    Wenzhang YIN,Jianqiang LI,Zhengmao XU,Chunhui ZHANG
    2019, 39 (2):  89-95.  doi: 10.3969/j.issn.0253-2417.2019.02.013
    Abstract ( 617 )   HTML ( 9 )   PDF (3144KB) ( 613 )   Save

    Pulp residue was used as raw material to prepare the dialdehyde cellulose(DAC) with sodium periodate oxidation method. The response surface method was used to optimize the preparation process of DAC. Then the microfibrillated cellulose (MFC) was prepared with dialdehyde cellulose through high-pressure homogenizer. Experimental results showed that when temperature, oxidant dosage and time corresponded to 48 ℃, 50% and 176 min respectively, the aldehyde group content of DAC would reach 947.38 μmol/g. After high-pressure homogenization treatment for 60 min, the average particle size of the MFC was 532 nm and the crystallinity was 27.13%. And MFC retained the structure of the cellulose, but the thermal stability was lower. The tensile strength and bursting strength of the paper could be increased 81.40% and 47.41%, respectively, whereas its air permeability was reduced by about 50% when adding 5% MFC in it. However, the opacity of paper was slightly improved when MFC as added.

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    Preparation and Properties of Wood Vinegar from Pyrolysis of Fir Sawdust Under Different Temperatures
    Xincheng LU,Jianchun JIANG,Jing HE,Kang SUN,Yunjuan SUN
    2019, 39 (2):  96-102.  doi: 10.3969/j.issn.0253-2417.2019.02.014
    Abstract ( 712 )   HTML ( 5 )   PDF (504KB) ( 628 )   Save

    The preparation and properties of wood vinegar obtained by pyrolysis of fir sawdust under different temperatures were studied. The results showed that the most important pyrolysis phase of fir sawdust was 150-250 ℃, which obtained the most of wood vinegar and organic compounds. Under this pyrolysis phase, the highest yield of organic compound was phenols, and followed with acids. The relative content of organic compounds in wood vinegar was increased with the increasing of prolysis temperature, which is up to 48% after 150 ℃. The relative content for each kinds of organic compounds was different under various temperature range, the highest relative content of acids was in 0-150 ℃, while phenols and ketones in 250-350 ℃, and aldehydes in 150-250 ℃.

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    Preparation of Walnut Shell Powders-supported Cu Nanoparticles and Its Application in Ynones Synthesis
    Xingquan XIONG,Yanlong WANG,Xu LIAO,Shilin LAI,Hui ZHANG
    2019, 39 (2):  103-108.  doi: 10.3969/j.issn.0253-2417.2019.02.015
    Abstract ( 522 )   HTML ( 6 )   PDF (785KB) ( 629 )   Save

    Walnut shell powders(WSPs), which were grinded from walnut shell, was used as supporter for the preparation of WSPs-supported copper catalyst(WSPs-Cu) by adsorption method. The heterogeneous catalyst WSPs-Cu was characterized by FT-IR, thermogravimetric analysis(TGA), X-ray diffraction analysis(XRD) and scanning electron microscopy/energy dispersive X-ray spectroscopy(SEM/EDS). The results showed that the WSPs-Cu catalyst was successfully prepared by this method. Copper were well distributed on the surface of WSPs. The copper content of the catalyst was 3.386% with good thermal stability within 100-200 ℃. The WSPs-Cu catalyst was used to prepare five ynones from benzoyl chloride derivatives and phenylacetylene via copper-catalyzed coupling reaction. The results revealed that ynones were synthesized under microwave irradiation and solvent-free conditions for 30 min at 40 ℃ by using triethylamine as acid-binding agent(61%-90%). The recyclability of WSPs-Cu was studied. It was found that the WSPs-Cu has high activity after using for five times and the yield was 79%. As the model reaction was amplified from trace to constant and the dosage of substrate was 80 mmol, the yield of ynone catalyzed by WSPs-Cu reached 82%.

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    Preparation of Hydroxypropylated Alkali Lignin and Its Effecton Hydrolysis Efficiency of Cellulase
    Cunyi ZHAO,Wenjun YING,Zhengjun SHI,Haiyan YANG,Zhifeng ZHENG,Jing YANG
    2019, 39 (2):  109-114.  doi: 10.3969/j.issn.0253-2417.2019.02.016
    Abstract ( 699 )   HTML ( 15 )   PDF (630KB) ( 659 )   Save

    Alkali lignin (AL) was modified by hydroxypropylationto obtain hydroxypropylated lignin (HL), and its effects on enzymatic hydrolysis and non-productive enzyme adsorption were further investigated. The results of Zeta potentials, X-ray photoelectron spectroscopy and hydrophobicity tests indicated that the surface charaoteristics of AL changed after hydroxypropylation. The surface negative charge increased and the surface elements distribution and chemical bonds composition changed greatly. The proportion of C—O and C—C═O bond increased, as well as the hydrophobicity decreased, resulting in the reducing of non-productive adsorption of cellulase onto HL, which significantly increased the enzymatic hydrolysis efficiency. Compared with these of Avicel with AL, the free enzyme protein of Avicel with 4 g/L HL increased by 152 % and the 72 h hydrolysis yield of glucose increased by 32.09%.

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    Separation of Unsaturated Fatty Acids by Melamine Inclusion Method
    Peiyan WANG,Yuanbo HUANG,Shouqing LIU,Zhifeng ZHENG,Delu NING
    2019, 39 (2):  115-121.  doi: 10.3969/j.issn.0253-2417.2019.02.017
    Abstract ( 636 )   HTML ( 3 )   PDF (968KB) ( 675 )   Save

    Separation of unsaturated fatty acids (UFAs), including monounsaturated (MUFAs) and polyunsaturated fatty acids (PUFAs) from mixed fatty acids (FAs) by melamine inclusion method were investigated. Effects of melamine/FAs mass ratio, crystallization inclusion temperature and inclusion time on yield, purification, and inclusion rate of UFAs were discussed. The melamine inclusion complex was characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) spectroscopy. Results showed that saturated fatty acids (SFAs) could be employed to form the inclusion crystallization (complex) in ethanol at low temperature by melamine. The optimized conditions were FAS 20 g, 95% ethand 96 mL, mass ratio of melanine and FAs (M/F) 0.9:1, dissolving at 75 ℃, inclusion at 9 ℃ for 7 h. Under these conditions, the maximum UFAs (yield of 60.83%, purity of 93.75%, and inclusion rate of 87.23%) were obtained. Compared with the ureainclusion method, the purity and inclusion rate of UFAs were higher, and MUFAs and PUFAs could be separated together from SFAs by melamine inclusion method. Compared with melamine crystals by structural analysis, the crystal structure of melamine inclusion complex with SFAs did not change, and SFAs could enter into melamine crystalline lamellae to form stable crystalline inclusion complex. After inclusion, melamine could be recycled, which would be promoted the further development of fatty acids separation.

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    Extraction and Properties Analysis of Polysaccharides, Extractum and Gutta-percha from Eucommia ulmoides Oliver Leaves
    Xiyu QUAN,Pai PENG,Peiyao WEN,Jinjin WEI,Junhua ZHANG
    2019, 39 (2):  122-128.  doi: 10.3969/j.issn.0253-2417.2019.02.018
    Abstract ( 597 )   HTML ( 10 )   PDF (699KB) ( 796 )   Save

    In order to extract bioactive components and gutta-percha effectively from leaves of Eucommia ulmoides Oliver, the successive extractions of the leaves by hot water, alkali, and enzyme-petroleum ether were used to obtain the extractum, polysaccharides(water-soluble polysaccharides and alkali-extracted polysaccharides) and gutta-percha, respectively. Effects of solid to liquid ratio and temperature on yields of bioactive components were investigated. Meanwhile, the effects of time and type of enzymes on enzymatic hydrolysis of the residues were discussed. Finally, the ferric reducing/antioxidant power and the scavenging DPPH radical activity of bioactive constituents, water-soluble and alkali-extracted polysaccharides were determined, and the molecular weights of gutta- percha were determined. The results showed that the highest yields of flavonoids and chlorogenic acid were 50.08 mg/g and 6.83 mg/g with solid to liquid ratio of 1:10 (g:mL)at 80 ℃. The water-soluble and alkali-extracted polysaccharides and extractum from E. ulmoides Oliver exhibited good antioxidant activity, in which the antioxidant activity of extractum was the highest. The total antioxidant activity of 5 g/L extractum was 4.01 mmol/L, and the scavenging rate of DPPH radical at 300 mg/L was 94.46%, which was the same as that of Vc. The hydrolysis rates of glucan and xylan were the highest when water-extracted residues of E. ulmoides leaves were hydrolysed for 48 h, which were 86.77% and 15.62%, respectively. The yields of extractum, water-soluble polysaccharides, alkali-extracted polysaccharides and gutta-pereha were 8.0%, 13.2%, 9.8%, 1.86%, respectively. The weight average relative molecular mass (Mw) and the number average relative molecular mass (Mn) of gutta-pereha were 330 398 and 84 526, respectively, which were higher than the molecular weights of polysaccharides. Meanwhile, Mw/Mn=3.91, and the dispersity of extractum was lower than that of polysaccharides.

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