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    30 November 2019, Volume 53 Issue 6 Previous Issue    Next Issue
    Research Report
    Preparation and Characteristics of Rubber Wood Cellulose Nanofibrils/MnO2/CNTs Flexible Electrode Materials
    Dingyuan ZHENG,Jinquan YUE,Daran YUE,Mengyang LI,Xianquan ZHANG
    2019, 53 (6):  1-8.  doi: 10.3969/j.issn.1673-5854.2019.06.001
    Abstract ( 452 )   HTML ( 1038 )   PDF (5378KB) ( 471 )   Save

    Rubber wood purified cellulose fibrils(PCF) were prepared by chemical treatment. Cellulose nanofibrils(CNF) was obtained by high-speed shearing followed by ultrasonication. Manganese dioxide(MnO2) nanosheet was prepared by one-way synthesis method. Flexible electrode materials were prepared by vacuum filtration using CNF as structural support, MnO2 and carbon nanotubes(CNTs) as active electrode materials. The structure and properties of CNF, MnO2 and electrode materials were characterized by various means, and the electrochemical properties of the prepared electrode materials were characterized. The results showed that the diameter of CNF was 3-10 nm. The obtained CNF had a large aspect ratio and could be utilized as a good structural substrate. Additionally, CNF had typical cellulose type I structure. The MnO2 nanosheets had petal-like structure with a crystal form of δ. The results of electrochemical performance showed that the specific capacitances at the scan rate of 50 mV/s and the current density of 0.1 A/g were 78.45 and 97.02 F/g, respectively. In the low frequency region, the slope of the straight part of the electrochemical impedance spectroscopy(EIS) was large, which indicated that the electrode material had good capacitance characteristics. The capacitance retention of the electrode material was always maintained at about 99% during the 200 charge and discharge cycle test. The results showed that the electrode material had good electrochemical properties and certain flexibility, and can be used as an electrode material for supercapacitors.

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    The Application Performance of Two-component Soybean Based Adhesive Treated by Sulfurous Acid
    Jiabao CHEN,Guangbin WANG,Jingya NAN,Lijun WANG,Chunpeng WANG,Fuxiang CHU
    2019, 53 (6):  9-14.  doi: 10.3969/j.issn.1673-5854.2019.06.002
    Abstract ( 291 )   HTML ( 20 )   PDF (582KB) ( 312 )   Save

    The two-component soybean meal adhesive was prepared by room temperature compounding method using soybean meal as the main raw material. The effects of the addition of sulfurous acid on the physical properties, curing viscoelasticity of the adhesive and the shear strength of the plywood were analyzed. The structures of the two-component soybean based adhesive that was prepared by the sulfurous acid treatment were characterized by FT-IR. The experimental results show that sulphate can reduce the viscosity of the adhesive system, and when the addition amount of sulfurous acid is 6%, the viscosity and the pH value of the two-component soybean meal adhesive are moderate. FT-IR shows that sulfite can promote protein hydrolysis and expose more active groups.The curing crosslinking degree and the curing viscoelasticity were better in the range of 120-150 ℃. The bonding strength of the three-layer plywood prepared by the two-component soybean based adhesive satisfies the requirement of the national standard for type Ⅰ and type Ⅱ plywood and reaches 1.02 MPa(100 ℃) and 1.24 MPa(63 ℃), respectively.

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    Comparative Study on Applicability of Bio Aviation Kerosene for Piston Aero Engine and RP-3 Fuel
    Fei YANG,Wei CHEN,Chen ZHANG,Gang LUO,Junming XU,Fanglin LI
    2019, 53 (6):  15-21.  doi: 10.3969/j.issn.1673-5854.2019.06.003
    Abstract ( 446 )   HTML ( 332 )   PDF (2265KB) ( 331 )   Save

    Bio aviation kerosene was prepared from soybean oil by catalytic cracking, distillation, aromatization and hydrogenation, and its composition and physicochemical properties were analyzed. A piston aero-engine was used to start the bench test, and the applicabilities of bio aviation kerosene and RP-3 fuel were compared and analyzed. The results showed that the basic components of bio aviation kerosene were straight-chain alkanes 74.54%, naphthenes 13.04%, aromatic hydrocarbons 10.31%, ethers 1.07% and non-alpha-chain olefins 1.04%. The calorific value of bio aviation kerosene was high(44.4 MJ/kg), freezing point was low(-48 ℃), but its viscosity was high(2.11 mm2/s). Compared with RP-3 fuel, bio aviation kerosene had lower start-up temperature; temperature rise rate(within 4 ℃ difference), fuel consumption(less than 0.02 g/s difference) were close to those of RP-3 fuel, the excess air coefficient fluctuated greatly(0.8-1.2) when engine speed exceeded 4 200 r/min, and those of combustion state deteriorated; engine disassembly inspection after bench test showed that coking occured after burning bio aviation kerosene. The phenomenon of carbon deposition was due to the high viscosity(>2 mm2/s) of bio aviation kerosene in this batch, which had an impact on the working performance of engines such as atomization efficiency and combustion adequacy.

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    Preparation and Application of Emulsifier Based on Undecylenic Acid
    Yonghe ZHANG,Gaowei FU,Liwei JIN
    2019, 53 (6):  22-26.  doi: 10.3969/j.issn.1673-5854.2019.06.004
    Abstract ( 287 )   HTML ( 87 )   PDF (503KB) ( 259 )   Save

    Undecylenic acid/maleic anhydride-dodecanol (UMA-DA) polymer was prepared by esterification reaction using dodecanol(DA) and undecylenic acid(UA)/maleic anhydride(MAH) as copolymer.The polymer is used as an emulsifier in the emulsion polymerization of UA and methyl methacrylate(MMA). FT-IR analysis showed that the self-made undecylenic acid/maleic anhydride(UMA) copolymer acted with DA by esterification of an acid anhydride with a hydroxyl group.The proton signal at δ 3.2-3.4 of —O—CH2—in 1H NMR show that UMA-DA copolymer was prepared successfully.The critical micelle concentration(CMC) value of UMA saponification was determined by surface tension method. The CMC value of UMA-DA was 9.6 g/L, and the surface tension γCMC was 23.04 mN/m. The γCMC value of UMA-DA is much lower than that of pure water(71.97 mN/m). The particle size and particle size distribution index(PDI) increased, butthe gel rate gradually decreasedwith the increase of UMA-DA dosage in emulsion polymerization. The emulsion is relatively stable, and the total monomer conversion rate reaches 98.1% when the amount of the self-made emulsifier UMA-DA is 10% of the total monomer and the ratio of UA to MMA is 10 : 90.

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    Structural Characterization and Pyrolysis Characteristics of Apricot Shell Lignin
    Huanhuan MA,Yiling WAN,Lingxiang XIE,Fanrui MENG,Jianbin ZHOU
    2019, 53 (6):  27-32.  doi: 10.3969/j.issn.1673-5854.2019.06.005
    Abstract ( 346 )   HTML ( 271 )   PDF (1303KB) ( 400 )   Save

    The lignin of apricot shell was separated from apricot shell by sulfuric acid removal method to study the structure, pyrolysis characteristics and product formation of apricot shell lignin, and its structure and composition were confirmed by Fourier transform infrared spectroscopy(FT-IR) and nuclear magnetic resonance(NMR). The formation characteristics of pyrolysis products was studied by thermogravimetric and thermogravimetric-infrared spectroscopy. The results showed that the yield of apricot shell lignin was 30.42% by sulfate removal method. The FT-IR showed that the apricot shell lignin could be qualitatively determined guaiacyl unit and syringyl unit. The 2D heteronuclear single quantum correlation nuclear magnetic resonance (2D HSQC NMR) of apricot shell lignin indicated which contained syringyl(S), guaiacyl(G) and p-hydroxyphenyl proane(H). Apricot shell lignin pyrolysised in a wide temperature range between 150 and 650 ℃, and the pyrolysis process was mainly divided into three stages analyzied by thermogravimetric and thermogravimetric-infrared spectroscopy. The maximum thermal decomposition weightlessness temperature was 360 ℃, and H2O, CO, CO2, CH4, alcohols, aldehydes, phenols and acids were generated. The precipitation temperature range of CO occured in a wide temperature range between 200-700 ℃, that mainly created by the dissociation of the ether bond on the side chain of phenylpropane at the low temperature, and created by the dissociation of the ether bond between benzene rings and the volatile decomposed secondary. The precipitation temperature range of CO2 was narrow between 250-650 ℃, which mainly created by the fracture and rearrangement of the carbonyl and carboxyl on the side chain of phenylpropane. The precipitation of CH4 had two peaks, the one 400 ℃ was the dissociation of the side chain of phenylpropane and the demethylation of the methoxy on the benzene, and the other one 600 ℃ was rupturing deeply of the aromatic ring.

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    Monosaccharide and Alduronic Acid Composition of Bamboo Leaves by Ion Chromatography
    Qiang ZHANG,Hongfu JI,Yan ZHOU,Yu FAN,Qing GE,Zhuqian XIAO,Jianwei MAO
    2019, 53 (6):  33-38.  doi: 10.3969/j.issn.1673-5854.2019.06.006
    Abstract ( 301 )   HTML ( 11 )   PDF (467KB) ( 330 )   Save

    A simple, rapid and accurate method for the determination of monosaccharide compositions from lignocellulose byionchromatographywas established. The HPAEC-PAD method was established to simultaneously detect 7 different monosaccharides and two types of alduronic acid. Dionex ICS-5000+ with CarboPACTMPA10(4 mm×250 mm) column and pulsed amperometric detection was involved in this method. This method could be simultaneously qualitatively and quantitatively analysed by the gradient elution of NaOH and CH3COONa.The results showed that the method has good linearity (R2≥0.999 0), high precision (RSD < 3%), adequate (98.53%-118.63% recovery) and good reproducibility (RSD < 1.16%)within the range. The limitions of quantitation and detection were 0.05-3.0 mg/L and 0.01-1 mg/L, respectively. The method was applied to determine the monosaccharide compositions from bamboo leaves hydrolysate.The results showed that bamboo leaves hydrolysate was composed of arabinose, galactose, glucose and xylose.The mole ratio of monosaccharide to n(arabinose) : n(galactose) : n(glucose) : n(xylose)=2.9 : 0.7 : 8.2 : 9.7.This method is successful and can be used for the determination of monosaccharides in lignocellulose.

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    Study on Extraction and Purification of Tea Saponin from Tea Seed Meal
    Wanli SUN
    2019, 53 (6):  39-44.  doi: 10.3969/j.issn.1673-5854.2019.06.007
    Abstract ( 413 )   HTML ( 19 )   PDF (550KB) ( 328 )   Save

    Tea saponin was extracted by alcohol extraction using tea seed meal as raw material. The optimum extraction conditions of tea saponin was as follows:the ratio of solid to liquid was 1 : 9(g/mL), the volume fraction of extraction solution(ethanol) was 60%, the extraction temperature was 60 ℃ and the extraction time was 3 h, under the above reaction conditions, the highest yield of tea saponin was 14.9%. Crude tea saponin was purified by NKA-9 macroporous resin. In the purification experiment, the static adsorption reached saturation for 0.5 h and the desorption rate of the volume fraction 80% ethanol reached the maximum of 91.1% in the static desorption, while the dynamic adsorption and desorption. The adsorption rate reached 66.04% at the rate of 8 mL/min, and the concentration of tea saponin was between 1.25 g/L and 1.57 g/L after elution with the volume fraction 80% ethanol of 50 mL at the flow rate of 5.0 mL/min, tea saponin purity 95%.

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    Isolation and Physical-chemical Data Testing of Levopimaric Acid
    Zhiwen QI,Chengzhang WANG,Jianxin JIANG
    2019, 53 (6):  45-50.  doi: 10.3969/j.issn.1673-5854.2019.06.008
    Abstract ( 410 )   HTML ( 902 )   PDF (558KB) ( 452 )   Save

    Levopimaric acid was isolated from turpentine by amination method and ultrasonic assisted recrystallization, and its physical and chemical data were experimental measured. By single factor and orthogonal test, the optimum isolation conditions of levopimaric acid were as follows:ethanol concentration 100%, crystallization temperature 0 ℃, volume ratio of ethanol used for crystallization 20 : 1(mL : g), ultrasonic frequency was 53 kHz, 2 recrystallization times; purity of levopimaric acid was 97%. Ultrasonic assisted crystallization was used to shorten the nucleation time of the levopimaric acid crystal, and a fine-uniform rectangular transparent crystal was obtained after 5-6 h. The molecular structure of levopimaric acid was characterized by FT-IR, NMR(1H NMR, 13C NMR) and GC-MS. According to the oxygen elastic calorimeter, TG-DSC and group contribution, the standard molar enthalpy(ΔfHm?) and melting enthalpy of levopimaric acid were -700.23 and 94.99 kJ/mol, respectively.

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    Review Comment
    Progress in the Synthesis of Biomass-based Glycerol Acetals and Ketals
    Ze XIAO,Chun CHANG,Jing BAI,Junying CHEN,Pan LI,Xiuli HAN
    2019, 53 (6):  51-58.  doi: 10.3969/j.issn.1673-5854.2019.06.009
    Abstract ( 479 )   HTML ( 51 )   PDF (569KB) ( 396 )   Save

    As an important biomass-based platform compound, glycerol can be condensed with carbonyl compounds under the action of acidic catalysts to form acetals and ketals. Acetals and ketals are widely used in the fields of fuel additives, perfumes, veterinary medicine preparations, plasticizers and polyols. The catalytic performance of traditional liquid acid catalyst and solid catalyst was compared based on the synthesis mechanism of glyceryl acetal and ketal; then, the synthesis processes of several important glycerol acetals and ketals such as solketal, cyclohexanone glycerol ketal, benzaldehyde glycerol acetal, glycerol formal and glycerol levulinate ketal were introduced, and their production technology was summarized; finally, the development and application prospects of bio-based glycerol acetal and ketal are prospected.

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    Research Progress of Rosin-based Polyurethane
    Jintao SHAO,Caili YU,Fa'ai ZHANG
    2019, 53 (6):  59-66.  doi: 10.3969/j.issn.1673-5854.2019.06.010
    Abstract ( 357 )   HTML ( 27 )   PDF (700KB) ( 393 )   Save

    The modification methods of rosin in solvent-based polyurethanes, waterborne polyurethanes, non-solvent polyurethanes, and non-isocyanate-based polyurethanes in recent years were reviewed. It is concluded that rosin and derivatives can effectively reduce the amount of the petrochemical and improve the water resistance, thermodynamic performance and mechanical properties. Meanwhile, there are still some problems, such as simple modification method, low molecular weight of rosin-based polyol, single application direction. The development trend and research direction of the rosin-modified polyurethanes are proposed.

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