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    25 April 2018, Volume 38 Issue 2 Previous Issue    Next Issue
    Characterization Methods of Wood Ultrastructure and Its Research Progress
    WANG Xuan, LIU Zhu, ZHANG Yaoli, PAN Biao
    2018, 38 (2):  1-10.  doi: 10.3969/j.issn.0253-2417.2018.02.001
    Abstract ( 543 )   PDF (4565KB) ( 471 )   Save
    The characterization methods of wood cell wall ultrastructure were generally reviewed in the context.In particular,four approaches including the X-ray diffraction, nuclear magnetic resonance, atomic force microscopy and confocal Raman microscopy, were detailed in their application and research status, which could provide the methods and ideas for future exploration of the microphase structure of wood. Additionally,the advantages and limitations of each technology were also summarized.Moreover,the existing drawbacks and future direction of cell wall structure research were clearly pointed out.
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    Research Advances on Glycoside Hydrolases with Two Catalytic Domains
    XIA Jilin, TAN Zhongbiao, ZHU Xiaoyan, SHI Hao, LI Xiangqian
    2018, 38 (2):  11-20.  doi: 10.3969/j.issn.0253-2417.2018.02.002
    Abstract ( 348 )   PDF (750KB) ( 416 )   Save
    This review presented the reaserch progresses in the natural domains analysis, artificial construction, modification, and application of glycoside hydrolases with two catalytic domains. The study of glycoside hydrolases with two catalytic domains on improving thermostability and catalytic activity were highlighted. In addition, the catalytic mechanism of glycoside hydrolases with two catalytic domains was explored, and also the research directions of glycoside hydrolases with two catalytic domains were prospected.
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    Process Conditions and Performance of Polyacrylate-based Super Absorbent Resin Prepared with Lignin-related Compounds
    QIAN Shuang, REN Hao
    2018, 38 (2):  21-28.  doi: 10.3969/j.issn.0253-2417.2018.02.003
    Abstract ( 394 )   PDF (4193KB) ( 270 )   Save
    Lignin including alkali lignin (AL), lignosulfonate (LS), lignocresol (LC), lignoresorcinol (LR) and lignopyrogallol (LP) were grafted by acrylic acid (AA) to synthesized water-absorbent resin under aqueous solution with potassium persulfate (KPS) as initiator and N,N'-methylene-bis-acrylamide (MBA) as crosslinking agent. The morphological characteristic water-absorbing capacity and salt tolerance of different resins were compared. The effects of different lignins on the pore structure and specific surface area were studied. The swelling behaviors of the resins were fitted by the swelling kinetics model. The results indicated that the water absorption capacities of resins were according to the order of lignopyrogallol grafted polyacrylic acid resin(LP-g-PAA, 2 137 g/g) >lignosulfonate grafted polyacrylic acid resin (LS-g-PAA, 1 348 g/g) > lignoresorcinol grafted polyacrylic acid resin (LR-g-PAA, 1 344 g/g)>lignocresol grafted polyacrylic acid resin (LC-g-PAA, 1 262 g/g) > Alkaline lignin grafted polyacrylic acid resin (AL-g-PAA, 518 g/g)>polyacrylic acid resin (PAA, 439 g/g). The FE-SEM and BET specific surface area analyses showed that the addition of different lignins could change the pore structure and specific surface area to different degree, shich would affect the absorption. And the swelling behaviors of the resins were proved to according with Schott swelling kinetics model(R2>0.98). Salt tolerance of LP-PAA resin were affected by the valence of ion,radius of hydrated ion and concentration of ion and the results were as follows:KCl>KNO3≈LiCl > K2SO4 > K2CO3 > CaCl2 > FeCl3.
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    Preparation of Woody Activated Carbon for Supercapacitor Electrode by Steam Activation
    DU Yanzhen, SHEN Baoshou, ZUO Songlin, XIA Hai'an
    2018, 38 (2):  29-38.  doi: 10.3969/j.issn.0253-2417.2018.02.004
    Abstract ( 426 )   PDF (1201KB) ( 427 )   Save
    In order to prepare activated carbons for supercapacitor electrode with low price and good performance, traditional steam activation method was employed to prepare activated carbons from masson pine wood. The elemental analyzer and the nitrogen adsorption/desorption were employed to analyze the element contents and pore structure of the activated carbons. The electrochemical performance of the activated carbon electrodes was examined by the methods including cyclic voltammetry, galvanostatic charge-discharge cycles and electrochemical impedance spectroscopy using 1-ethyl-3-methyl imidazole tetrafluoroborate/acetonitrile (EMIMBF4/AN) as electrolytes. The effects of activation temperature and time on the electrochemical performance of activated carbon were investigated. The results showed that the specific copacitance of activated carbon increased first and then decreased with the increment of activation temperature and activation time. The activated carbon prepared at carbonization temperature 900℃ and activation temperature 900℃ for 1 h reached the maximum of the specific capacitance. Its specific capacitance reached 155 F/g with a sweep speed of 5 mV/s and remaind 105 F/g at 100 mV/s, and the energy density in organic electrolyte was as high as 33.6 (W·h)/kg. After 5 000 cycles, specific capacitance was remain at value of 89%.
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    Influence of Metallic Elements Exuded from Wood Based Fly Ash on Treatment of TMP Effluent
    SUN Yonghui, LIU Zhong, FATEHI Pedram
    2018, 38 (2):  39-45.  doi: 10.3969/j.issn.0253-2417.2018.02.005
    Abstract ( 325 )   PDF (1358KB) ( 199 )   Save
    In the process of thermomechanical pulping(TMP) effluent treatment using wood based fly ash (FA) as reactant, inorganic metallic ions can exude into the effluent from FA complex. In order to determine the metallic elements in FA would flocculate and remove the organics in the effluent under the alkaline condition, the removal behaviors of organic material were investigated by means of simulation with different kind of metallic ions addition at various dosage levels and adjusting pH value of TMP effluent, respectively. It concluded that the metallic ions combined with organics precipitate simultaneously under the alkaline condition by charge neutralization and H-bond to form large particles. The removal rates increased with the increment dosage of Mg2+ and Fe3+, while the Ca2+ and Al3+ would not be affected by their dosage under the alkaline condition. When the pH values were 10 and 12, respectively, the removal capability of Ca2+ and Mg2+ was maximum at pH value 12, while Al3+ achieved peak removal rate at pH 10. The removal efficiency from Fe3+ kept constant between pH value 10 and 12.
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    Preparation of Rosin-based N-Heterocyclic Carbene Catalyst and Its Catalytic Properties for Addition Reaction of Aryl
    LI Jian, ZHANG Junhua, SONG Zhanqian, SHANG Shibin
    2018, 38 (2):  46-50.  doi: 10.3969/j.issn.0253-2417.2018.02.006
    Abstract ( 391 )   PDF (489KB) ( 212 )   Save
    Two kinds of rosin-based N-heterocyclic carbene (NHC) from dehydroabietylamine and acrypimaric amine were designed and synthesized, and their structures were identified by FT-IR, 1H NMR, 13C NMR, MS and elemental analysis. For screening the catalysts and evaluating their activity, the novel rosin-based NHC molecules were used to catalyze the addition reaction of aromatic aldehydes and aryl boronic acids. The results showed that catalytic activity of the acrypimaric-based NHC(Ap-NHC) was better than that of dehydroabietic-based NHC(Da-NHC), and the optimal catalytic effect was presented at reaction conditions of reaction temperature 60℃, the reaction time 4 h, the amount of catalyst 2.5% and potassium tert-butoxide as alkali, and the yield reached to 95%. Finally, the influence of different substituent groups on the reactant was studied. When the aryl boronic acid reacted with the aromatic aldehyde with electron withdrawing group, the yield was the highest, while the substituent on the boric acid had little effect on the reaction.
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    Effects of Inorganic Elements Spray on the Content of Polyphenols in Eucommia ulmoides Olive Leaves
    PENG Mijun, PENG Sheng, WANG Xiang, ZHANG Linjie
    2018, 38 (2):  51-58.  doi: 10.3969/j.issn.0253-2417.2018.02.007
    Abstract ( 382 )   PDF (2095KB) ( 259 )   Save
    The effect of three kinds of microelement fertilizers spray, such as iron, zinc and manganese, on the biomass of Eucommia ulmoides Olive leaves and the contents of total polyphenols, flavonoids and chlorogenic acid(CA) in leaves were studied. Quadratic saturation D-optimization design was used to carry out the foliage spray. The equation of fertilizer effect of Fe, Zn, and Mn were established by stepwise regression method, and optimized by frequency analysis method. The result showed that the effects of Fe, Zn, and Mn on E. ulmoides leaves were not linear accumulation of individual effects. There were interactions between the factors. During the fertilization process, interaction effects should be considered synthetically to find the balance point of fertilizer application. The suitable fertilizer application for leaves of E. ulmoides were FeSO4·5H2O 0.20%-0.22%, ZnSO4·7H2O 0.17%-0.21% and MnSO4·5H2O 0.18%-0.21%. Under the condition of Fe 0.21%, Zn 0.19% and Mn 0.20%, the biomass of leaves was 220 g each, content of total polyphenol was 6.212%, content of flavones was 3.611% and content of chlorogenic acid was 1.918%, which was significantly better than the control group.
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    Self-assembly,Mixed System and Drug-loading Research of Rosin-based Tertiary Amine Salt
    LIN Haixia, YANG Mingsheng, TIAN Chao, HAN Chunrui
    2018, 38 (2):  59-66.  doi: 10.3969/j.issn.0253-2417.2018.02.008
    Abstract ( 392 )   PDF (1945KB) ( 228 )   Save
    A novel maleic rosin-based ester tertiary amine salt surfactant (RETAS) with three hydrophilic groups was synthesized through D-A addition reaction, acyl chlorination, esterification reaction and salt forming reaction with rosin acid as raw material. The critical micelle concentration (CCMC) of RETAS was 0.73 mmol/L (0.50 g/L), and the corresponding surface tension at CMC (γCMC) was 38.58 mN/m. The RETAS was mixed with natural soapnut saponin. The best compound proportion of mixed system was obtained by determining the surface tension, emulsification property and foam property to study the synergistic effect. And the self-assembly behavior and micelle morphology of the composite system was characterized by transmission electron microscopy (TEM) and the micelle formation mechanism was speculated in detail. The results showed that the γCMC and CCMC of mixtures were 37.57 mN/m and 0.40 g/L when the optimum mass ratio of RETAS/soapnut saponin was 5:5. The emulsifying properties of RETAS and saponin were only 292 s and 310 s respectively, but the emulsifying properties increased to 373 s in the optimum mass ratio. Finally, the cytotoxicity of RETAS on human colon adenocarcinoma cells (Caco-2) was investigated and it was found that it had non-toxic or low toxicity and was applied to study the drug loading properties of anticancer drug doxorubicin (DOX). The release rates of DOX on RETAS were 67% and close to 100% in pH value 7.4 and 5.0, respectively. While the release rates of DOX on the mixture were 68% and close to 90% in pH value 7.4 and 5.0. The results showed that both RETAS and mixed product could be used as the target carrier of DOX. Under simulated tumor conditions, DOX was still slowly released after 24 hours in pH=5.0.
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    Preparation of Oxidized Cellulose Being Used as Dispersant for Carbon Nanotubes
    LIU Zhenzhen, GUO Yanzhu, WANG Xing, LI Haiming
    2018, 38 (2):  67-74.  doi: 10.3969/j.issn.0253-2417.2018.02.009
    Abstract ( 427 )   PDF (1510KB) ( 240 )   Save
    The oxidized cellulose(OC) was prepared through selective oxidation of softwood dissolving pulp cellulose by HNO3/H3PO4/NaNO2 oxidant. The effects of oxidizing conditions, e.g., oxidizing time, temperature and dosages of NaNO2 on the yields and carboxyl groups contents of OC were studied. The structures and properties of OC samples were characterized by Fourier transform infrared spectroscopy(FT-IR), X-ray diffraction(XRD) and thermogravimetric analysis(TGA) respectively. The nanoparticle solution was prepared by dispersing the OC sample in aqueous solution under ultrasound wave. The sizes and morphologies of particles were characterized by dynamic light scattering(DLS) and transmission electron microscopy(TEM). The results showed that the nanoparticles were spherical in shape with monodisperse, and the sizes of micelles were in the range of 30 nm to 80 nm. The optimum conditions of OC preoaration were as the followings:reaction temperature 50℃, NaNO2 dosage 1.4% and reaction for 12 h. Compared with water and cellulose, the OC nanoparticle was an excellent aqueous dispersant for multi-walled carbon nanotube(CNT).
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    Effect of Pretreatment Methods on Cellulase Adsorption Profiles of Sugarcane Bagasse
    DONG Yifan, LIU Zhijia, LAN Tianqing
    2018, 38 (2):  75-79.  doi: 10.3969/j.issn.0253-2417.2018.02.010
    Abstract ( 390 )   PDF (947KB) ( 286 )   Save
    The effects of two pretreatment methods, sulfite (SPORL) pretreatment and dilute sulfuric acid (DA) pretreatment, on the enzymatic hydrolysis of sugarcane bagasse (SCB) substrates were investigated and the adsorption of cellulose on SCB during the hydrolysis was studied. The enzymatic hydrolysis efficiency, composition, surface morphology, adsorption isotherms and kinetics of two kinds of pretreated SCB were compared. The results showed that the enzymatic hydrolysis efficiency of SPORL-SCB(81.92%) was significantly higher than that of DA treated SCB(60.89%). Compared with the untreated SCB, the surface of SCB treated by SPORL and DA became rough, the surface fibres were partially stripped and the internal fibre skeleton was exposed. The holocellulose contents of these two treated SCB substrates were not significantly different, but the Klason lignin content of SPORL treated SCB was lower. The XPS images suggested that the treated SCB substrates both adsorbed cellulase. The adsorption isotherm and kinetics curves showed that the maximum adsorption of cellulase on SPORL treated SCB was 61.91 mg/g and lower than that on DA treated SCB(82.69 mg/g), but the adsorption affinity and adsorption strength of SPORL treated SCB were higher than those of the DA treated SCB.
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    Isolation and Identification of Antifungal Ingredients from Artemisia hedinii
    XU Jie, CHENG Chuanke, HU Guoyuan, YANG Chunlei, YU Jun, YANG Jinpeng
    2018, 38 (2):  80-86.  doi: 10.3969/j.issn.0253-2417.2018.02.011
    Abstract ( 284 )   PDF (664KB) ( 221 )   Save
    The extraction of Artemisia hedinii Ostenf. et Pauls(A. hedinii) were rough and further isolated by chromatographic separation technology, and the antifungal activity of the component was evaluated by the the spore germination method. Furthermore, the composition of antimicrobial components was analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS). The results showed that 13 kinds of components(Fr.1-Fr.13) were rough isolated from the extraction of A. hedinii, in which the component Fr.5 showed the best antifungal activity. Four kinds of components (Fr.5.1-Fr.5.4) were obtained by the further separation of the component Fr.5. The EC50 of A. hedinii crude extraction on Alternaria alternate (A.alternate) spores was 5.04 g/L, and that of the component Fr.5.2 was 0.57 g/L. The HPLC-MS results showed that the components of Fr.5.2 mainly contained deoxy double hydroxyl artemether (17%),deoxy dihydroartemisinin (43.65%) and deoxyartemisinin (16.15%). The content of dihydroartemisinin of component Fr.5.2 was calculated as 40.95% by using dihydroartemisinin as the standard. The EC50 of dihydroartemisinin on A.alternate was 2.70 g/L, indicating that the major antifungal matter in component Fr.5.2 was artemisinin derivatives.
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    Synthesis of Rosin Based Crosslinking Agent and Its Effect on Properties of Cured Silicone Rubber
    LI Qiaoguang, LIU He, LI Jianfang, SHANG Shibin, SONG Zhanqian
    2018, 38 (2):  87-93.  doi: 10.3969/j.issn.0253-2417.2018.02.012
    Abstract ( 393 )   PDF (1213KB) ( 312 )   Save
    Rosin modified aminopropyltriethoxysilane(RA) was obtained via rosin derivatization reaction. RA was used as crosslinking agent to prepare rosin based room temperature vulcanized silicone rubber and to study its effect on the morphology, mechanical and thermal properties of rubber. It was found that rosin based silicone rubber had better mechanical and thermal properties than those of the traditional silicone rubber. The tensile strength and elongation at break of rosin based silicone rubber were 0.51 MPa and 353% respectively, under the conditions of 11.1 g RA and 30 g hydroxyl terminated polydimethylsiloxane as primary polymers. Compared with the traditional silicone rubber, tensile strength and elongation at break of rosin increased by 11% and 84%, meanwhile the maximum weight loss rate temperature was 592℃, rising by 201℃. Correspondingly, the residual rate at 800℃ increased by 4.17% and the glass transition temperature of the silicone rubber also increased slightly.
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    Physicochemical Property, Evaluation and Screening of Seed Oil from 88 Species of Non-food Biodiesel Plants in Xiangxi Region
    WANG Bingqing, ZHANG Jie, XU Liang, CHEN Gongxi
    2018, 38 (2):  94-104.  doi: 10.3969/j.issn.0253-2417.2018.02.013
    Abstract ( 334 )   PDF (813KB) ( 421 )   Save
    The physical and chemical properties of seed oil from 88 non-food biodiesel plants species with the oil content >30% in Xiangxi region were analyzed, evaluated and screened by measurement of acid value, iodine value, saponification value and the components of fatty acids. The results showed that within the 88 species, the acid value, iodine value, saponification value and linolenic acid in the oil ranged from 0.63-202.35 mg/g, 1.85%-288.26%, 70.72-576.16 mg/g and 0.02%-63.93%, respectively. According to the evaluation standard in Xiangxi region, 14 species of 88 non-food biodiesel plants species were preliminarily screened. Based on the analytic hierarchy process (AHP) from 8 evaluation indexes, belonging to three classes, i.e., the specie natural property, seed oil physicochemical property and the oil composition content, these 11 non-grain biodiesel plants were evaluated and ranked as Lindera reflexa > Glochidion puberum > Carya hunanensis > Arctium lappa > Chimonanthus praecox > Sloanea sinensis > Corylus chinensis > Decaisnea insignis > Symplocos paniculata > Camellia cuspidata > Koelreuteria bipinnata. Combing the biological traits of these species, it was proposed that L. reflexa,C. hunanensis,A. lappa,C. praecox and S. paniculata were suitable for the biodiesel development in Xiangxi region, among which four species (L. reflexa and C. hunanensis) showed the largest potentiality.
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    Synthesis and Antibacterial Activity of Derivatives of Rhein
    WANG Xingda, LI Lei, HAN Yongping
    2018, 38 (2):  105-111.  doi: 10.3969/j.issn.0253-2417.2018.02.014
    Abstract ( 459 )   PDF (3972KB) ( 323 )   Save
    Based on carboxyl amidation of rhein(1), a series of derivatives of rhein were synthesized by structure modification of C7 of anthraquinone mother nucleus. And the antibacterial activity and structure-activity relationship of the derivatives were preliminary discussed. The derivatives of rhein were respectively rhein piperidine amide(2), 7-hydroxymethyl-rhein piperidine amide(3), 7-bromomethyl-rhein piperidine amide(4), 7-(4-morpholino)methyl-rhein piperidine amide(5a), 7-(pyrrolidin-1-yl)methyl-rhein piperidine amide(5b), 7-(1-methyl-4-piperazinyl)methyl-rhein piperidine amide(5c). The structures of the compounds were characterized by IR, 1H NMR, 13C NMR, MS. The minimal inhibitory concentrations (MIC) of the compounds obtained were tested and the MIC of compounds 5a and 5b against E.coli reached 0.78 and 0.39 mg/L respectively. Their antibacterial activity were stronger than that of rhein(MIC 3.13 mg/L) obviously, even stronger than that of the kanamycin(MIC 1.56 mg/L); and the MIC of compound 5a against S. aureus reached 1.56 mg/L, which was similar to that of rhein. The preliminary analysis of structure effective relationship showed that if none replace heterocyclic groups were introduced into substituent of C7 of the mother nucleus, the antibaterial activity on E.coli would be stronger.
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    Preparation of Aromatic Compounds by Catalytic Pyrolysis of Lignin over Mesoporous Molecular Sieves
    LI Weixue, LIU Shiwei, YU Shitao, SONG Zhanqian
    2018, 38 (2):  112-118.  doi: 10.3969/j.issn.0253-2417.2018.02.015
    Abstract ( 370 )   PDF (1640KB) ( 273 )   Save
    The mesoporous molecular sieve PNS-7 was synthesized by using ionic liquid[P123mim] Cl as template, and characterized by XRD, TEM, SEM and N2 adsorption/desorption techniques. Compared with the traditional mesoporous molecular sieve MAS-7, the synthesized molecular sieves PNS-7 had the typical hexagonal mesoporous structure, and the advantages of long-range orderliness, good crystallinity, narrow pore size distribution and high specific surface area. The effects of catalyst type and dosage, reaction temperature, and reaction time on the reaction of lignin were investigated by single factor and orthogonal experiments using PNS-7 and MAS-7 molecular sieves as catalysts. It was found that the molecular sieves PNS-7 had an outstanding catalytic performance for the lignin pyrolysis, and the lignin cracking residue rate was 27.6%, the selectivities of vanilla acid and vanillin were 28.2% and 29.6% under the reaction conditions of ethylene glycol as solvent, lignin 1.0 g, PNS-7 0.1 g, reacted temperature 180℃ and reaction time 3 h. In addition, the molecular sieves PNS-7 had good reusability for the lignin pyrolysis. After 4 repetitions, catalytic performance of PNS-7 was not obviously changed.
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    Thermal Decomposition Characteristics and Kinetics of Tea Stalk
    GUO Xianhua, ZHANG Jianyu, ZHAN Fangdong, HE Yongmei, LI Bo, JIANG Ming
    2018, 38 (2):  119-125.  doi: 10.3969/j.issn.0253-2417.2018.02.016
    Abstract ( 401 )   PDF (873KB) ( 484 )   Save
    In order to provide comprehensive utilization of tea stalk waste by thermochemical conversion, the thermal decomposition process of tea stalk and its kinetics were studied with simultaneous measurements of thermogravimetry (TG)/differential thermal analysis (DTA). The TG-DTG-DTA curves of tea stalk were acquired in a nitrogen atmosphere. The results indicated that the mass loss process of the samples could be divided into five stages. Among the five stages, most of the decomposition occurred in the third and fourth stages. The two main stages were indicated as exothermic processes, with the average weight loss rates of 55.12% and 28.48% at different heating rates of 10, 15, 20, 25 K/min, respectively. At higher heating rate, the fourth stage of the decomposition reaction was shifted to higher temperature range. The thermal decomposition kinetic parameters were calculated by Kissinger, FWO peak maximum evolution and FWO isoconversional methods. The results showed that the Kissinger and FWO peak maximum evolution methods were more suitable for the thermal decomposition kinetic parameters. The apparent activation energies were calculated to be 666.53 and 642.80 kJ/mol by the two methods, respectively. And natural logarithm of the pre-exponential factor (lnA) calculated by Kissinger method was given as 145.83.
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    Synthesis Mechanism of Tris(2-hydroxyethyl)isocyanate Modified Melamine Formaldehyde Impregnated Resin
    WANG Rongxing, ZHANG Zuxin, CHEN Riqing, WANG Chunpeng
    2018, 38 (2):  126-132.  doi: 10.3969/j.issn.0253-2417.2018.02.017
    Abstract ( 541 )   PDF (889KB) ( 295 )   Save
    The tris(2-hydroxyethyl)isocyanate(THEIC) modified melamine formaldehyde(MFT) impregnated resin was prepared with THEIC, melamine(M) and formaldehyde(F) as raw materials. The MFT resin could achieve the requirements of GB/T 14732-2006. The stability of MFT resin was significantly improved with THEIC, as the n(THEIC)/n(F) was 10% or 15%. MFT resin(n(F)/n(M)=1.85 and n(THEIC)/n(F)=15%) remained highly transparent up to 24 days, and its free formaldehyde was only 0.05%. Infrared characterization of MFT resin analysis showed that the absorption peaks of carbonyl functional groups of MFT resin changed to 1680.9 cm-1 from 1670.7 cm-1 in THEIC. The CN absorption peak in melamine ring was 1525.7 cm-1, and split up into two peaks(1545.3 and 1504.0 cm-1) in MFT resin. 13C NMR qualitative and quantitative analysis the reaction process of the MFT resin showed that the hydroxymethyl of amino in melamine was the main reaction and accompanied with the etherification reaction (between hydroxymethyl, hydroxymethyl and THEIC). The main reaction products were oligomers. The joining of the THEIC made the reverse reaction of the condensation of amino and hydroxyl groups, which was hydrolysis reaction,and proved that the resin storage period increased.
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    Synthesis and Catalytic Performance of Isolongifolenone Sulfonic Acid
    LIU Yanfang, RUI Jian, XU Xu, GU Wen, WANG Shifa
    2018, 38 (2):  133-138.  doi: 10.3969/j.issn.0253-2417.2018.02.018
    Abstract ( 344 )   PDF (484KB) ( 259 )   Save
    Isolongifolenone sulfonic acid (IFSA) was synthesized by sulfonation of isolongifolenone using concentrated sulfuric acid as the sulfonation reagent and isolongifolenone as the starting material, and the catalysis effect of IFSA was investigated by catalyzing the esterification reaction of dipropylene glycol methyl ether (DPM) and acetic acid (HAc). Effects of the charging sequence, dosage of sulfuric acid, reaction temperature, and the amount of acetic anhydride on the sulfonation reaction were examined, and the suitable sulfonation conditions were determined as follows:the reactants mole ratio of isolongifolenone and H2SO4 1:1.4; acetic anhydride was used as the solvent, and the mass ratio of isolongifolenone/acetic anhydride was 1:2.0; sulfonation temperature 40℃,reaction time 40 min. The yield of IFSA reached 82.36% in the aforesaid conditions. The catalysis effect of IFSA was compared with other catalysts by catalyzing esterification reaction of dipropylene glycol methyl ether (DPM) and acetic acid (HAc), and test results showed that IFSA was the best than others. Effects of DMP/HOAC molar ratio, dose of IFSA, esterification temperature and time on the esterification reaction were examined, and the suitable esterification conditions were as follows:the molar ratio of DPM and HAc 1:1.5, the mass ratio of isolongifolenone sulfonic acid and DPM 0.045:1, cyclohexane as the water-carrying reagent, esterification temperature 90℃, esterification time 6 h. The yield of dipropylene glycol methyl ether acetate (DPMA) reached 96.69% at the aforesaid esterification conditions. In addition, the yield of DPMA was still maintained at more than 90.07% when IFSA was reused for 3 times. Qualitative analysis, quantitative analysis, and structure characterization of the products were carried out by GC, GC-MS, HPLC, FT-IR, 1H NMR, 13C NMR, X-ray single crystal diffraction methods.
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