Table of Content

30 December 2013, Volume 32 Issue 6 Previous Issue    Next Issue

1研究报告

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Short Process ECF Bleaching of Corn Stalk Rind Pulp by Organic Acid Biorefinery HUANG Ping;ZHAI Hua-min 2012, 32 (6):  1-4.  Abstract ( 709 )   PDF (922KB) ( 967 )   Save To obtain a bleaching process with a reasonable brightness, low consumption of fiber resource and energy, the bleaching properties of organic acid biorefinery corn stalk rind pulp (OABCSRP) by a short ECF bleaching process of ED1D2 were investigated in present study. The results indicates alkali extraction is high selective on delignification of OABCSRP, and the extraction is a foundation for next effective D1D2 bleaching stages. A pulp with 95.4% yield, 23.5% delignification ratio, 115 mPa·s viscosity and 44.2% ISO brightness was obtained when pulp with 10.0% concentration was treated by 4.0% NaOH for 1.5 h at 70 ℃. Interesting findings revealed that the ester linkages between lignin and carbohydrate were hydrolyzed in the extraction process. The pulp with an accumulated yield 88.0%, 124 mPa·s and brightness 74.7% ISO respectively when 4.0% NaOH and 3.6% ClO2 dosages were applied in ED1D2 bleaching. ED1D2 short bleaching process was suitable for OABCSRP bleaching to produce cultural papers. Related Articles | Metrics

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Carbon Footprint Calculation Method for Pulping and Papermaking with Straw Material and the Measurements for Lowing Carbon ZHANG Huan;ZHANG Hui 2012, 32 (6):  11-16.  Abstract ( 706 )   PDF (1010KB) ( 881 )   Save Calculation method of carbon footprint and carbon-sinks ratio of wheat straw papermaking industry was discussed in present study. The proposed method was applied to calculate the carbon-sinks ratio of a cultural paper production line (40t/d) with straw material. The ways to improve carbon-sinks ratio for China papermaking mills with straw material were proposed as well. The results showed that the life cycle assessment is suitable for the carbon footprint calculation in papermaking industry. The carbon emission and the carbon-sinks ratio for 1t paper in the typical line (40t/d) are 2248.5 kg CO2 and 0.8, respectively; The higher carbon-sinks ratio (>1.0) in papermaking industry could be realized when the production capacity increased from 40 t/d to 80 t/d, and more advanced technologies and equipments were used in wheat straw papermaking to reduce carbon emission. Related Articles | Metrics

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Effects of Washing Method on Detoxification of Steam Explosion Corn Stalk ZHANG Nan-nan;LAI Chen-huan;LI Xin;ZHU Jun-jun;ZHANG Guan-xing;YU Shi-yuan;YONG Qiang 2012, 32 (6):  32-36.  Abstract ( 702 )   PDF (985KB) ( 772 )   Save Corn stalk pretreated through steam explosion was detoxified by three washing methods. The effects of different washing methods, as well as water consumption of countercurrent washing on removal of inhibitors and ethanol fermentation of enzymatic hydrolyzate were investigated in present study. The efficiency of detoxification among tested washing methods declined by countercurrent washing, three-stage batch washing and batch washing successively. The sugar consumption and ethanol yield were 97.58% and 93.74% respectively, when the steam explosion pretreated corn stalk was detoxified by countercurrent washing with solid-liquid ratio 1∶7.5, and the concentrated hydrolyzate was fermented by Saccharomyces cerevisiae for 24 h. Related Articles | Metrics

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Isolation and Identification of 7-Oxo-8,15-isopimaric Acid in UV-cured Products of Isopimaric Acid ZHANG Lei;ZHAO Zhen-dong;LU Yan-ju;CHEN Yu-xiang;BI Liang-wu;LI Dong-mei; 2012, 32 (6):  5-10.  Abstract ( 795 )   PDF (1250KB) ( 834 )   Save A non-polymerized compound with strong UV absorption was detected during investigation on UV-cured product of isopimaric acid (iPA) by HPLC-UV. The compound was isolated through silica gel column chromatography and preparative HPLC in purity of 82.6 % analyzed with GC. It was identified as 7-oxo-8,15-isopimaric acid (7-O-8,15-iPA), a kind of oxidized derivative of iPA, by means of spectroscopic data of UV-vis, FT-IR, MS, 1HNMR and 13C NMR in accord with the data reported in references. The formation mechanism of 7-oxo-8,15-isopimaric acid from iPA was also predicted. Related Articles | Metrics

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Synthesis of Rosin Pentaerythritol Ester under Microwave Heating Conditions LI Jian-fang;SHANG Shi-bin;SONG Zhan-qian;WANG Dan; 2012, 32 (6):  17-21.  Abstract ( 782 )   PDF (948KB) ( 906 )   Save An efficient and rapid method of synthesizing rosin pentaerythritol ester is described under microwave conditions in a closed system. Conventional heating process of rosin esterification needs 270 min. This unprecedented synthesis improves the performance of the products significantly and reduces reaction time to 40 min. Furthermore, an orthogonal test of L9(34) was also designed in order to study factors which affected the color and acid value of the products. The optimized synthesis conditions are as follows: the dosage of BEP, 0.30%; the dosage of pentaerythritol, 16%; heating time, 40 min; microwave power, 200W. The rosin pentaerythritol ester with light color (Gardner 4), low acid value (12.7 mg/g), and high softening point (102℃) was obtained under optimized conditions. Related Articles | Metrics

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Direct Catalytic Conversion of Cellobiose into Sorbitol in Extremely Low Acid over Ruthenium Catalysts LI Ji-biao;WU Shu-bin;ZHANG Jun 2012, 32 (6):  37-40.  Abstract ( 752 )   PDF (956KB) ( 769 )   Save Ru/C catalyst and extremely low acid were employed for one-step conversion of cellobiose into sorbitol in the presence of hydrogen. Effects of reaction temperature, reaction time and catalyst usage on sorbitol yield were discussed. Experimental results showed that the highest sorbitol yield of 87.1% was obtained at reaction temperature of 458 K and catalyst usage of 15 % for 1 h under 3 MPa H2 with the stirring rate of 600 r/min. Meanwhile, catalyst recycling showed that Ru/C was an ideal hydrogenation catalyst with high catalytic efficiency, which could be recycled several times. Related Articles | Metrics

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Synthesis and Characterization of Cardanol Novolac Epoxy Resin HUO Shu-ping;KONG Zhen-wu;CHEN Jian;WU Guo-min;LIU Gui-feng 2012, 32 (6):  41-46.  Abstract ( 928 )   PDF (1300KB) ( 1601 )   Save Cardanol novolac epoxy resin I (Epoxy-I) and cardanol novolac epoxy resin II (Epoxy-II) with higher epoxy value were synthesized from cardanol novolac resin synthesized from cardanol reacted with formaldehyde. The effects of various reaction factors on these reactions were investigated. The results showed that the optimal reaction conditions for the synthesis of cardanol novolac resin were as follows: 3% weight ratio of cardanol used as the amount of zinc acetate, the reaction temperature 90 ℃ and the reaction time 3 h. The optimal reaction conditions for the synthesis of Epoxy-I were that the amount of quaternary BTEAC was 2 % weight ratio of cardanol novolac resin, the reaction temperature was 90 ℃ and the reaction time was 4 h. And the epoxy value of Epoxy-II reaches to the highest when the amount of epoxidizing agent is 80% the weight ratio of Epoxy-I, the reaction temperature is 70 ℃ and the reaction time is 6 h. The chemical structure of both novolac epoxy resin were characterized by FT-IR and NMR spectra. Related Articles | Metrics

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Preparation and Characterization of Poly (N-isopropylacrylamide)-poly (acrylic acid) Nanocapules NAN Jing-ya;CHEN Ying;WANG Chun-peng;CHU Fu-xiang 2012, 32 (6):  22-26.  Abstract ( 797 )   PDF (1286KB) ( 890 )   Save In this study, a novel approach has been developed for the preparation of poly (N-isopropylacrylamide)-poly (acrylic acid) (PNIPAm-PAA) nanocapules. In the first instance, the core-shell nanoparticles, which diameter was about 130 nm, were synthesized by precipitation polymerization with hydropropylcellulose-poly (acrylic acid) (HPC-PAA) particles as the core and the cross-linked PNIPAm as the shell. After the selective removal of HPC from the particles by adjusting the pH of solution to 8.0, hollow PNIPAm-PAA nanocapules were obtained and the average diameter was 500 nm. Furthermore, the loading and releasing behaviors of PNIPAm-PAA nanocapules were evaluated in mild condition by using anti-cancer drug Doxorubicin hydrochloride (Dox) as a hydrophilic model drug. It showed a super-high drug loading capacity of about 130 %, and a sustained-release characteristic under the physiological pH and temperature. Related Articles | Metrics

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Chemical Structure and Reaction Scheme of Modified Bamboo Powder with Silane Coupling Agent CHEN Qin-hui;BAI Wei-bin;XU Yan-lian;LIN Jin-huo 2012, 32 (6):  27-31.  Abstract ( 952 )   PDF (1267KB) ( 1411 )   Save The bamboo powder modified with the silane coupling agent of KH-560 (KB) was studied by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscope. The modified mechanism was also investigated in this work. Results showed that the hydrolysis of KH-560 was found to enhance the attachment on the surface of bamboo powder by the formation of hydrogen bond and dehydration condensation. XRD analysis indicated that the degree of crystallinity of bamboo powder didn't change after the modification by KH-560. However, the reaction of bamboo powder and KH-560 was certified by the appearance of absorption of ether bond in FT-IR spectrum and the XPS peak of silicon at 101.18 eV. At the same time, the binding energy of C1s changed from 288.16eV to 288.52eV and the peak of oxygen atom (attributed to C=O) at 530.98eV disappeared. All results indicated that the reaction between bamboo powder and KH-560 didn't occur on the bamboo fibre due to the exist of the strong hydrogen bonding force, but on the aldehyde groups from lignin at the absence of mechanical force and chemistry reagent. Related Articles | Metrics

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Preparation of Propyl Gallate Catalyzed by the Whole Cells of Aspergillus niger PEI Jian-jun;YAO Ling-ling;LI Xun;ZHAO Lin-guo; 2012, 32 (6):  52-56.  Abstract ( 773 )   PDF (944KB) ( 879 )   Save In the present study, Aspergillus niger cells were used as a whole-cell biocatalyst for propyl gallate production. The effects of various organic solvents, pre-treatment of the cells, substrate concentration, reaction time, and the water content in the mixture on the enzymatic reactions were investigated. Results showed that benzene was the most suitable solvent and the moisture content of mycelium was 80%. On that basis, the orthogonal experiment was performed. The maximum molar conversion (36.4%) was achieved with 0.5g hyphaes, 7.3% 1-propanol and 7mmol/L gallic acid at stirring speeds of 200r/min and reaction temperature of 40℃ in 25mL conical flask. The process has several advantages, such as mild reaction conditions, less environmental pollution, less accessory substance, and so on. Related Articles | Metrics

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Identification of Chemical Structure of Urushiol from Maoba Lacquer by HPLC-MS HE Yuan-feng;WANG Cheng-zhang;LU Rong 2012, 32 (6):  47-51.  Abstract ( 938 )   PDF (1083KB) ( 1132 )   Save Middle pressure chromatography was used to purify urushiol. Its purity reached above 90%. HPLC,HPLC-MS,MS was applied to analyze urushiol that was extracted from Maoba lacquer. HPLC was performed under a methanol-water system(volume ratio) with a flow rate of 1mL/min. Eighteen peaks appeared under UV detector of 210 nm. Thirteen compounds were separated by HPLC-MS, mainly contained C15/17 with different degrees of unsaturation. The middle pressure chromatography and HPLC could be used as a efficient preparation and analysis method. Related Articles | Metrics

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Antioxidation of Polysaccharides from Bamboo Leaves on Edible Oil ZHU Xing-yi;WANG Jian-guo;XIE Jie;GUO Qiao-feng;WANG Ping 2012, 32 (6):  57-60.  Abstract ( 944 )   PDF (1154KB) ( 951 )   Save The antioxidation of the polysaccharides from bamboo leaves on edible oil was investigated. The peroxide value (POV) was determined via Schaal oven-storage test using palm oil and rice bran oil as substrate, respectively. Results showed that polysaccharides from bamboo leaves(PBL) had good antioxidant activities on palm oil and rice bran oil with dose effect. When the amount of polysaccharides was 0.01%, the antioxidant effect with palm oil was the same as VE. VC, citric acid and tartaric acid exhibited remarkable synergistic effect on polysaccharides from bamboo leaves in the antioxidation. When the amount of polysaccharides was 0.04%, the antioxidant effect was slightly better than VE and butylated hydroxyanisole (BHA) with the maximum addition and inferior to tertiary butylhydroquinone (TBHQ). When the amount of polysaccharides was larger, the antioxidant effect boosted slightly, so the appropriate amount was 0.04%. Related Articles | Metrics

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Influence of Pichia stipitis on Xylose Fermentation KONG Duan-nan;BAI He-chao;CAO Xian-ting;WU Bo-jie;YU Shi-yuan 2012, 32 (6):  61-68.  Abstract ( 668 )   PDF (1192KB) ( 923 )   Save Effects of aeration rate, pH value and initial cell concentration on xylose fermentation by Pichia stipitis CBS 5776 were investigated in present study. The optimum initial cell concentration, and pH value rage, liquid holdup and the optimum shaking speed were 5-7g/L and 4.7-5.5, 75 mL and 150 r/min, respectively. In a 2L fermenter, the highest ethanol concentration and ethanol yield was 18.29g/L and 83.2%, respectively, when the aeration rate and fermentation time were 0.075L/min and 32h. When the aeration rate was 0, the highest ethanol concentration and ethanol yield increased to 19.09g/L and 86.5%, respectively, the optimal aeration rate for xylose fermentation by Pichia stipitis was 0-0.075L/min. The resistance ability of CBS 5776 to acetic acid was close related to initial pH value and aeration rate. The ethanol yield increased by 166.6% with the aeration rate increase on the condition of shaking speed 150r/min and pH value 5. The optimum conditions obtained in previous experiments were verified in domesticated yeast by acid steam-exploded corn stover hydrolysate as well. Related Articles | Metrics

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Synthesis of the 3-Methylenenopinone from β-Pinene QU Ling;XU Xiao-wei;WEI Bai-song;XU Xu;WANG Shi-fa 2012, 32 (6):  69-74.  Abstract ( 739 )   PDF (1008KB) ( 1021 )   Save Synthesis of the 3-methylenenopinone was carried out using β-pinene as the starting material. Nopinone was prepared by selective oxidation with acidic potassium permanganate in acetone. The influences of oxidants, solvents, reaction temperature and reaction time on the oxidation selectivity of β-pinene and the yield of nopinone were investigated. 3-Methylenenopinone was further synthesized by aldol condensation of nopinone and formaldehyde catalyzed by potassium hydroxide. The influences of the molar ratio of nopinone to formaldehyde, types and dosages of catalysts, solvents, reaction temperature and reaction time on the aldol condensation were examined in detail. The optimum reaction conditions were determined according to the results of orthogonal experiments as follows: n(formaldehyde)∶n(nopinone) molar ratio 21∶1; potassium hydroxide used as the catalyst for aldol condensation, and n(KOH)∶n(nopinone) molar ratio 1.5∶1; the reaction conducted at 65℃ for 2h without solvent. The yield of 3-methylenenopinone was over 92% under the aforesaid conditions, and its chemical structure was analyzed GC-MS, FT-IR, 1HNMR and 13CNMR spectra. Related Articles | Metrics

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Leaching Law and Pyrolysis Characteristics of Extractives from Eucalyptus grandis Pretreatment under Ethanol/Water Solution System ZHANG Bin;WU Shu-bin 2012, 32 (6):  75-83.  Abstract ( 560 )   PDF (1241KB) ( 957 )   Save Eucalyptus grandis chips were pretreated under ethanol/water solution system with a sealed helicoid furnace and four extractives were obtained by pure water and ethanol/water mixtures with ratio of 1∶4, 1∶2, 1∶1,respectively. Basic leaching rule was studied through ultimate analysis and micro particle size detection. Sugar content in each extractive was determined by ionic chromatograph analysis, meanwhile TG and Py-GC/MS reveal were designed to reveal the pyrolysis properties of extractives. The results showed that all three extractives from ethanol/water extraction had similar total extractive quality and sugar content. Very few differences were observed in view of the element content among ethanol/water extractives (EWE), but for water extractive (WE), it had more O content and less C content. Micro particle distribution of all EWE were similar, but remarkable difference could be found WE was compared with EWE. It could be concluded that roles of ethanol and water in extraction were indepen-dent. Pyrolysis properties of the WE and EWE extractives were quiet different, but for three EWEs, they showed similar pyrolysis characteristics. The main pyrolisis products of WE were ketones, phenols and acids. However, for EWE, furans, furfurals, phenols and ketones were found. Related Articles | Metrics

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Optimization of Microwave-assisted Extraction of Tannic Acid from Chinese Gallnut Using Response Surface Method QIN Qing;MIN Fan-qin;XU Hao;ZHANG Zong-he;LI Wen-jun;WANG Cheng-zhang; 2012, 32 (6):  84-88.  Abstract ( 873 )   PDF (1360KB) ( 968 )   Save The microwave-assisted extraction process of tannic acid from Chinese gallnut were optimized using response surface method (RSM). The effects of three independent variables, i.e. liquid to solid ratio, microwave extraction time and extraction temperature, on the yield of tannic acid, was also investigated. Results indicated that the optimum microwave-assisted extraction was obtained as the powder of Chinese gallnut 10 g, microwave power 600 W, liquid to solid ratio 32∶1(mL∶g), ultrasonic extraction time 7 min and temperature 62℃, respectively. Under this optimum condition, the extraction yield of tannic acid was 65.13%. Related Articles | Metrics

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Extraction and Characterization of Saponins from Sapindus GAO Fei-fei;ZHAO Yang;LUO Jin-yue; 2012, 32 (6):  89-93.  Abstract ( 776 )   PDF (1079KB) ( 886 )   Save Saponins have the functions of detoxification,eliminating phlegm and anticancer etc. It is widely used in the field of medical and daily chemical products. The saponins yields were investigated by soxhlet extraction and microwave extraction based on the leaves of Sapindus. The resonable extraction technique was obtained. It is concluded that the suitable conditions of soxhlet extraction were 80% ethanol as extractant, ratio of liquid to material 30∶1 (g∶g), extraction temperature 95℃, extraction time 3h×2. The extraction yield was 21.7%. The suitable conditions of microwave extraction were microwave power 300W, extraction temperature 70℃, 90% ethanol as extractant, ratio of liquid to material 20∶1, extraction time 45min. The extraction yield reached 22.3%. The chemical structure of target extract was identified by FT-IR, HPLC and 1HNMR. Related Articles | Metrics

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Recent Advances on Biologic Activity of Dehydroabietic Acid Derivatives CUI Yan-jie;RAO Xiao-ping;SHANG Shi-bin;SONG Jie 2012, 32 (6):  99-106.  Abstract ( 807 )   PDF (1795KB) ( 1459 )   Save Dehydroabietic acid is an important derivative of rosin. It has benzene ring and several chiral centers, and its derivatives exhibit wide range of bioactivities. They have important application in the pharmaceutical and insecticide fields. According to the structural characteristics, a series of bioactive derivatives of dehydroabietic acid were synthesized by typical carboxyl reaction, including esterification, synthesizing acyl chloride, being amine or alcohol by reduction, decarboxylated degradation, and electrophilic substitutions, removing isopropyl from aromatic ring. In this paper, recent advances on biologic activity of dehydroabietic acid derivatives are summarized from two aspects,i.e. carboxyl modification and aromatic modification. Related Articles | Metrics

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Purifying Effect of the Straw Atmospheric Acid Hydrolysate WANG Yong-gui;ZHOU Ya-xin;YUE Jin-quan 2012, 32 (6):  94-98.  Abstract ( 705 )   PDF (977KB) ( 859 )   Save Based on the utilization technology for the whole components from rice straw by extrusion method, the hydrolysate's purifying process and effects were investigated. The results showed that the optimum additional hydrolysis time was 1h, and appropriate amount of activated carbon was 25%. Under these conditions, the purity of hydrolysate reached up to 95%, the loss ratio of reducing sugar was below 5% and the transmittance of hydrolysate was 97.7%. This condition could meet production requirements of xylose or xylitol. Related Articles | Metrics

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Research Progress of Chemical Constituents and Pharmacology of Cassia LI Ting;FENG Zhan-min;YANG Xun-yun;WANG Li-qin 2012, 32 (6):  107-118.  Abstract ( 879 )   PDF (1564KB) ( 2378 )   Save Plants of Cassia genus were widely used as folk medicines. This review summarized the research progress of the chemical constituents of Cassia and their pharmacological effects. It will provide reference basis for their further research and development. Related Articles | Metrics