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    30 November 2018, Volume 52 Issue 6 Previous Issue    Next Issue
    Antifeedant Activity of Rosin Nitrogen Derivatives Against Agrotis ypsilon 4 Instars and Its Structure Activity Relationship
    ZHAI Zhaolan, YAN Xinyan, XU Ji, SONG Zhanqian, SHANG Shibin, RAO Xiaoping
    2018, 52 (6):  1-7.  doi: 10.3969/j.issn.1673-5854.2018.06.001
    Abstract ( 462 )   PDF (871KB) ( 568 )   Save
    The antifeedant activities of four different kinds of rosin nitrogen derivatives against Agrotis ypsilon 4 instars were investigated by using the method of leaf disc. The results showed that dehydroabietylamine p-chlorine salicylaldehyde Schiff base(2i) and dihydroabietic isopropanol acyl thiourea(4b) could almost completely inhibit A. ypsilon 4 instars feeding, and the antifeedant rates of 2i and 4b were 86.12% and 85.13% at 1 g/L after 24 hours, respectively. In addition, dehydroabietylamine p-methoxy benzaldehyde Schiff base(2b), dihydroabietic 2-hydroxymethyl-1,3-propanediol acyl thiourea(4c) and dihydroabietic furna acyl thiourea(4g) showed strong antifeedant activities against A. ypsilon 4 instars and their antifeedant rates were 52.04%, 66.70% and 50.48%, respectively. The 50% antifeedant concentration(AFC50) for 2i was 0.04 g/L, which was quite low. The values of AFC50 for 2b, 4b, 4c and 4g were 0.66,0.25,1.47 and 0.69 g/L, respectively. Dehydroabietylamine benzaldehyde Schiff base and dihydroabietic acyl thiourea showed strong antifeedant activities against A. ypsilon 4 instars. Methoxy, chlorine atom and hydroxyl could efficiently increase the antifeedant activities of dehydroabietylamine benzaldehyde Schiff base. The position and number of hydroxyl groups in dihydroabietic acyl thiourea had obvious impact on its antifeedant activities. The changes in the structure of dehydroabietamide and dehydroabietic acyl thiourea had little influence on the antifeedant activities against A. ypsilon 4 instars.
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    Pyrolysis Characteristics and Kinetics of Shells Biomass
    FAN Fangyu, HUANG Yuanbo, YANG Xiaoqin, ZHENG Yunwu, LIU Can, WANG Zhen, ZHENG Zhifeng
    2018, 52 (6):  8-14.  doi: 10.3969/j.issn.1673-5854.2018.06.002
    Abstract ( 599 )   PDF (841KB) ( 607 )   Save
    Pyrolysis properties of forest shells biomass(macadamia nut shell, camellia tea shell and walnut shell) were studied by TG-DTG, and the kinetics were analyzed by distributed activation energy model(DAEM). Pyrolysis characteristics showed that the maximum weight loss rate of camellia tea shell was the minimum. Initial temperature, pyrolysis temperature and the end of the temperature for maximum weight loss rate were lower than those of macadamia nut shell and walnut shell. Pyrolysis characteristic values of macadamia nut shell and walnut shell were approximate, and pyrolysis process transferred from low temperature zone to high temperature zone with increasing the heating rate for three kinds of shell biomass. DAEM were suitable for studying the kinetics of pyrolysis of three kinds of shell biomass, and the correlation coefficients(R2) were 0.914-0.999. The activation energies of macadamia nut shell, camellia tea shell and walnut shell were 83.91-211.86 kJ/mol, 68.64-244.49 kJ/mol and 98.69- 267.75 kJ/mol, respectively. With the increase of conversion rate, the activation energies of three kinds of shell biomass showed the same change trend, but the range of change was different.
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    Preparation and Performance of Spherical Cellulose Nanofibril Aerogels
    LIU Shuang, ZHANG Yang, JIANG Hua, YAO Yuan, WANG Xiaoyu, ZHAO Hua
    2018, 52 (6):  15-22.  doi: 10.3969/j.issn.1673-5854.2018.06.003
    Abstract ( 466 )   PDF (7405KB) ( 346 )   Save
    Spherical cellulose nanofibril(CNF) aerogels with different CNF mass fraction(1%,1.5%,2% and 25%) were obtained with eucalyptus pulp as raw material. The resulting CNF aerogels were mainly characterized by scanning electron microscopy(SEM), automatic surface area and porosity analyzer(BET), Fourier transform infrared spectroscopy(FT-IR), combined multi-function horizontal X-ray diffraction(XRD) and thermogravimetric analyzer(TG). The results showed that the cellulose aerogels prepared in this experiment were spherical, the spherical CNF aerogels were mesoporous materials with three-dimensional network structure, and the densities were 0.024 8-0.042 7 g/cm3, porosity ≥ 97.33%, pore size ≤ 19.4 nm. The aerogels possessed the infrared characteristic peak of nanocellulose, and its crystal structure was still cellulose I type structure and had excellent thermal stability. When the CNF mass fraction was 2%, the maximum weight loss rate temperature(Tmax) was 306.52 ℃. With the increase of CNF mass fraction, the desity and porosity of CNF aerogels gradually decreased, the pore volume and BET specific surface area increased first and then decreased and the pore size decreased first and then increased.
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    Characteristic Analysis of Co-pyrolysis Products of Lignite and Soybean Pod
    LI Cuihua, HE Xuanming, LI Chong, FENG Dongzheng, LIU Jing, KE Ping
    2018, 52 (6):  23-30.  doi: 10.3969/j.issn.1673-5854.2018.06.004
    Abstract ( 410 )   PDF (2350KB) ( 536 )   Save
    The characteristics of co-pyrolysis products of lignite and soybean pod were studied by using homemade carbonization apparatus and the influences of different soybean pod ratios and blending Fe2O3 in lignite on the yields were also studied.The characteristics of co-pyrolysis products were analyzed by FT-IR, GC-MS, SEM-EDX and UV-vis, meanwhile, the char was used to study the adsorption of methylene blue.The results showed that the yield of pyrolysis tar rose to 11.98% with the blending ratio of 30%, which was increased by 44.86% compared to lignite pyrolysis alone and reached the most-positive deviation to the theoretical values(0.8%) and the results indicated that the addition of soybean pod had synergistic effect of promoting the production of tar.The addition of soybean pod could facilitate the breakage of oxygen-containing heterocycles, increase the number of straight-chain alkanes and reduce of aromatic compounds in co-pyrolysis tar. It could also enhance the quantity of oxygen-containing groups and the surface roughness of co-pyrolysis char. Blending of Fe2O3 increased the phenols and alcohols content in co-pyrolysis tar, and the folds of the char were more obvious. The methylene blue removal rate of co-pyrolysis char reached 33.62%, which was risen by 8.84% compared with that of coal char. And the removal rate of co-pyrolysis char with Fe2O3 reached 55.57%, which was risen by 65.29% compared with that of co-pyrolysis char.
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    Research on Phenol Liquefied Products of Peanut Shell-urea-formaldehyde Resin Adhesive
    HOU Xing'ai, SUN Fengwen, LIU Longlong, MI Ling
    2018, 52 (6):  31-37.  doi: 10.3969/j.issn.1673-5854.2018.06.005
    Abstract ( 514 )   PDF (858KB) ( 478 )   Save
    The phenol liquefied product of peanut shell was used as raw material to prepare the phenol liquefied product of peanut shell-urea-formaldehyde(PLPUF) resin adhesive. The optimal ratio of PLPUF resin adhesive was studied by orthogonal test, and its comprehensive performance was improved. The results showed that the substance ratios of first batch of urea(U1)/the second batch of urea(U2), liquefaction products(PL)/urea(U), and the total amount of liquefied product and urea(PL+U) to the amount of formaldehyde(F) were 3:1, 1:1.5 and 1:1, respectively, which were the best ratio of PLPUF resin adhesive preparation. Under these conditions, the ratio of the bonding strength reached 0.83 MPa, the solid content was 47.11%, and the free formaldehyde content was 0.05%. With the phenolic resin adhesive as the standard, the PLPUF resin adhesive could meet the requirements of the wood industry resin. The viscosity of PLPUF resin gradually increased as time went on. When the resin was stored for 5-15 days, the bonding strengths were 0.87-1.15 MPa. After 22 days, the bonding strength reduced to 0.74 MPa. Therefore, the conditions of use be met within 22 days. In the FT-IR spectra of PLPUF resin, the stretching vibration peaks such as amide C=O and C—N appeared, indicating that urea participated in the reaction and modified resin, and the FT-IR absorption peaks of the resin before and after the addition of the curing agent were the same. Combined with the DSC curve, the addition of the curing agent did not change the structure of PLPUF resin, but could improve the curing process of the PLPUF resin and decrease the curing temperature and reaction heat.
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    Preparation and Properties of Silicone Rubber Modified by Dehydroabietic Amine
    LI Baowei, DAO Jianhua
    2018, 52 (6):  38-44.  doi: 10.3969/j.issn.1673-5854.2018.06.006
    Abstract ( 456 )   PDF (1965KB) ( 529 )   Save
    Dehydroabietic amine(DA) was prepared with dehydroabietic acid as raw material via derivatization reaction and the structure of the product was confirmed by FT-IR, 1H NMR and 13C NMR. Dehydroabietic amine modified silicone rubber was obtained by using polysiloxane and dehydroabietic amine via condensation reaction.And by studying its effect on the properties of silicone rubber, it was found that with the increase of the dosage of dehydroabietic, the morphologies of modified silicone rubbers became more and more rough, the densities and hardness increased, and the drying time decreased. Moreover, the mechanical properties and thermal stability of silicone rubber firstly increased and then decreased, with the increase of the amount of dehydroabietic amine.When dehydroabietic amine added 5%,the tensile strength, elongation at break, the temperature of 10% weightloss and the temperature of maximum weight loss increased to 0.57 MPa, 170%, 373 ℃, 583 ℃,respectively.
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    Adsorptive Performance of Mikania micrantha Powder on Methylene Blue and Basic Fuchsin
    YANG Xinzhou, TIAN Xianjiao, MA Yanfen, YANG Qi
    2018, 52 (6):  45-50.  doi: 10.3969/j.issn.1673-5854.2018.06.007
    Abstract ( 482 )   PDF (748KB) ( 465 )   Save
    The powder of Mikania micrantha at different particle sizes was prepared as adsorbent. The adsorption properties of M. micrantha powder on methylene blue(MB) and basic fuchsine(BF) were studied at different conditions. It showed that the optimal adsorption conditions were as follow: the dosage of M. micrantha powder 20 and 10 g/L, pH value 5, particle size 0.3-0.45 mm, adsorption time 40 min and temperature 40 ℃. Under these conditions, the adsorption capacities of MB and BF were 4.870 and 9.729 mg/g. The pseudo-first-order, pseudo-second-order were used to simulate the kinetic process of it. The results showed that the pseudo-second kinetic equation was more suitable for describing the adsorption process. The thermodynamic parameters of Gibbs free energy(ΔG), enthalpy(ΔH) and en-tropy change(ΔS) were calculated and results were as follow: during the process of M. micrantha powder adsorption of methylene blue and basic fuchsine, the ΔG were between -2.13--1.58 kJ/mol and -4.66--1.63 kJ/mol; ΔS were 0.034 and 59.25 J/(mol·K),respectively; ΔH were 0.0099 and 14.75 kJ/mol,respectively. In the process of M. micrantha powder adsorption of methylene blue and basic fuchsine, the values of ΔG, ΔS, and ΔH were kept as ΔG<0, ΔH>0 and ΔS>0, which indicated that it was a spontaneous, disorderly and endothermic process.
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    Preparation of DNJ Bi-layer Osmotic Pump Tablets and Its Pharmacokinetics Study in Beagle Dogs
    SUN Zhaoying, NIE Yanyan, ZHAO Huanan, LIU Zhiming
    2018, 52 (6):  51-56.  doi: 10.3969/j.issn.1673-5854.2018.06.008
    Abstract ( 430 )   PDF (839KB) ( 463 )   Save
    The 1-deoxynojirimycin(DNJ) bi-layer osmotic pump tablets were prepared, and the prescription was optimized by dissolution. The in vitro release of DNJ bi-layer osmotic pump tablets was investigated. And the pharmacokinetics of bi-layer osmotic pump tablets and immediate release tablets were studied in Beagle dogs. The optimal prescription for DNJ bi-layer osmotic pump tablets was the dosage of containing drug layer hydroxypropylmethyl cellulose(HPMC) E50 10 mg, the boost layer polyoxyethylene(PEO, Mr6×106) 80 mg, the coating layer cellulose acetate(CA) 15 mg and polyethylene glycol(PEG) 4000 5 mg. Under these conditions, the dissolution rate of DNJ was the most suitable, and it was not affected by the change of pH value. The drug was completely dissolved in 12 h and slowly released at a constant rate. Comparing the bi-dose two-cycle crossover test of DNJ bi-layer osmotic pump tablets and immediate release tablets in Beagle dogs, the results showed that the time to peak(tmax) (9.3±3.8) h of the release of bi-layer osmotic pump tablets was longer than that of the immediate release tablets (4.4±2.2) h, achieving the purpose of controlled release. The relative bioavailability of osmotic pump tablets was (96.1±9.8)%, and the 90% confidence interval was 84.8%-103.7%. And the absorption degrees of osmotic pump tablets and immediate release tablets were organisms equivalent.
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    Optimization of 5-Hydroxymethylfurfural Preparation from Hydrolysis of Maltose Dehydration by Response Surface Methodology
    WANG Yonggui, REN Shuzhi, GENG Qingbao, ZHANG Weigang, GE Xiutao
    2018, 52 (6):  57-61.  doi: 10.3969/j.issn.1673-5854.2018.06.009
    Abstract ( 522 )   PDF (1041KB) ( 503 )   Save
    The catalytic effects of phosphate, sulfuric acid, zinc acetate and sodium hydroxide catalysts on the preparation of 5-hydroxymethylfurfural(5-HMF) were investigated with maltose as raw material and water as solvent, and the results showed that the catalytic capacity of sodium hydroxide was much higher than that of other catalysts and the dosage was less. Response surface methodology(RSM) was utilized for optimization the reactive conditions with the yield of 5-HMF as yardstick. The optimum values of these factors were found to be as follows: reaction temperature 95.20 ℃, mass of sodium hydroxide 2.25 g, reaction time 6.17 h. In this case, the yield of 5-hydroxymethylfurfural reached 61.13%.The result of infrared spectrogram analysis was consistent with the standard sample,and 5-HMF was prepared from maltose.
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    RAFT Polymerization of Dehydroabietic Acid Monomer with CPDB Chain Transfer Reagent
    GUO Tengfei, WANG Chunpeng
    2018, 52 (6):  62-66.  doi: 10.3969/j.issn.1673-5854.2018.06.010
    Abstract ( 567 )   PDF (925KB) ( 545 )   Save
    Using (β-methylacryloyloxy)propyl ester of dehydroabietic acid(DAHPMA) as monomer, azobisisobutyronitrile(AIBN) as initiator and 2-cyano-2-propyl benzodithioate(CPDB) as chain transfer reagent, dehydroabietic acid ester homopolymer was prepared by reversible addition-fragmentation transfer radical polymerization(RAFT) in tetrahydrofuran solution. The successful synthesis of the rosin homopolymer was confirmed by nuclear magnetics, and the contact angle test showed high hydrophobicity of the polymer. The kinetic study showed that the dehydroabietic acid monomer could be active and controlled under RAFT polymerization. The concentration of CPDB was found to be related to the polymerization process. Rate and controllability as well as molecular weight and molecular weight distribution had a certain impact.
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