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    30 April 2010, Volume 30 Issue 2 Previous Issue    Next Issue
    研究报告
    Study on Pyrolysis Characteristics and Kinetics of Walnut Shell
    ZHENG Zhi-feng;HUANG Yuan-bo;JIANG Jian-chun;YANG Xiao-qin;ZHOU Ling
    2010, 30 (2):  6-10. 
    Abstract ( 588 )   PDF (858KB) ( 888 )   Save
    The pyrolysis characteristics of walnut shell at different heating rates (5-50K/min) under the stream of N2 were studied using thermogravimetric analysis. The result showed that the pyrolysis process of walnut shell included four stages, namely drying, pre-pyrolysis, fast-pyrolysis and slow decomposition of residue. The weight loss during the fast-pyrolysis stage and the slow decomposition stage of residue was about 55% and 32%, respectively. The pyrolysis process could be described by the first-order global model for both fast-pyrolysis and slow decomposition stages. With the method of Coats-Redfern, the average activation energy was 50.7 and 17.3kJ/mol for both pyrolysis stages, respectively. The pyrolysis speed increases with increasing of heating rate.
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    Study on Spray-drying of Ginkgo biloba Linn.Seed Paste
    ZHANG Cai-hong;HUANG Li-xin;MUJUMDAR A S
    2010, 30 (2):  17-22. 
    Abstract ( 704 )   PDF (1006KB) ( 729 )   Save
    Ginkgo biloba Linn.(GB) seed paste was used as testing material of spray drying. L16(45) orthogonal experimental design was used. Parameters of inlet air temperature, air flow rate, outlet air temperature, feed concentration were taken as affecting factors. Properties of GB seed powder, i.e., moisture content (MC), color difference (CD), mean particle size (MPS), protein mass fraction (wp), were analyzed after spray drying. From analysis of data, it was found that moisture and wpwere significantly affected by outlet air temperature, and mean particle size was affected by feed concentration. Inlet air temperature also significantly affected protein mass fraction, but significance was less than that by outlet air temperature. Finally, the optimal conditions were as follows:inlet air temperature 190℃, air flowrate 120m3/h, outlet air temperature 110℃, feed mass fraction 10%. Powder properties under this condition were: moisture mass fraction 5.20%, color difference 19.76, mean particle size 22.0μm, wp9.83%, which reached the range of the best quality, completely.
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    HPLC Determination of Maslinic Acid Content in Different Parts of Oil Olive
    JIAO Zhi-min;CHEN Long-sheng;XU Shu-wen;CHEN Lan;REN Feng-lian
    2010, 30 (2):  23-26. 
    Abstract ( 959 )   PDF (726KB) ( 1105 )   Save
    A systematic study of the distribution of maslinic acid(MA) in different parts of oil olive introduced from Longnan was carried out. The content of maslinic acid in various parts of Olea europaea Linn. was detected by HPLC. The samples were separated on a Kromasil C18 column (250mm×4.6mm, 5μm) with the mobile phase of methanol-water (volume ratio 88:12), which contained 1.0% acetic acid. The detection wave length was set at 215nm. The results showed that the content of maslinic acid in the whole olive fruit was 0.16%, while in the fruit pulp was 0.17%, in the olive leaves was 0.73%, in the epidermis of olive branches was 0.31% and in the fruit pomace was 0.41%. However, maslinic acid was not detected in the fruit stone and branches xylem. In the parts which contained maslinic acid, the average recoveries of standard addition were 94.1%, 93.9%, 95.5%, 92.3% and 94.7%(n=3) respectively, with relative standard deviations (RSD) of 2.12%, 1.85%, 2.03%, 1.69% and 1.34%(n=3) respectively. Good linearity was achieved at the feed of maslinic acid in the range of 3.15-36.6mg/L. 
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    Preparation and Cell Body Structure Property of Reticulated Polyurethane Foam Composites from Ligninsulfonate/Renewable Polyurethane Foam
    LIU Li-li;LI Chang-yu
    2010, 30 (2):  47-51. 
    Abstract ( 572 )   PDF (952KB) ( 558 )   Save
    The impacts of alcoholysis reagent (glycol and diethylene glycol) and glycol on renewable polyurethane foam (PUF) were studied. The results showed that the alcoholysis performance of glycol is better than that of diethylene glycol and viscosity of renewable PUF decreased with increase of glycol dose. Reticulated polyurethane foam composite was prepared by lignosulphonate (LS) and renewable PUF. Its microstructure, thermal conductivity as well as compressive property were studied. The thermal conductivity of the polyurethane foam composite was going up with the increased dosage of renewable PUF, which is attributed to the increase of hole-opening rate of film cell bodies with the increase of renewable PUF, so that its thermal insulating properties decreased. Compressive strength (σ10) was from 38.4 to 544kPa. The results of scanning electron microscopy (SEM) showed that the increased dosage of renewable PUF had a great effect on the thickness of cell body skeleton and cell body structure.
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    Synthesis and Property of Polyamide Resin for Water-based Inks
    DING Hai-yang;XIA Jian-ling;LI Mei;LIAN Jian-wei;YANG Xiao-hua;ZHANG Yan
    2010, 30 (2):  27-31. 
    Abstract ( 868 )   PDF (892KB) ( 579 )   Save
    Carboxyl-terminated and low-molecular weight polyamide(CLMPA)was synthesized from polycondensation reaction among oleic dimeric acid(ODA), polymerized rosin(PR)and 1,2-ethylenediamine(EDA). Polyhydroxy polyamide(PHPA)was obtained by ring-opening polymerization among adipic acid(AA), epoxy-51(E-51)and CLMPA. Polycaoboxylic polyamide(PCPA)was synthesized by esterification of PHPA with methyltetrahydrophthalic anhydride(Me-THPA), and anionic water-soluble polyamide resin(AWPA)was obtained by means of salt-formation from neutralization. The effects of PR/ODA,CLMPA/AA on the properties of the water-soluble polyamide such as water solubility,water resistance,relative molecular mass(Mr), viscosity and glass transition temperature(Tg)were investigated. The structures of the intermediates and the target product were characterized by FT-IR and 1H NMR. The results showed that the optimum molar ratios were as followed: molar ratio of PR to ODA was 4:6, molar ratio of CLMPA to AA was 2:10, the polyamide resin was water soluble, with Mr 7264, water absorption 27.6%, viscosity 42.3 Pa·s(100℃) and Tg 47.15℃.
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    Study on Properties and Performance of UV-curing Coating of 2-Hydroxyethyl Acrylate/Acrylic Rosin Derivatives
    WU Hong;LIN Ming-tao;WANG Ji-fu;WANG Chun-peng;CHU Fu-xiang;LIU Mei-hong;
    2010, 30 (2):  43-46. 
    Abstract ( 670 )   PDF (840KB) ( 894 )   Save
    Ultraviolet-curing coatings were prepared by blending acrylic rosin(β-acryloxyl ethyl)ester(ARA)with 2-hydroxyethyl acrylate(HEA) in the presence of photoinitiator 1173 and characterized by measurements of FT-IR, TGA, gel content, pencil hardness and adhesion. The results showed that the introduction of HEA can improve wetting of glass but reduce the pencil hardness of coating. The coating possessed the optimum properties of adhesion grade(grade 1), pencil hardness (2H), gel content and thermal stability when HEA fraction of coating was 20%.
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    Analyses on Chemical Compositions of Ethanolic Extractives of Propolis Collected from Two Regions in China by HPLC
    XU Yuan-jun;LUO Li-ping;LI Yan;CHEN Bin;FU Yu-xin;GAO Yin-yu
    2010, 30 (2):  61-66. 
    Abstract ( 561 )   PDF (1182KB) ( 892 )   Save
    The method of high-performance liquid chromatography (HPLC) was developed to determine 23 polyphenolic components in propolis. The ethanolic extractive of propolis (EEP) from Shandong(SD) and Yunnan(YN) Provinces respectively were analyzed. The separation was performed on ZORBAX Eclipse XDB C18 column (4.6mm×150mm, 5μm) by gradient elution. The mobile phase consisted of methanol with 0.1% formic acid aqueous solution at the flow rate of 1.0mL/min. The detection wavelengths were 256 and 280nm. The injection volume was 20μL, and the column temperature was maintained at 35℃. The result shows that mixed reference materials and EEPs could be separated well. By comparing the retention time and ultraviolet absorption spectrum, twenty compounds were detected in EEP of Shandong, and fourteen compounds were detected in EEP of Yunnan. Similarity of spectra between extractives of Shandong and Yunnan was 0.417 and 0.499 at 256 and 280nm, respectively. The chemical compositions of porpolis from Shandong and Yunnan were significantly different. The differences of climate and vege-tation may be the main reasons for the difference, since Shandong and Yunnan locate at temperate and tropic zones respectively.
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    Study on Variations of Content and Main Constituent of Essential Oil from Stem and Leaf of Linalool-type Cinnamomum camphora (Linn.) Presl in Guangxi Province
    MO Jian-guang;YANG Yi-lin;HUANG Zhi-biao;XIE Yi-xing;LU An-gen;LAO Yan-wen;ZHOU Xiang;WU You-mei;PAN Yan-kun;QIN Zi-hai
    2010, 30 (2):  72-76. 
    Abstract ( 585 )   PDF (1008KB) ( 932 )   Save
    Essential oil from stem and leaf(samples of mixed leaves and old leaves)of linalool-type Cinnamomum camphora (Linn.) Presl was extracted respectively by steam distillation method. The essential oils were analyzed with gas chromatography and GC-MS-DS quantitatively and qualitatively. The results show that content and chemical compositions of essential oil from stem and leaf of linalool-type C.camphora have great difference. The mass fraction of essential oil in leaves (1.39%) is higher than in stem (0.54%); The mass fraction of linalool in leaf essential oil (89.59%) is higher than in stem (74.49%); The mass fraction of camphor in leaf essential oil (0.61%) is lower than in stem (4.34%); The quality of leaf essential oil collected in October (linalool 92.69%, camphor 0.40%) is superior to leaves collected in July (linalool 86.49%, camphor 0.82%).
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    Refining and Application of Fractions of Biomass-pyrolysis Oil
    XU Jun-ming;JIANG Jian-chun;LÜWei;GAO Yi-wei
    2010, 30 (2):  1-5. 
    Abstract ( 510 )   PDF (477KB) ( 802 )   Save
    A novel procedure of refining biomass-pyrolysis oil was developed. The procedure was based on fractionation of the bio-oil with water into water-soluble and water-insoluble fractions. Water-soluble fraction was used to obtain ester mixture through reactive rectification. The yield of ester mixture was about 21%(based on original bio-oil). According to its molecular structure, two methods were provided to utilize water-insoluble fraction(mixture of phenolic compounds) as follows: 1)Water-insoluble fraction was used as a substitute for phenol at different ratio to prepare phenolic novolac resins. The obtained resin possessed suitable curing time and softening point as conventional novolac resins. 2)Upgraded bio-oil was obtained by Williamson reaction using phase transfer catalysis. The result of GC-MS analysis showed that carboxylic and phenolic groups in the water-insoluble fraction were transformed into corresponding esters and ethers while acidity was lowered and stability was improved.
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    Progress of Research on Preparation and Application of Nanocellulose Whiskers
    LI Jin-ling;CHEN Guang-xiang;YE Dai-yong
    2010, 30 (2):  121-125. 
    Abstract ( 1667 )   PDF (930KB) ( 3596 )   Save
    Advances of research on preparation, modification and application of nanocellulose whiskers(NCW) are reviewed. NCW are produced from natural cellulose by sulfuric-acid hydrolysis. Recent progress of research on hydrolysis process, preparation methods and conditions, characterization of properties of NCW, surface modification methods and the application of NCW in the fields of fine chemical and material science,etc. are mainly introduced.
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    Study on Purification of Solanesol
    LI Yu-shan;WANG Jing-an
    2010, 30 (2):  103-106. 
    Abstract ( 675 )   PDF (791KB) ( 747 )   Save
    Crude solanesol was purified using saponification followed by column chromatography. The saponification conditions were optimized based on the orthogonal test. Results showed that the optimal conditions were as follows: crude solanesol 50g, ethanol 250mL, 20%NaOH solution 20mL, temperature 80℃ and reaction time 3h. Using 6# solvent oil-acetic ether (10:1, volumn ratio) as eluant for column separation, the yield and purity of the product were 14% and 95.8%, respectively.
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    Catalytic Hydrogenation of Cardanol as Well as Purification and Characterization of the Product
    MAO Zhi-bo;LUO Ting-liang;WANG Yu;ZHANG Hua-sen;LIU Guo-ji
    2010, 30 (2):  52-56. 
    Abstract ( 865 )   PDF (909KB) ( 828 )   Save
    Catalytic hydrogenation of cardanol was carried out by using Raney nickel as catalyst. The effects of reaction temperature, hydrogen pressure, reaction time, amount of catalyst, stirring speed on the conversion of cardanol were systematically studied, and the stability of catalyst was also investigated. Results showed that at conditions of temperature 118℃, reaction time 4.5h, catalyst amount 1.38%(based on material mass), hydrogen pressure 3.6MPa, and stirring speed 400r/min, the conversion of cardanol reached 100%. The catalyst was not obviously deactivated after being used for 6 cycles. The product was purified by distillation and crystallization, to obtained m-pentadecylphenol of high purity which was characterized in this work.
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    Study on Extracting Eucommia ulmoides Oliv.Gum by Cellulase Pretreatment
    LIU Gui-hua;ZHANG Yong-kang;XIAO Mei-feng;PENG Xin-jun
    2010, 30 (2):  77-82. 
    Abstract ( 699 )   PDF (1325KB) ( 753 )   Save
    The conditions of enzymatic pretreatment of shell of Eucommia ulmoides Oliv. were investigated, using the amount of total sugars from enzymatic hydrolysate of shell of E.ulmoides with anthrone colorimetry and extraction yield of E.ulmoides gum as assessing index. The optimum enzymatic pretreatment conditions were:temperature 50℃, pH value 3.8,cellulase dose 0.3g, solid-liquid ratio 1:15(g:mL), extracting twice and 3h each time. E.ulmoides gum was extracted from raw materials pretreated. The gum yield of the first extraction from the pretreated shell was57.7%, which was 1.3 times of that from shells without pretreatment. The results of TLC determination showed that the composition of E.ulmoides gum extracted from pretreated shell is basically similar to that from non-pretreated shell.
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    综述评论
    Research Progress and Prospects of Dioscorea and Diosgenin
    LI Xiang;MA Jian-zhong;SHI Yun-dong
    2010, 30 (2):  107-112. 
    Abstract ( 717 )   PDF (1198KB) ( 790 )   Save
    Classification,resource distribution, breeding of dioscorea, as well as extraction, isolation, structure identification, analysis and testing, and pharmacological effects of diosgenin were demonstrated. It was found by surveying diosgenin demand and substitutes of diosgenin, that in the next 10 to 20 years, the optimum acreage of planted Dioscorea zingiberensis would be kept at (2.67-3.33)×104 hm2, diosgenin output would be kept at 2000t/a, and diosgenin price will be maintained above 450000yuan/t. Environmental benignity and high quality of diosgenin are the basic requirement of the present era. After several years market consolidation, China's D.zingiberensis, diosgenin industry will forward along the track of healthy development.
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    研究报告
    Study on Hydration of Dihydromyrcene in Subcritical Water
    ZHENG Hui-dong;GE Xiu-xiu;WANG Bi-yu;WU Yan-xiang
    2010, 30 (2):  94-98. 
    Abstract ( 736 )   PDF (1076KB) ( 739 )   Save
    Catalytic hydration of dihydromyrcenol in subcritical water(SCW) was studied using strong-acid cation exchange resin NKC-9 as catalyst. The probable reaction mechanism was explored. The influences of reaction temperature, catalyst dose, reaction pressure and molar ratio of water to dihydromyrcene on hydration were investigated. Experimental results show that dihydromyrcenol is the main hydrated product, and the reaction rate increases with the increases of temperature and dosage of catalyst. The reaction pressure has negligible effect on the reaction. Under the reaction conditions of catalyst dosage 19%, molor ratio of dihydromyrcene to water 35:1, pressure 8.0MPa, reaction time 6h, the conversion of dihydromyrcenol was 13.27% and yield of the products was 4.56%.
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    Sustainable Development of Pulp-and-paper Industry Combining with Integrated Forest-biomass Biorefinery
    GAO Yang;NI Yong-hao;ZHANG Feng-shan;QIN Meng-hua
    2010, 30 (2):  113-120. 
    Abstract ( 720 )   PDF (1490KB) ( 715 )   Save
    Studies on the integrated forest-biomass biorefinery are being intensively carried out. The integration of conventional pulping process with biomass conversion will be revolutionary for the forest industry. This approach can utilize lignocellulosic materials more effectively, and has huge impacts on the related industries. This paper reviewed the concept of integrated forest biomass biorefinery, especially the conversion of a kraft pulp mill into an integrated forest-biomass biorefinery one. Novel technologies are yet to be developed for economically utilizing forest resources, and also for the energy strategy to substitute part of fossil fuels with bio-fuels from renewable resources.
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    Research on Synthesis of n-Octyl Gallate without Water-carrying Agent
    CHEN Qian-wen;GU Wen-zhong
    2010, 30 (2):  57-60. 
    Abstract ( 632 )   PDF (855KB) ( 642 )   Save
    A new process of synthesizing n-octyl gallate was studied by using non-oxidative acid to replace concentrated sulfuric acid as catalyst without addition of water-carrying agent. The effects of different preparation parameters were studied with orthogonal test. The results show that optimum conditions of synthesizing octyl gallate were obtained as following:ratio of acid to alcohol 1:6, catalyst dose 12%, reaction temperature 120℃, reaction time 4h, average yield of product 92.3%.
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    Research on Structure Characteristics of Sweet-bamboo Lignin
    CAO Quoc-an;LI Zhong-zheng
    2010, 30 (2):  37-42. 
    Abstract ( 674 )   PDF (871KB) ( 734 )   Save
    The cellulolytic enzyme lignin(CEL) was separated from sweet-bamboo in Northern Vietnam by using enzymatic hydrolysis. The structure characteristics of lignin were analyzed by chemical method and spectroscopy, and compared with Bambusa textiles McClure in Southern China. The results showed that sweet-bamboo lignin was composed mainly of syringl, guaiacyl and p-hydroxylphenyl units, and the mass fractions of three units are 7.68%, 5.67% and 3.97%, respectively. Mass fraction of three units in sweet-bamboo was lower than in B.textiles. The mass fraction of functional groups had been changed after cooking, methoxyl group decreased to 12.35%, while phenolic hydroxyl group increased to 3.17% and carboxyl group also slightly increased to 5.99%. Cooking affects also the molecular weight of lignin. Raw material lignin mainly concentrated in the molecular weight of less than 4000(accounted for 50.5%). After slurrying, the molecular weight of <4 000 is decreased, and >8000 is increased.
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    Adsorption of Pb(II) from Aqueous Solution Using Collagen-tannin Resin
    SUN Xia;LIAO Xue-pin;SHI Bi
    2010, 30 (2):  11-16. 
    Abstract ( 608 )   PDF (1055KB) ( 889 )   Save
    Collagen was extracted by enzymatic hydrolysis of bovine hide using pepsin. The collagen-tannin resin (C-TR) was prepared via reaction of collagen with black wattle tannin and aldehyde. The adsorption behaviors of C-TR to Pb(II) in aqueous solution was investigated. It was found that C-TR has high adsorption capacity to Pb(II). The adsorption capacity of C-TR (100mg) to Pb(II) was 0.34mmol/g at 303 K and pH value 4.5 when the initial concentration of Pb(II) solution (100mL) was 1.0mmol/L. The pH value had a significant effect on the adsorption capacity of C-TR to Pb(II) and a maximal adsorption capacity was achieved around pH value 4.5. The adsorption isotherms can be described by Freundlich equation, and temperature has almost no effect on adsorption capacity. Adsorption kinetics data can be described by a pseudo-second-order equation. The breakthrough point of Pb(II) in adsorption column was around 60mL when feeding rate of Pb(II) solution (1.0mmol/L) was 30mL/h.
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    Study on Synthesis of Methyl Gallate Catalyzed by Heteropolyacid-loaded Activated Carbon
    HUANG Li;XIE Hui;TAO Bo;ZHANG Sai-nan
    2010, 30 (2):  99-102. 
    Abstract ( 789 )   PDF (865KB) ( 853 )   Save
    Methyl gallate was synthesized using the catalyst of H7PW12O42·4H2O (PW12) heteropolyacid supported by activated carbon(AC). The characteristics of the catalyst was investigated in detail including XRD analysis, N2 adsorption and NH3-TPD. The effects of catalyst on reaction conditions were studied. The results showed that under following conditions: gallic acid 0.52mol, methanol 0.4mol, loading amount of PW12 on AC 30%, reaction time 4h and catalyst dosage 5%, the yield of MG could reach 90.1%. The catalyst had a high catalytic activity, could be recovered easily and used repeatedly.
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    One-pot Synthesis of Polyethylene Glycol 400 Glucoside Rosin Ester under Atmospheric-pressure
    TANG Shi-hua;ZHANG Ke;LEI Fu-hou
    2010, 30 (2):  67-71. 
    Abstract ( 765 )   PDF (875KB) ( 717 )   Save
    Polyethylene glycol 400(PEG 400) glucoside rosin ester was synthesized with ethylene glycol 400, rosin and starch as raw material and p-toluene sulfonic acid as catalyst using one-pot method under atmospheric pressure. The optimum synthesis conditions were obtained as follows: ratio of n(PEG 400):n(glucose unit of starch):n(rosin)4.5:1.5:1, mass of catalyst 10%(based on rosin mass), reaction time 7h, reaction temperature 200℃ and acid value was less than 5mg/g. The acid value of the product refined by CaO was less than 1mg/g. The prepared sample was identified using infrared spectroscopy and elemental analysis. The synthesized product possesses good emulsifying performance.
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    Optimization of Extraction of Alkaloids from Corydalis yanhusuo W.T. Wang by Response Surface Methodology
    SHANG Xiao-jin;QIAN Jun-qing;GUO Hui
    2010, 30 (2):  32-36. 
    Abstract ( 520 )   PDF (1004KB) ( 818 )   Save
    For improving the yield of alkaloids from Corydalis yanhusuo W.T.Wang, response surface methodology was adopted to optimize the extraction process. The effects of different parameters on yield and purity of alkaloid were studied. Based on response surface methodology, the extraction conditions on the basis of single factor experiment using alkaloid yield as index were optimized. The optimal conditions were: extraction time 116 min, extraction temperature 49℃, 80% (volume fraction) EtOH as solvent, EtOH dose 10mL/g (based on raw material). Under optimal conditions, the yield of alkaloids and purity were 0.598% and 17.38% respectively, after three times extraction.
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    Conditions of Enzymolysis of Cellulose from Waste Corrugated Paper and Modification of Fiber Structure during Enzymolysis
    XIAO Ling-ping;TANG Yong;DENG Li-hong
    2010, 30 (2):  83-88. 
    Abstract ( 642 )   PDF (2748KB) ( 815 )   Save
    The effects of conditions of enzymolysis of cellulose from waste corrugated paper on glucose production, as well as the variation of crystallinity and microstructure of fibers during enzymolysis are investigated. The optimum conditions of temperature 50℃, pH value 4.8, enzyme loading 80FPU/g and substrate concentration 100g/L, after 36h of hydrolysis, 53.8g/L of glucose concentration and 76.9% of cellulose hydrolysis efficiency are obtained. The modification of crystallinity of fibers during hydrolysis is carried out in two stages. Hydrolysis mainly occurs at amorphous region firstly, causing the increase of crystallinity. Then the hydrolysis of both amorphous and crystallinic regions occurs, resulting in the crystallinity keeping stable. The photos of scanning electronic microscopy show that during hydrolysis the fragments are decorticated from the fibers, in succession the fibers are broken off and become hollow, and the structure of the fibers is completely destroyed.
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    Studies on the Extraction of Extracts from Flowers of Robinia pseudoacacia Linn.by Petroleum Ether and Its Application in Cigarettes
    ZHOU Fu-chen;WANG Yue-xia;LI Yan-qiang;GUO Xue-ke
    2010, 30 (2):  89-93. 
    Abstract ( 783 )   PDF (874KB) ( 751 )   Save
    Flowers of Robinia pseudoacacia Linn.was extracted using petroleum ether to obtain the extract. The parameters of boiling range of petroleum ether,extraction time,liquid-solid ratio on the yield of R.pseudoacacia extract were researched. Thirteen volatile components of extract were identified with GC-MS. The flavoring of the extract for tobacco was evaluated and pyrolysis at 800℃ was conducted. The result showed that the optimum extraction conditions were: 60-90℃ petroleum ether, liquid-solid ratio 4:1-5:1,extract time 4-5h. The extract can increase aroma, shield offensive odor, and increase smoke thoroughness.
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