稻草皮层硅化物的XPS研究（Ⅰ）
邱玉桂1，2 陈春霞2 欧海龙2 汤丁亮3
（1.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640；2.东莞市质量计量监督检测所，广东东莞，523120；3.厦门大学分析测试中心，福建厦门，361005）
摘 要：对稻草茎部和叶鞘的外表面及穗轴等进行了皮层硅化物的X射线光电子能谱（XPS）研究。结果表明，所研究的几个部位皮层中，自外至里，硅化物的含量及分布具有相同的规律性；茎部皮层外表面硅化物的含量（面积）最低，但半峰宽则比皮层内部高；叶鞘及穗轴的皮层外表面硅化物的含量及半峰宽均比其皮层内部低。初步测定表明，所有部位中的硅化物均为无机硅化物，不同部位硅化物的组成不同；但各测定点的半峰宽都明显高于基准值1.57，说明在测定范围内的硅化物均是由两种或两种以上的硅化物组成的。因此，对各部位的Si2P峰均需进行分峰拟合分析才能得到正确的结果。
关键词：稻草皮层；硅化物含量及组成；XPS；半峰宽；分峰拟合
中图分类号：TS721+.3
文献标识码：A
文章编号：1000-6842（2009）03-0001-05
Study on Silicides in Cuticle of Rice Straw by Means of XPS （Ⅰ）
QIU Yu-gui 1,2,* CHEN Chun-xia2 OU Hai-long2 TANG Ding-liang3
（1. State Key Lab of Pulp & Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640; 2. Dongguan Institute of Metrology and Quality Supervision Testing, Dongguan, Guangdong Province, 523120; 3. Analytical & Testing Center, Xiamen University, Xiamen, Fujian Province, 361005）
（*E-mail: lcygqiu@scut.edu.cn）
Abstract：The silicides in the outer surface cuticle of rice straw stem and leaf sheath as well as the cuticle of rice shaft were researched by means of XPS.The results showed that the content profile of silicides in the above parts of rice stem are in the same pattern. The outer surface of the rice stem cuticle has the lower silicide content and higher full-width at half-maximum(FWHM) than that in the inner cuticle layers. The outer-surfaces of cuticle of leaf sheath and rice shaft show lower silicide content and FWHM than that in the inner layers of the cuticle. Our preliminary studies showed that all silicides are inorganic silicides but they have different composition in different parts of rice straw. Because of the FWHM of the Si2P peaks of the tested samples is obviously higher than the standard value of 1.57, the silicides in all above parts must be consisted of two or more than two sorts of silicides, and all Si2P peaks have to be further demonstrated by peak-differentating and imitating analysis.
Key words：cuticle of rice straw；the content and composition of silicides；XPS；full-width at half-maximum(FWHM)；peak-differentiating and imitating
（责任编辑：常 青）
稻草皮层硅化物的XPS研究(Ⅱ)
邱玉桂1，2 陈春霞2 欧海龙2 汤丁亮3
（1.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640；2.东莞市质量计量监督检测所，广东东莞，523120；3.厦门大学分析测试中心，福建厦门，361005）
摘 要：用XPS测定结合分峰拟合分析，研究稻草茎部、叶鞘、穗轴等部位皮层中硅化物的组成。结果表明，在实验范围内，各部位中的硅化物均由有机硅化物和无机硅化物组成，但都以无机硅化物为主，并且不同部位中硅化物的组成有明显的差异，无机硅化物与有机硅化物的比例也不同。测定出的无机硅化物主要有5种形式的SiO2、钠沸石、Na2SiF6、滑石、高岭土、硅灰石、分子筛型物质及富铝红柱石等；有机硅化物中主要是Ph3Si-O-SiPh3、Et3SiCl、Et2SiCl2、EtSiCl3、Et3SiBr、树脂及线状p-Methylsil等。
关键词：稻草皮层；XPS；分峰拟合分析；无机硅化物；有机硅化物
中图分类号：TS721+.3
文献标识码：A
文章编号：1000-6842（2009）03-0006-05
Study on Silicides in Cuticle of Rice Straw by Means of XPS （II）
QIU Yu-gui1,2,* CHEN Chun-xia2 OU Hai-long2 TANG Ding-liang3
（1. State Key Lab of Pulp & Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640; 2. Dongguan Institute of Metrology and Quality Supervision Testing, Dongguan, Guangdong Provice， 523120; 3. Analytical & Testing Center, Xiamen University, Xiamen, Fujian Province, 361005）
（*E-mail: lcygqiu@scut.edu.cn）
Abstract：The silicide components in cuticle of rice straw stem, leaf sheath and rice shaft were studied by means of XPS-peak-differentation-imitating analysis. The results showed that, under experimental conditions, the silicides in every above part are composed of inorganic and organic silicides, and the ratio of inorganic silicides to organic silicides are distinctly different from each other. And most of the silicides are inorganic. Silicides including five kinds of SiO2, the Vycor, quartz, alpha cristabal and gel, and many other inorganic silicides, e.g. Ca3Si3O9, Natrollite, Na2SiF6, Talc, Kaolinite, several sorts of Mol. Sieve, Al2SO5 etc. Meanwhile there are many sorts of organic silicides such as Ph3Si-O-SiPh3, Et3SiCl, Et2SiCl2, EtSiCl3, p-Methylsil （linear and resin）, etc.
Key words：cuticle of rice straw；XPS；peak-differentation-imitating；inorganic silicides；orgamic silicides
（责任编辑：常 青）
桉木半纤维素预提取的效果评价——两种测定方法之间的关系
迟聪聪 张 曾 刘 轩 戈玮玮
（华南理工大学制浆造纸工程国家重点实验室，广东广州，510640）
摘 要：对桉木片分别进行碱预处理和热水预水解，采用间接法（差值计算法）和直接法（比色法）两种方法测定和计算了两种预处理条件下的戊聚糖的提取率。实验结果表明，两种测定方法所得戊聚糖提取率之间存在一定关系。对碱预处理试样，两种方法之间的关系为y=4.6682lnx-5.5536，相关系数R2=0.9901；对热水预水解试样，两者之间呈现较好的线性关系，关系方程为y=0.5612x-1.2086，相关系数R2=0.9872（y与x分别表示比色法和差值法得到的结果）。因此，可以根据比色法的测定结果推算出预处理后木片的戊聚糖含量，从而用简单快速的比色法来评价预处理后木片的戊聚糖提取率。
关键词：桉木；半纤维素；戊聚糖提取率；比色法；差值法
中图分类号：TS71+1
文献标识码：A
文章编号：1000-6842（2009）03-0011-04
Evaluation of Hemicellulose Pre-extraction Efficiency ——The Relationship between Two Determination Methods
CHI Cong-cong* ZHANG Zeng LIU Xuan GE Wei-wei
（State Key Lab of Pulp & Paper Engineering, South China University of Technology,Guangzhou, Guangdong Province, 510640）
（*E-mail: congcongchi@163.com）
Abstract：Alkaline pretreatment and hot water prehydrolysis of eucalyptus chips were carried out. Two methods were used to determine and calculate the extraction yield of pentosan or pentose. One is indirect method, which is based on the difference of pentosan contents between the chips with and without pre-extraction. The other method is to directly measure the pentosan or pentose content in the extracting liquor with spectrophotometric method. The results indicated that there is certain relationship between the two methods. For the alkaline pre-extraction, the relationship can be expressed as y=4.6682lnx-5.5536 （R2=0.9901）. For the hot-water-hydrolyzed samples, good linear relationship is shown, which can be expressed as y=0.5612x-1.2086 （R2=0.9872）, y and x in the equations represent the results from spectrophotometric method and differential approach, respectively. The pentosan content in the extracted chips can be calculated based on the equations and the spectrophotometric results. Therefore, a simple and rapid method of spectrophotometry can be used to evaluate the extraction yield of pentosan from the extracted chips.
Key words：eucalyptus；hemicellulose；extraction yield of pentosan；spectrophotometric method；differential approach
（责任编辑：王 岩）
碱抽提乙醇麦草浆纤维表面性质的AFM和XPS研究
徐永建1，２ 张美云1,2 李可成3
（1.陕西科技大学陕西省造纸技术与特种纸品开发重点实验室，陕西西安，710021；2.陕西科技大学教育部轻化工助剂化学与技术重点实验室，陕西西安，710021；3.加拿大New Brunswick大学化学工程系，加拿大弗雷德里克顿，Ｅ3B2L2）
摘 要：研究了碱抽提乙醇麦草浆纤维表面的形貌学特征、化学组成和木素的分布。AFM研究结果表明，随抽提时间的延长，碱抽提后乙醇麦草浆纤维表面无定形木素覆盖区域面积减少，木素颗粒减少，颗粒尺寸减小，部分区域呈现清晰的微细纤维纹路，反映出木素在纤维表面的分布不均匀，纤维表面不同区域木素对碱抽提的适应性也不同。XPS分析结果表明，与未经碱抽提的乙醇麦草浆相比，碱抽提后的乙醇麦草浆纤维表面O/C比值显著下降，而更接近木素O/C比值的理论值，说明碱抽提后乙醇麦草浆纤维表面仍然存在木素，在碱抽提过程中也存在溶解木素在纤维表面二次吸附和沉积的现象。
关键词：乙醇麦草浆；碱抽提；木素沉淀；AFM；XPS
中图分类号：TS743+.9
文献标识码：A
文章编号：1000-6842（2009）03-0015-04
Study on Surface Properties of Alkali-extracted Ethanol Pulp Fibers by Using AFM and XPS
XU Yong-jian1,2,* ZHANG Mei-yun1,2 LI Ke-cheng3
（1. Shaanxi Province Key Lab of Papermaking Technology and Specialty Paper, Shaanxi University of Science and Technology, Xian, Shaanxi Province, 710021; 2.Key Lab of Auxiliary Chemistry and Technology for Chemical Industry of Education Ministry, Shaanxi University of Science and Technology, Xian, Shaanxi Province, 710021; 3.Univercity of New Brunswick， Fredericton, Canada,E3B2L2）
（*E-mail: xuyongjian@sust.edu.cn）
Abstract：The microscopic morphology, chemical composition and lignin distribution of alkaline-extracted ethanol wheat straw pulp were studied using AFM and XPS. AFM images showed that the amorphous lignin area of ethanol wheat straw pulp fiber surface decreases with alkaline extraction, the number and size of lignin particles become fewer and smaller, fibrillar structure distinctly appears on some region. It proves that the distribution of lignin on fiber surface is not homogeneous, and the response of lignin at different area of fiber surface to alkaline extraction is dissimilar too. XPS results showed that the O/C ratio of ethanol wheat straw pulp fiber surface decreases dramatically after alkaline extraction and more close to the theoretical O/C ratio of lignin compared to ethanol wheat straw pulp. Both results prove that lignin still exists on the alkaline-extracted fiber surface and dissolved lignin can precipitate back onto the fiber surface during alkaline extraction.
Key words：ethanol wheat straw pulp；alkali extraction；lignin precipitation；XPS；AFM
（责任编辑：马 忻）
非木材化学浆表面超微结构的AFM观察
李 辉 付时雨* 刘 浩 詹怀宇
（华南理工大学制浆造纸工程国家重点实验室，广东广州，510640）
摘 要：利用原子力显微镜（AFM）
研究了几种非木材化学浆DQP漂白前后纤维表面超微结构的变化。经过DQP漂白，几种非木材化学浆的白度达到80%以上，脱木素率均超过88%，漂白对几种非木材化学浆的强度有一定的提高，但作用效果因原料种类而异。利用AFM对纸浆纤维表面进行观察，结果表明，漂白前覆盖在纤维表面的颗粒状物质经过漂白后溶出，反映了表面木素的脱除。另外，大量微细纤维暴露出来，图像的相差降低，反映了漂白后纤维表面的亲水性和均一性得到提高，即漂白后纸浆表面性质得到改善，这可能是纸浆强度提高的原因。
关键词：非木材浆；纤维；超微结构；原子力显微镜（AFM）
中图分类号：TS721+.3
文献标识码：A
文章编号：1000-6842（2009）03-0019-05
The Ultrastructure of Non-wood Pulps Studied by Atomic Force Microscopy
LI Hui FU Shi-yu* LIU Hao ZHAN Huai-yu
（State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640）
（*E-mail: shyfu@scut.edu.cn）
Abstract： The ultrastructures of several non-wood pulps before and after bleaching were studied by Atomic Force Microscopy （AFM）.The results indicated that all non-wood pulps could be bleached to a brightness of above 80% ISO by using a DQP bleaching sequence, with the delignification rate more than 88% and improved strength, but the results vary from different raw materials. The results of AFM showed that the granules covered on fibers surface were disappeared after bleaching, which was ascribed to the removal of lignin. Furthermore, the exposed cellulose microfibrils and the decreased phase contrast indicated the increase of hydrophilicity and homogeneity of fiber surfaces, and the pulp surface properties improved, this probably was the reason of pulp strength improved.
Key words：non-wood pulps；fiber；ultrastucture；Atomic Force Microscopy
（责任编辑：孙秋菊）
化学氧化预处理对MFC性能的影响
张俊华1,2 宋海农1,* 林 鹿2 刘新亮1
(1.广西大学轻工与食品工程学院，广西南宁，530004；2.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640)
摘 要：以漂白硫酸盐竹浆为原料，结合PFI磨的前期磨浆预处理和高压均质机的后期高压均质化处理制备微纤化纤维素（MFC），探讨了由2,2,6,6-四甲基哌啶氧化物自由基(TEMPO)、NaClO和NaBr组成的氧化体系的主要工艺参数（TEMPO、NaBr及NaOH用量）对竹浆MFC主要性能（如相对保水值）的影响，确定了最佳的化学预处理工艺。基于氧化后浆料的黏度与最终所得MFC的相对保水值之间的关系以及在优化氧化条件下NaOH用量与氧化后浆料黏度的关系，建立了预测MFC相对保水值的数学方程。
关键词：MFC；化学氧化；TEMPO；竹浆
中图分类号：TS102.6+4
文献标识码：A
文章编号：1000-6842（2009）03-0024-04
The Effect of Chemical Oxidation Pretreatment on the Preparation of Microfibrillated Cellulose （MFC）
ZHANG Jun-hua1,2 SONG Hai-nong1，* LIN Lu2 LIU Xin-liang1
（1. School of Light Industry and Food Engineering, Guangxi University, Nanning, Guangxi Zhuang Autonomous Region, 530004; 2. State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640）
（*E-mail: hnsong@gxu.edu.cn）
Abstract：MFC can be obtained from bleached KP bamboo pulp using a procedure containing PFI mill pretreatment and high pressure homogenization. A chemical oxidation system is consisted of TEMPO, NaClO and NaBr, the effects of chemical oxidation pretreatment parameters such as the dosages of TEMPO, NaBr and NaOH on the main property such as relative water retention value （WRV） of bamboo MFC were investigated, and the optimal chemical pretreatment process was also defined. A mathematic equation for predicting the relative WRV of MFC, which is based on the relation between the viscosity of the oxidized pulp and the relative WRV of MFC, the relation between the viscosity of the oxidized pulp and the dosage of NaOH in the optimized oxidation condition, was established.
Key words：microfibrillated cellulose；chemistry oxidation；TEMPO；bamboo
（责任编辑：梁 川）
速生桉木及其KP和氧脱木素浆中木素结构的变化
郭三川1 詹怀宇1 罗小林1,* 程合丽1 付时雨1 柴欣生1，2
（1.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640；2.乔治亚理工大学造纸研究所，美国亚特兰大，GA30332）
摘 要：用不同方法从速生桉木及其卡伯值分别为17.1和9.5的KP和氧脱木素浆中分离木素，用常规的光谱分析和硝基苯氧化法对纯化的木素进行表征。结果表明，3种木素样品中，n(紫丁香基)∶n(愈创木基)∶n(对-羟苯基)分别为1.5∶1.0∶0.3、2.3∶1.0∶0.2和1.8∶1.0∶0.3；
在硫酸盐蒸煮和氧脱木素过程中，木素中大量的β-O-4芳基醚键被破坏，羧基含量不断增加。从31P-NMR定量分析的对比研究可知，速生桉木中的对-酚羟基较三倍体毛白杨和南方松的难脱除且氧脱木素中木素发生缩合的程度较高。
关键词：速生桉木；木素结构；硝基苯氧化；UV-Vis；FT-IR；31P-NMR
中图分类号：TS749
文献标识码：A
文章编号：1000-6842（2009）03-0028-05
Structural Change of Fast-growing Eucalyptus Lignin during KP Pulping and Oxygen Delignification
GUO San-chuan1 ZHAN Huai-yu1 LUO Xiao-lin1,*
CHENG He-li1 FU Shi-yu1 CHAI Xin-sheng1,2
（1. State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640; =2. Institute of Paper Science and Technology, Georgia Institute of Technology, Atlanta, Georgia, USA, GA 30332）
（*E-mail: luoxiaolin128@yahoo.com.cn）
Abstract：Fast-growing eucalyptus was cooked and oxygen delignified to kappa number 17.1 and 9.5 respectively, three lignin samples were extracted with two-stage method from wood, kraft pulp and oxygen delignified pulp. The purified lignin samples were characterized by UV, FT-IR, 31P-NMR and the alkaline nitrobenzene oxidation. Noticeable amounts of aliphatic hydroxyl, condensed phenolic hydroxyl, guaiacyl and demethylated phenolic hydroxyl, and traces of both p-phenolic hydroxyl and carboxyl were identified in three lignin samples. Nitrobenzene oxidation analysis showed that the molar ratio of S∶V∶H in three lignin preparations were 1.5∶1.0∶0.3, 2.3∶1.0∶0.2 and 1.8∶1.0∶0.3, respectively.
Besides, β-O-4 aryl ether bonds in lignins were well cleaved and —COOH content increased during Kraft cooking and oxygen delignification process. It could be found from the results of 31P-NMR analysis that p-phenolic hydroxyl of eucalyptus lignin was more difficult to be removed than other species like poplar and southern pine, and the degree of condensation was also higher than the other species.
Key words：fast-growing eucayptus；structure of lignin；nitrobenzene oxidation；UV-Vis；FT-IR；31P-NMR
（责任编辑：陈丽卿）
未漂硫酸盐浆过氧化物酶催化交联的研究
王 鹏1 谢益民2,* 范建云1
(1.莆田市产品质量监督检验所，福建莆田，351100； 2.湖北工业大学化学与环境工程学院，湖北武汉，430068)
摘 要：低卡伯值未漂硫酸盐阔叶木浆与松柏醇葡萄糖苷在过氧化物酶体系存在下可发生聚合反应，生成脱氢聚合物（DHP）及DHP-碳水化合物复合体。用红外光谱和高分辨率CP/MAS 13C-NMR对DHP-碳水化合物复合体结构进行分析。结果表明，DHP-碳水化合物复合体中DHP结构单元之间主要通过β-O-4、β-β、β-5和β-1方式连接，DHP结构单元还通过缩醛键、苯甲酯键和苯甲醚键与浆中碳水化合物相连；经过松柏醇葡萄糖苷处理后，纸张的干强度提高不大，但湿强度为空白样的2.1倍。
关键词：未漂硫酸盐浆；过氧化物酶；松柏醇葡萄糖苷；DHP-碳水化合物复合体；交联
中图分类号：TS749
文献标识码：A
文章编号：1000-6842（2009）03-0033-04
Study on Crosslinking of Unbleached Kraft Pulp Catalyzed by Peroxidase
WANG Peng1 XIE Yi-min2,* FAN Jian-yun1
（1. Putian Institute of Supervision & Testing on Product Quality, Putian, Fujian Province, 351100； 2. School of Chemical & Enviromental Enginecring, Hubei University of Technology, Wuhan, Hubei Province, 430068)
（*E-mail: ppymxie@sdili.edu.cn）
Abstract：Dehydrogenation Polymer （DHP） and DHP-Carbohydrate Complexes were prepared through polymerization of low kappa number unbleached kraft hardwood pulp and coniferin in existence of peroxidase system. FT-IR and CP/MAS 13C-NMR were used to analyze the structure of DHP-carbohydrate complexes. It was found that DHP-carbohydrate complexes, which could produce crosslinking between fibers, were formed on the surface of fibers. The structural units of DHP-carbohydrate complexes were connected by β-O-4, β-β, β-5 and β-1 structures. Furthermore, DHP was also linked with fibers of kraft pulp by acetal linkages, benzyl ether linkages and ester bonds. Dry strength of paper was not enhanced obviously after kraft pulp was treated with coniferin, but the wet strength was increased by 2.1 times as the blank sample.
Key words：unbleached pulp；peroxidase；coniferin；DHP-carbohydrate complexes；crosslinking
（责任编辑：陈丽卿）
漆酶体系酶解马尾松浆表面性能的研究
尤纪雪 王玉秀
（南京林业大学化学工程学院，南京林业大学江苏省制浆造纸科学与技术重点实验室，江苏南京，210037）
摘 要：对漆酶/介体体系（LMS）、由白腐菌直接合成的漆酶/木聚糖酶体系（LXS）以及复配的漆酶/木聚糖酶体系(L+X)3种漆酶体系降解木质素的能力进行比较，并应用扫描电镜及X射线光电子能谱（XPS）表面分析等手段从微观角度探讨了酶处理降解木质素的机理。结果表明，L+X降解木质素的能力不如LXS和LMS，若用L+X取代LMS并不能达到理想的处理效果。通过扫描电镜观察及浆料的XPS表面分析，进一步证明了LXS具有与LMS相似的木质素降解能力，用LXS完全可以代替LMS用于生物制浆和生物漂白等领域。
关键词：漆酶/木聚糖酶体系；漆酶/介体体系；木质素脱除；XPS分析
中图分类号：TS743+.14
文献标识码：A
文章编号：1000-6842（2009）03-0037-05
Study on Surface Characteristics of the Masson Pine Pulp Enzymelyzed with Three Laccase Systems
YOU Ji-xue* WANG Yu-xiu
（College of Chemical Engineering, Nanjing Forestry University, Jiangsu Provincial Key Lab of Pulp and Paper Science and Technology, Nanjing, Jiangsu Province, 210037）
（*E-mail: yjxaxn@yahoo.com.cn）
Abstract：The delignification abilities of laccase/mediator system （LMS）, laccase/xylanase system （LXS） from white rot fungus and composite laccase/xylanase （L+X） were compared in this paper. The mechanisms of lignin degradation with three enzyme systems treatment were studied by the analysis of X-ray photoelectron spectroscopy （XPS） and Scanning electron microscope （SEM）. The results indicated that the delignification ability of L+X is not as good as LXS and LMS. The SEM observation and surface analysis of the pulp further illustrated that LXS has as strong delignification ability as LMS. The LXS can entirely replace expensive and complicated LMS for bio-delignification application.
Key words：laccase/xylanase system；laccase/mediator system；Bio-delignification；X-ray photoelectron spectroscopy （XPS）
（责任编辑：郭彩云）
超声处理对蔗渣在碳酸乙烯酯中液化的影响
吴学众 谌凡更* 李延鹏 周雪松
(华南理工大学制浆造纸工程国家重点实验室，广东广州，510640)
摘 要：研究了超声处理对蔗渣形态结构以及蔗渣在碳酸乙烯酯中液化行为的影响。蔗渣经超声处理后，表面变得较粗糙，细胞壁在一定程度上破碎，出现很多微孔，从而有利于液化反应的进行。蔗渣超声处理前后的红外光谱表明，纤维的组成和结构并无明显变化。实验表明，当超声频率为28 kHz时，蔗渣液化反应的残渣率最低。延长超声处理时间或者增大超声功率都有利于降低液化反应的残渣率。超声处理缩短了液化达到最低残渣率的时间。合适的超声处理可以使液化产物的相对分子质量分布变窄，但对液化产物相对分子质量影响较小。
关键词：蔗渣；超声；液化；空化
中图分类号：TS749+.6
文献标识码：A
文章编号：1000-6842（2009）03-0042-05
Impact of Ultrasonic Pretreatment on the Liquefaction of Bagasse in Ethylene Carbonate
WU Xue-zhong CHEN Fan-geng* LI Yan-peng ZHOU Xue-song
（State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640）
（*E-mail: fgchen@scut.edu.cn）
Abstract：The influences of ultrasonic pretreatment on the morphology and liquefaction behavior of bagasse were studied. SEM images showed that the fiber surface of bagasse became less compact and the cell wall was broken severely after sonication. The FT-IR spectra of bagasse, however, showed that no significant change of chemical structure occurred after sonication. These increase the accessibility of the bagasse fiber, accelerate the liquefaction, decrease the coupling of the free radicals derived from the liquefaction intermediates, which are in favor of liquefaction. The impacts of the sonication time, the frequency and the power of ultrasound on the morphology and liquefaction behavior of bagasse were investigated. The result showed that suitable frequency for the treatment is 28 kHz. Both prolonging the time of sonication and increasing the power of ultrasound reduce the residue rate of the liquefaction. The liquefaction process is also accelerated after sonication. The relative molecular weight distribution of the liquefaction product, however, has little change after the ultrasonic pretreatment, indicating that the liquefaction mechanism is not changed by sonication.
Key words：bagasse；ultrasound；liquefaction；cativation
（责任编辑：刘振华）
纳米TiO2光催化降解紫丁香基木素模型物
王 昶 李晨陶 贾青竹 李桂菊 刘 芳
（天津科技大学海洋科学与工程学院，天津，300457)
摘 要：在光催化反应器中，以紫外灯作为光源，对紫丁香基木素的模型物紫丁香醇进行光催化降解实验，讨论了悬浮体系中纳米TiO2光催化降解紫丁香醇的反应特性。实验结果表明，在避光条件下反应60 min后，溶液中紫丁香醇在纳米TiO2催化剂表面可以达到吸附解吸平衡，纳米TiO2表面饱和吸附量为起始质量浓度的16.3%；根据降解吸光度曲线，当纳米TiO2用量0.4 mg/L、pH值7、连续曝气和搅拌条件下，经一定光强的紫外光照射12 h，初始质量浓度为40.5 mg/L的紫丁香醇溶液去除率达到52.08%，继续光照4 h，最终可以完全矿化；根据降解吸光度曲线和特征官能团显色实验初步推断：紫丁香醇结构中部分双甲氧基在光照条件下，与苯环发生了断裂，生成了具有单甲氧基结构的中间体——愈创木酚；并定量分析了降解过程中紫丁香醇和愈创木酚的质量浓度。
关键词：TiO2光催化降解；紫丁香基木素；愈创木基木素；吸附平衡
中图分类号：X793
文献标识码：A
文章编号：1000-6842（2009）03-0047-05
Photocatalytic Degradation of Model Compound-syringe lignin by Titanium Dioxide Suspension
WANG Chang* LI Chen-tao JIA Qing-zhu LI Gui-ju LIU Fang
（College of Marine Science and Engineering, Tianjin University of Science & Technology, Tianjin, 300457）
（*E-mail: wangc88@163.com）
Abstract：The degradation of the syringe lignin obtained from organic wastewater in a cylindrical photocatalytic reactor, in which the suspended TiO2 was used as activated photocatalyst and a 11W UV lamp （λ＝253.3nm） as light source was studied. The experimental results showed that the syringe could reach adsorption and desorption equilibrium on the surface of TiO2 after 60 min dark reaction, and max adsorption amount was 16.3%; removal rate reached 52.08% with 12 hours illusion, then after 4 hours SL could be completely degraded. According to the absorbance curve and color shade measuring of functional groups, it could be estimated that the double methoxy of the syringe partly broke and became single methoxy structure like guaiacol under illustration condition. The concentrations of the syringe and guaiacol were quantitatively analyzed by a combination formula.
Key words：TiO2 photocatalytic degradation;guaiacol lignin;syringe lignin;adsorption equilibrium
（责任编辑：郭彩云）
纳米TiO2光催化氧化紫丁香醇降解机理研究
王 昶 李晨陶 贾青竹 李桂菊 刘 芳
（天津科技大学海洋科学与工程学院，天津，300457)
摘 要：采用自制纳米TiO2作光催化剂，在一定降解条件下，对木质素模型的紫丁香醇(SL-M)光催化降解的动力学进行了研究。实验结果表明，SL-M的光催化降解过程包括吸附和降解两个过程，SL-M在TiO2光催化剂表面上的吸附常数Ka=2.754×10-2，最大吸附量Qmax=11.468 mg/g，运用L-H方程讨论了SL-M的降解动力学，并得到反应动力学方程1/r=3.675/c+0.1012。同时，探论了降解过程的各种单因素条件如溶液初始质量浓度、溶液pH值、曝气量对SL-M降解速率的影响。
关键词：紫丁香醇；光催化降解；反应动力学
中图分类号：C643；X7
文献标识码：A
文章编号：1000-6842（2009）03-0052-04
Study on the Photocatalytic Degradation Mechanism of Syringe Lignin with TiO2
WANG Chang* LI Chen-tao JIA Qing-zhu LI Gui-ju LIU Fang
（College of Marine Science and Engineering, Tianjin University of Science & Technology, Tianjin, 300457）
（*E-mail: wangc88@163.com）
Abstract：The photo-catalytic degradation kinetic mechanism of syringe lignin（SL）（OHC6H3（OCH3）2）was investigated using self-prepared TiO2 as an activated catalyst. The results showed that the SL photo-catalytic degradation consisting two processes of adsorption and degradation. The adsorption equilibrium constant on TiO2 surface Ka=2.754×10-2, max adsorption amount Qmax=11.468 mg/g. Reaction kinetic equation 1/r=3.675/c+0.1012 was derived based on the discussion of degradation kinetic of SL with L-H equation. Some factors affected SL degradation rate, such as solution initial concentration, pH, and oxygen amount were discussed.
Key words：syringe lignin;TiO2 photocatalytic degradation;reaction kinetics equations
（责任编辑：常 青）
高分散改性蒽醌的制备工艺优化
姚占静 郭 睿 张春生
（陕西科技大学化学与化工学院，陕西西安，710021）
摘 要：以苯乙酮为溶剂将蒽醌溶解，用转相法对油相进行乳化，制备出O/W型蒽醌乳液，以提高乳液在蒸煮液中的分散性。通过正交实验，得出了最佳乳化条件，并将制备的蒽醌乳液在硫酸盐法制浆中进行了应用。结果表明，最佳乳化条件为：转相温度95℃、乳化时间45 min、Span-80用量0.6 g、Tween-80用量2.0 g、Tween-20用量1.0 g、去离子水用量50 mL，采用剂在油中法进行乳化。通过蒸煮对比实验，得出蒽醌乳液较晶体蒽醌蒸煮液表面张力降低了28.4%，残碱有所提高，纸张性能也有所提高。蒽醌乳液浆色浅，纸张白度、抗张指数、耐破指数和撕裂指数分别较晶体蒽醌浆提高了６.２个百分点、4.9%、3.8%和4.7%。
关键词：蒽醌；乳化；稳定性；纸浆得率
中图分类号：TS727+.1
文献标识码：A
文章编号：1000-6842（2009）03-0056-05
Optimal Preparation Process and Application of a High Dispersed Modified Anthraquinone
YAO Zhan-jing* GUO Rui ZHANG Chun-sheng
（College of Chemistry and Chemical Engineering, Shaanxi University of Science & Technology, Xian, Shaanxi Province, 710021）
（*E-mail: yaozhanjing2008@163.com）
Abstract：In order to increase the dispersion of anthraquinone in cooking liquor, the oil-in-water （O/W） emulsion of anthraquinone was prepared by dissolving the anthraquinone with hypnone at fist then emulsifying the oil phase by using phase inversion process. The emulsification conditions were optimized by using orthogonal design, and the emulsion of anthraquinone was applied in KP cooking. The result showed that the best emulsification conditions were: phase inversion temperature was 95℃, emulsifying time was 45 minutes, the dosages of Span-80, Tween-80, Tween-20 and water were 0.6 g, 2.0 g, 1.0 g and 50 mL respectively, anthraquinone emulsification was carried out by the method of putting the agent in the oil. In the KP cooking experiment, the surface tension of cooking liquor decreased by 28.4% and residual alkali increased in some extent compared with using crystal anthraquinone for cooking. The qualities of resultant paper including brightness, tensile index, burst index and tear index increased 6.2% 4.9%, 3.8%, and 4.7% respectively.
Key words：anthraquinone; emulsification; stability; pulp yield
（责任编辑：马 忻）
交联聚乙二醇二丙烯酸酯的制备及对漆酶的固定化研究
赵 敏1 孟庆辉2 王 炎3
（1.东北林业大学生命科学学院，黑龙江哈尔滨，150040；2.哈尔滨工业大学应用化学系，黑龙江哈尔滨，150001；3.哈尔滨工业大学理学中心，黑龙江哈尔滨，150001）
摘 要：采用3种不同相对分子质量(600、6000、20000)的聚乙二醇(PEG)为单体合成了聚乙二醇二丙烯酸酯，所得产物经偶氮二异丁腈引发交联后得到具有溶胀性的固体材料，将材料作为载体通过物理吸附用于漆酶的固定化。研究了载体制备条件对固定化漆酶酶活的影响，发现交联的聚乙二醇(PEG20000)二丙烯酸酯对漆酶的固定化效果最好, 适宜的交联反应条件为：交联剂质量分数0.5%，175℃反应30 min；以聚乙二醇(PEG20000)为载体进一步优化了漆酶的固定化条件；2，4-二氯酚的降解实验表明，固定化漆酶中单位质量酶的降解能力要远远高于游离漆酶。
关键词：固定化；漆酶；交联聚乙二醇二丙烯酸酯
中图分类号：Q55；TS727+.1
文献标识码：A
文章编号：1000-6842（2009）03-0061-06
Synthesis of Cross-linked Polyethylene Glycol Diacrylates and Their Application as
Supports for Laccase Immobilization
ZHAO Min1,* MENG Qing-hui2 WANG Yan3
（1. College of Life Sciences, Northeast Forestry University, Harbin, Heilongjiang Province, 150040; 2. Department of Applied Chemistry, Harbin Institute of Technology, Harbin, Heilongjiang Province, 150001; 3. Sciences Research Center, Harbin Institute of Technology, Harbin, Heilongjiang Province, 150001）
（*E-mail: 82191513@163.com）
Abstract：Cross-linked polyethylene glycol diacrylates （PEGDA） were prepared with polyethylene glycols （PEG） of three different molecular weight （600, 6000 and 20000） as monomers, respectively. The products have three dimensional networks and high swelling capacity, and they were used as the carriers for the immobilization of laccase by physical adsorption. The influence of preparation conditions on the activities of immobilized enzyme were investigated and it was found that the cross-linked PEG（20000）DA showed the best immobilization effect for laccase. The proper conditions for cross-linking are as follows: cross-linking initiator concentration 0.5%, reaction temperature 175℃ and reaction time 30 min. The immobilization conditions were further optimized with PEG （20000） DA as the carrier. The degardation experiment of 2,4-dichlorophenol demonstrated that the degradation performance of the immobilized lacase was much higher than that of free lacase.
Key words：immobilization;laccase;cross-linked polyglycol diacrylate
（责任编辑：王 岩）
新型受阻胺类光返黄抑制剂的合成及在竹子化机浆中的应用
覃炳达 宋海农* 王双飞
(广西大学轻工与食品工程学院，广西南宁，530004）
摘 要：以己二胺哌啶（HMBTAD）为原料合成了新型受阻胺类光返黄抑制剂——己二胺哌啶氮氧自由基（HMB-TEMPO），详细研究了合成过程中的各种影响因素以及HMB-TEMPO在粉单竹BCTMP中的应用。最佳合成工艺条件为：以乙醇为溶剂，H2O2与HMBTAD摩尔比为4.0∶1，温度70℃，反应总时间10 h，其中H2O2滴漏时间3～4 h，催化剂Mg(OH)2用量为1.0%，产率达91%以上。与外购商品返黄抑制剂4-OH-TEMPO的对比实验表明，HMB-TEMPO具有较好的性质和返黄抑制效果，更适合竹子化机浆的光诱导返黄抑制。
关键词：竹子化机浆；光诱导返黄抑制剂；氮氧自由基；白度稳定性
中图分类号：TS727.2
文献标识码：A
文章编号：1000-6842（2009）03-0067-06
Synthesis of Novel Hindered Amine Photo-yellowing Inhibitor and Its Application in Bambusa Chungii BCTMP Pulp
QIN Bing-da SONG Hai-nong* WANG Shuang-fei
（College of Food and Biological Engineering, Guangxi University, Nanning, Guangxi Zhuang Autonomous Region, 530004）
（*E-mail: hnsong@gxu.edu.cn）
Abstract：In this paper, the controlling factors for the synthesis of the novel hindered amine photo-yellowing inhibitor N,N-bis （2,2,6,6 -tetramethyl-piperidinyloxy）-1,6-hexandiamine （HMB -TEMPO） by oxidizing N,N-bis（2,2,6,6 -tetramethyl -piperidinyl）-1,6- hexandiamine （HMBTAD） and its application in Bambusa Chungii （bamboo） BCTMP were studied. The optimal conditions of synthesis are as follows: ethanol as solvent, n（H2O2）∶n（HMBTAD）=4.0∶1; reaction temperature 70℃; totally reaction time 10 h, including 3～4 h of dropping time of H2O2， charge of Mg（OH）2 as catalyst 1.0%, the yield of the product is over 91%. The results showed that HMB-TEMPO has much better properties than 4-OH-TEMPO, and is more suitable for Bambusa Chungii BCTMP as light-induced yellowing inhibitor.
Key words：bamboo chemi-mechanical pulp;photo-yellowing inhibitor;nitroxides radical;brightness stability
（责任编辑：赵旸宇）
石油树脂作松香补充剂对松香胶性能及其施胶作用的影响
宋兆萍 刘温霞*
（山东轻工业学院制浆造纸科学与技术省部共建教育部重点实验室，山东济南，250353）
摘 要：利用未改性的C5和C9石油树脂直接与普通松香一起熔融制备阳离子分散松香胶。研究了其对胶料性能及松香施胶的影响，并通过XRD和XPS分析了其在松香施胶中的作用机理。结果表明，C5和C9石油树脂可降低阳离子分散松香胶中分子的短程有序性，抑制松香的结晶，并趋于分布在松香胶膜表面，提高阳离子分散松香胶的施胶性能，但需要调整乳化剂。含有20％C5石油树脂、10％C9石油树脂的阳离子分散松香胶在其加入量为0.8%~1.0%和硫酸铝用量为1.5%~2.0%的条件下，可获得好于普通阳离子分散松香胶的施胶效果。
关键词：阳离子分散松香胶；C5石油树脂；C9石油树脂；施胶
中图分类号：TS727+.5
文献标识码：A
文章编号：1000-6842（2009）03-0073-06
Function of Petroleum Resins in Rosin Sizing
SONG Zhao-ping LIU Wen-xia*
（Key Lab of Paper Science and Technology of Ministry of Education, Shandong Institute of Light Industry, Jinan, Shandong Province, 250353）
（*E-mail: liuwenxia@sdili.edu.cn）
Abstract：In this paper, unmodified C5 and C9 petroleum resins were directly melted together with natural rosin in preparing cationic rosin size emulsion. The effects of the petroleum resins on the stability and sizing performance of the cationic rosin size were investigated. By means of XRD and XPS, the function of the petroleum resins in rosin sizing was analyzed. The results showed that petroleum resins decrease the short-range-order domains of rosin size and reduce the carboxyl groups on the interface of rosin size and aqueous solution during emulsification. However, the introduction of petroleum resins can not enhance the emulsification ability of rosin sizes. Efficient sizing is developed when the cationic rosin size and aluminum sulfate are added at the dosage of 0.8%~1.0% and 1.5%~2.0%, respectively.
Key words：cationic dispersed rosin size;C5 petroleum resin;C9 petroleum resin;sizing
（责任编辑：孙秋菊）
封闭聚氨酯改性PAE纸张增湿强剂的研究
李刚辉 沈一丁 唐 新 赖小娟
(教育部轻化工助剂化学与技术重点实验室，陕西科技大学，陕西西安，710021)
摘 要：以咪唑为封闭剂制备出封闭聚氨酯（BPU），用BPU代替部分环氧氯丙烷(ECH)与聚酰胺多胺反应得到改性PAE纸张增湿强剂（MPAE）。研究了BPU封闭率、ECH添加量、助留剂及抄造系统pH值等因素对纸张性能的影响。结果表明，异氰酸酯基团比PAE分子中活性基团对提高纸张湿强性能更有效；w(ECH)为25.71%时，纸张湿抗张指数和湿强度保留率分别达到7.08 N·m/g和33.6%；助留剂CPAM可间接提高MPAE的留着率；抄造系统的中(弱)碱性有利于发挥增湿强剂的应用性能。
关键词：增湿强剂；咪唑封闭聚氨酯；聚酰胺多胺环氧氯丙烷；封闭率；助留剂
中图分类号：TS727+.2
文献标识码：A
文章编号：1000-6842（2009）03-0079-04
Study on Paper Wet Strength Agent of PAE Modified with Blocked Polyurethane
LI Gang-hui* SHEN Yi-ding TANG Xin LAI Xiao-juan
（Key Laboratory of Auxiliary Chemistry & Technology for Chemical Industry, Ministry of Education, Shaanxi University of Science & Technology, Xian, Shaanxi Province, 710021）
（*E-mail: ligh@sust.edu.cn）
Abstract：The paper wet strength agents of PAE modified with imidazole-blocked poly, urethane were prepared by the reaction of polyaminamide and epichlorohydrin （ECH） in BPU N-methyl pyrrolidone solution. The influence of the blocked ratio of BPU, the dosages of ECH, the charge and adding process of retention agent, and the pH value of pulp on the physical properties of the treated paper was studied. The results showed that isocyanate groups are more efficient than the active groups in the PAE molecular in increasing the wet tensile index of paper. When the dosage of ECH is 25.71%, the wet tensile index and the wet strength can reach as high as 7.08 N·m/g and 33.57% respectively. CPAM can indirectly increase the retention of MPAE. It is advantageous of pulp under neutral-weak alkaline condition to increase the application performance of the wet strength agents.
Key words：wet strength agent;imidazole-blocked polyurethane;polyaminamide epichlorohydrin;blocked ratio;retention agent
（责任编辑：关 颖）
CPAM对PCC悬浮液絮凝作用的分形研究
胡 芳1,2 胡惠仁3
（1.齐齐哈尔大学轻工纺织学院，黑龙江齐齐哈尔，161006； 2.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640； 3.天津科技大学材料科学与化学工程学院，天津， 300457）
摘 要：絮体具有分形结构特征，研究了造纸湿部常用助留剂——阳离子聚丙烯酰胺（CPAM）对沉淀碳酸钙（PCC）悬浮液的絮凝作用，应用图像分析法计算絮体的分维。CPAM能使PCC悬浮液中形成形状复杂的絮体，具有自相似性的分形特征。絮体的分维和沉淀后的上清液浊度之间表现出良好的相关性。CPAM形成絮体的分维在1.3062～1.6468范围内，且其与CPAM的用量、电荷密度及分子质量有关。对于研究中采用的3种CPAM，电荷密度较高的CPAM，形成絮体的分维较高；分子质量较大的CPAM形成的絮体分维相对较低。
关键词：CPAM；絮凝；絮体；分维
中图分类号：TS71+4
文献标识码：A
文章编号：1000-6842（2009）03-0083-05
Fractal Study on Flocculation of PCC Suspension Induced by CPAM
HU Fang1,2,* HU Hui-ren3
（1. College of Light Industry and Textile, Qiqihar University, Qiqihar, Heilongjiang Province, 161006; 2. State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640; 3. College of Material Science and Chemical Engineering, Tianjin University of Science & Technology, Tianjin, 300457）
（*E-mail: fangh16@163.com）
Abstract：The flocs have fractal structure. In this paper, the flocculation of PCC suspension induced by retention aid system CPAM was studied and the fractal dimension was calculated with image analysis technology. Retention aid system CPAM induced flocculation of PCC suspension and the flocs had the complex shape and self-similar structure. The results showed that fractal dimension had good relation to the turbidity of the supernatant. The fractal dimensions of flocs induced by CPAM were at the range of 1.3062～1.6468, depending on the dosage, charge density and molecular weight of CPAM. For three kinds of CPAM used in the experiment, CPAM with higher charge density formed the flcos with higher fractal dimension; CPAM with higher molecular weight formed the flocs with lower fractal dimension.
Key words：CPAM;flocculation;floc;fractal dimension
（责任编辑：田风洲）
歧化松香胺-木质素乳化剂的合成及其表面物化性能
刘祖广 刘 登 李美繁 朱华龙
（广西民族大学化学与生态工程学院，广西南宁，530006）
摘 要：通过Mannich反应，分别在硫酸盐木质素中引入了亲油性的歧化松香胺甲基和亲水性的二乙烯三胺甲基基团，合成了歧化松香胺-木质素复合阳离子乳化剂，并对目标产物进行了红外光谱、元素分析和基本表面物化性能的测试。实验结果表明，木质素经与歧化松香胺、二乙烯三胺和甲醛反应后，分别在木质素分子结构中引入了相应的胺甲基。经改性后的复合阳离子乳化剂在pH值为2.0的盐酸溶液中的最低表面张力可达26.6 mN/m，与未接枝歧化松香胺甲基的木质素胺的表面张力49.3 mN/m相比显著降低，其形成胶束的质量浓度约为5 g/L，HLB值为12，对标准油样的乳化能力及起泡性能均有所提高。
关键词：阳离子乳化剂；木质素；Mannich反应；歧化松香胺
中图分类号：TQ423.92
文献标识码：A
文章编号：1000-6842（2009）03-0088-05
Preparation of Disproportionated Rosin Amine-Lignin Composite Cationic Emulsifier
and Its Physico-chemical Properties
LIU Zu-guang* LIU Deng LI Mei-fan ZHU Hua-long
（College of Chemistry and Ecological Engineering, Guangxi University for Nationalities, Nanning, Guangxi Zhuang Autonomous Region, 530006）
（*E-mail: liuzug@sohu.com）
Abstract：The disproportionated rosin amine-lignin composite cationic emulsifier was prepared from disproportionated rosin amine, diethylenetriamine, formaldehyde and lignin by Mannich reaction. The physico-chemical properties of the resultant product were measured and its structure was characterized by elemental analysis and IR spectroscopy. The experiment results showed that disproportionated rosin amine methyl and diethylenetriamine methyl were introduced onto lignin respectively by Mannich reation. The value of the minimum surface tension of disproportionated rosin amine-lignin composite cationic emulsifier was 26.6 mN/m, critical micelle concentration was 5 g/L and HLB was 12. Its emulsifying power （with HLB=12 mixed oil of turpentine and soya bean oil） and foaming power were improved too.
Key words：cationic emulsifier;lignin;Mannich reaction;disproportionated rosin amine
（责任编辑：刘振华）
水滑石对造纸阴离子垃圾模拟物吸附性能的影响
杨冬梅1 宋湛谦2 钱学仁1，*
(1.东北林业大学生物质材料科学与技术教育部重点实验室，黑龙江哈尔滨，150040； 2.中国林业科学研究院林产化学工业研究所，国家林业局林产化学工程重点开放性实验室，江苏南京， 210042)
摘 要：以不同摩尔比的镁与铝制备了一系列水滑石，考察了其对造纸系统中阴离子垃圾模拟物如苯甲酸、苯酚和油酸的吸附性能。结果表明，对苯甲酸和苯酚的吸附，随着镁与铝摩尔比的增加，吸附量逐渐增大，对苯甲酸的吸附效果比苯酚好，两者的吸附等温线均符合Freundlich模型；对油酸的吸附率可达99%以上。
关键词：水滑石；镁铝摩尔比；吸附；阴离子垃圾
中图分类号：TS753.9
文献标识码：A
文章编号：1000-6842（2009）03-0093-04
Effect of the Mg/Al Molar Ratio of Hydrotalcite on the Adsorption Behavior
of Papermaking Anionic Trash Models
YANG Dong-mei1 SONG Zhan-qian2 QIAN Xue-ren1,*
（1. Key Laboratory of Bio-based Material Science and Technology of Ministry of Education, Northeast Forestry University, Harbin, Heilongjiang Province, 150040; 2.Institute of Chemical Industry of Forest Products, CAF; Key and Open Lab on Forest Chemical Engineering, SAF, Nanjing, Jiangsu Province, 210042）
（*E-mail: qianxueren@yahoo.com.cn）
Abstract：Mg-Al hydrotalcites with different Mg/Al molar ratios were prepared, the adsorption experiments were carried out using benzoic acid, phenol, D-glucuronic acid and oleic acid as mimic anionic trash in papermaking furnish. The results indicated that the amounts of the benzoic acid and phenol adsorbed by LDH increase with increasing Mg/Al molar ratio. In general, benzoic acid adsorption on the LDH is better than phenol. The adsorption isotherms of both benzoic acid and phenol are in agreement with the Freundlich model. The absorption of D-glucuronic acid in the range of low concentration is more effective than in high concentration. The optimized LDH are capable of removing oleic acid by 99%.
Key words：hydrotalcite;Mg/Al molar ratio;adsorption;anionic trash
（责任编辑：马 忻）
脂肪酶处理TMP白水中树脂类物质
胡惠仁1 王松林2
（1.天津科技大学天津市制浆造纸重点实验室，天津，300457； 2.青岛科技大学化工学院，山东青岛，266042）
摘 要：热磨机械浆（TMP）造纸循环白水的溶解和胶体物质（DCS）中含有较多的树脂类物质，在造纸过程中会以多种形式沉积在设备表面，造成停机和纸质下降等树脂障碍问题。通过脂肪酶处理TMP模拟白水，利用甘油铜比色法和GC-MS分析等方法分析树脂类物质的降解情况。结果表明，经脂肪酶处理后DCS的阳离子需求量(CD值)减少20%左右。GC-MS分析脂肪酶处理后产物检测出脂肪酸和醇类物质，表明脂肪酶对树脂类物质具有明显的降解作用。
关键词：热磨机械浆（TMP）；造纸白水；溶解和胶体物质（DCS）；树脂；脂肪酶
中图分类号：TS743+.3；TS743+.14
文献标识码：A
文章编号：1000-6842（2009）03-0097-05
Lipase Treatment of Pitch in Papermaking with TMP as Main Furnish
HU Hui-ren1,* WANG Song-lin2
（1. Tianjin Key Lab of Pulp and Paper, Tianjin University of Science & Technology，Tianjin, 300457； 2. College of Chemical Engineening, Qingdao University of Science & Technology, Qingdao, Shandong Province, 266042）
（*E-mail: huiren@tust.edu.cn）
Abstract：The dissolved and colloidal substances（DCS）in papermaking with TMP as main furnish contain certain amount of pitch species which can deposite on the surface of equipment,cause papermachine shut down and the quality of paper product decrease.Experiment results showed that treating the simulated white water with lipase could reduce the cationic demand by 20%.Cupric-glycerinate-colorimetric method and GC-MS were used for the analysis of degraded components caused by lipase treatment. Fat acid and alcohol species were identified by GC-MS analysis,which indicated that pitch species could be decomposed by lipase.
Key words：thermo-mechanical pulp（TMP）；papermaking white water；dissolved and colloidal substances（DCS）；pitch;lipase
（责任编辑：梁 川）
桉木CTMP制浆废液水质特征及色度特性分析
胡志军
（浙江科技学院，浙江杭州，310023）
摘 要：采用不同工艺及设备模拟CTMP工艺，得到了桉木CTMP废液。探讨了不同工艺条件下废液的水质参数、可生化性、污染物质、分子质量及色度等。研究结果表明，桉木CTMP制浆废液污染负荷高，可生化性一般，色度深且随pH值升高显著加深。木素衍生物和多酚类物质的酚羟基的离子化及与金属离子的络合是废液色度深的主要原因。相对分子质量大于10000的有机组分是色度的主要构成。混合制浆时，桉木比例越大，色度越深，COD负荷相对较小；预处理段和磨浆段污染负荷表现出与全桉木相反的情况，可能原因是混合磨浆过程中两者的溶出物发生进一步反应，有利于更多物质的溶出。
关键词： 桉木；CTMP；废液；色度
中图分类号：X793
文献标识码：A
文章编号：1000-6842（2009）03-0102-04
The Study on Pollution and Chromaticity Characteristics of Eucalyptus CTMP Effluent
HU Zhi-jun
（Zhejiang Institute of Science and Technology, Hangzhou, Zhejiang Province, 310023）
（E-mail: foxhuz@163.com）
Abstract：The eucalyptus CTMP effluent was prepared by simulating CTMP pulping technology in different laboratory conditions. The waste water quality parameters, biodegradability, pollutants, the molecular mass characteristics of organic pollutants, chromaticity characteristics of the effluent and so on were investigated. The results showed that the pollution load of effluent was high, the biodegradability was moderate, and the chromaticity was dark and increased significantly with the pH value. The main reasons of dark chromaticity were the ionization of polyphenols hydroxyl and its metal complexes of lignin derivatives and polyphenols in the effluent. The main source of the chromaticity was the organic components with molecular weight higher than 10000. When the mixed woods raw material was used, the greater the proportion of eucalyptus wood was, the darker chromaticity was, and COD load was relatively low. The pollution loads of refining stage and pretreatment stage showed complete difference between eucalyptus and the mixed masson pine and eucalyptus. The reason probably was due to the further reaction of the dissolved materials from mixed raw material refining process, and it was favorable to more organic material dissolve.
Key words：eucalyptus wood;CTMP;effluent;chromaticity
（责任编辑：赵旸宇）
麦草烧碱法制浆污染物核算方法初探
范景阳 曹春昱 冯文英 苏振华 徐 明 郑燕生 丁建平
（中国制浆造纸研究院，北京，100020）
摘 要：研究了制浆工艺参数和原料降解程度对黑液有机物发生量的影响，探讨了利用工艺参数和原料不同组分进行CODCr、BOD5产污系数核算的可行性，并进行了核算方法实用性的验证。结果表明，根据工艺参数和原料不同组分溶出程度测算烧碱法蒸煮污染物负荷是可行的，但某些相关性不高的核算途径还有待于进一步应用验证。
关键词：黑液有机物；原料成分溶出率；CODCr；BOD5；产污系数核算
中图分类号：TS749+.2；TS77
文献标识码：A
文章编号：1000-6842（2009）03-0106-06
Preliminary Study on the Methods for Accounting the Pollutants Derived from Wheat Straw Soda Pulping
FAN Jing-yang* CAO Chun-yu FENG Wen-ying SU Zheng-hua XU Ming ZHENG Yan-sheng DING Jian-ping
（China National Pulp and Paper Research Institute, Beijing, 100020）
（*E-mail: jygansy@sina.com）
Abstract：This paper introduced several methods to account the production coefficients of CODCr, BOD5 in the pulp mills where wheat straw soda pulping process was applied. The influence of pulping parameters and degradation degree of raw material on the organic material content produced in black liquor was investigated, and the relations among the loads of CODCr, BOD5 in black liquid, process parameters and degradation rate of raw materials were explored. These methods have been proved by some applications, but further more tests and verifications in more mills are necessary.
Key words：organic in black liquid;raw material degradation rate;CODCr;BOD5;creation factor
（责任编辑：田风洲）
接枝改性木质素磺酸钙的制备及应用
贾陆军1 王海滨2 霍冀川1，* 吕淑珍1 雷永林1 刘树信2
(1.西南科技大学应用化学研究所，四川绵阳，621010；2.绵阳师范学院，四川绵阳，621000)
摘 要：以H2O2-Fe2+为引发剂，通过自由基溶液共聚反应，在木质素磺酸钙表面接枝丙烯酸、马来酸酐等单体，合成了接枝改性木质素磺酸盐减水剂，并用红外光谱法测定了木质素磺酸钙及其改性产物的结构特征参数；研究了改性木质素磺酸盐减水剂对水泥净浆流动度、凝结时间、抗压强度和减水率的影响，并进行了对比实验。结果表明：改性木质素磺酸钙具有较好的减水性能，减水率可达22.26%，水泥净浆7 d、28 d的抗压强度分别可达空白实验的110％和113％。
关键词：木质素磺酸盐；接枝共聚；减水剂
中图分类号：TQ351.01+3
文献标识码：A
文章编号：1000-6842（2009）03-0112-04
Preparation and Application of Grafted Calcium Lignosulfonate Superplasticizer
JIA Lu-jun1 WANG Hai-bin2 HUO Ji-chuan1,* LV Shu-zhen1 LEI Yong-lin1 LIU Shu-xin2
（1. Institute of Applied Chemistry, Southwest University of Science and Technology, Mianyang, Sichuan Province, 621010; 2. Mianyang Normal University, Mianyang, Sichuan Province, 621000）
（*E-mail: huojichuan@swust.edu.cn）
Abstract：Grafted calcium lignosulfonate superplasticizer （GCL） was prepared by grafting the monomers of Crylic Acid and Maleic Anhydride onto the surface of calcium lignosulfonate using H2O2-Fe2+ as initiator through the free radical solution copolymerization reaction. The molecular structure of calcium lignosulfonate and its modified products were characterized by FT-IR; and the influence of the grafted calcium lignosulfonate superplasticizer on the fluidity, consolidating time, compressive strength and water reducing rate of net cement slurry was studied and a comparative experiment was carried out. The results showed that the Grafted calcium lignosulfonate superplasticizer has a better water-reducing performance and water-reducing ratio reaches 22.26%,it is comparable with the high grade concrete water reducing agent, the compressive strength of 7 days and 28 days of net cement slurry can achieve 110％ and 113％ compared with the blank test value of net cement slurry.
Key words：lignosulfonate;graft copolymerization;water-reducer
（责任编辑：关 颖）
基于振动信号的打浆质量NPLS软测量模型
宋乃建1 沈文浩2 朱小林2 刘焕彬2
（1.渭南师范学院化学化工系，陕西渭南，714000； 2.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640）
摘 要：总结了盘磨机振动信号的研究成果，提出了振动信号的分析方法，建立了基于盘磨机振动信号和比能的打浆质量NPLS软测量模型。结果表明，用该NPLS模型
对打浆度和湿重进行预测，预测值与实测值的相关系数为86%。
关键字：打浆质量；振动信号；多维偏最小二乘法模型
中图分类号：TS752
文献标识码：A
文章编号：1000-6842（2009）03-0116-05
The NPLS Soft Measuring Model of Refining Quality Based on the Vibration Signal of Pulp Refiner
SONG Nai-jian1,* SHEN Wen-hao2 ZHU Xiao-lin2 LIU Huan-bin2
（1. Department of Chemistry and Chemical Engineering, Weinan Teacher University, Weinan, Shaanxi Province, 714000; 2. State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640）
（*E-mail: hzggs@163.com）
Abstract：The research findings about vibration signal of pulp refiner were summarized, and the digital signal process of vibration signal was proposed. Based on those, the N-way Partial Least Square model of pulp quality was established. The results indicated that this NPLS model can describe 86% variation of pulp quality during refining.
Key words：pulp refining quality;vibration signal;N-way Partial Least Square Model
（责任编辑：梁 川）
油液分析技术及其在现代造纸机械故障诊断中的应用
邱荣华1,2 张 辉1,2,* 张笑如3
（1.南京林业大学江苏省制浆造纸科学与技术重点实验室，江苏南京，210037； 2.华南理工大学制浆造纸工程国家重点实验室，广东广州，510640； 3.亚洲浆纸金东纸业（江苏）有限公司，江苏镇江，212132)
摘 要：介绍了国内外油液分析技术研究与应用进展，对比分析了几种油液分析方法，进一步提出将油液分析技术应用到现代造纸机械日常在线维护、状态监测与故障诊断中的必要性、潜在价值、基本思路和前景，以促进我国造纸工业加快适应和提高应用现代化装备的技术水平。
关键词：造纸机械；油液分析技术；状态监测；故障诊断；预知性维护
中图分类号：TS734+.1；TH165+.3；TH117；TP206+.3
文献标识码：A
文章编号：1000-6842（2009）03-0121-06
Oil Analysis Technique and Its Application in Modern Papermaking Machinery Fault Diagnosis
QIU Rong-hua1,2 ZHANG Hui1,2,* ZHANG Xiao-ru3
（1. Jiangsu Provincial Key Lab of Pulp and Paper Science and Technology, Nanjing Forestry University, Nanjing, Jiangsu Province, 210037; 2. State Key Lab of Pulp and Paper Engineering, South China University of Technology, Guangzhou, Guangdong Province, 510640; 3. Gold East Paper （Jiangsu） Co., Ltd. of APP, Zhenjiang, Jiangsu Province, 212132）
（*E-mail: zhnjfu@njfu.com.cn）
Abstract：Oil analysis technique research and application progress both in China and abroad were introduced and several oil analysis methods were analyzed and compared with each other. The necessity, potential value, basic idea and prospect of oil analysis technique application in daily on-line maintenance, condition monitoring and fault diagnosis of modern papermaking machinery were further discussed. The paper will be of benefit to promote Chinas papermaking industry to adapt and improve the technical level of using modern paper machines.
Key words：papermaking machinery;oil analysis technique;condition monitoring;fault diagnosis;predictive maintenance
（责任编辑：关 颖）
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