草酸水解制备纤维素纳米纤丝工艺条件的优化
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摘要
运用响应面法对草酸水解制备纤维素纳米纤丝的条件进行设计实验,并运用Design-Export软件对影响纤维素纳米纤丝尺寸的3个重要因素即反应温度、草酸质量分数以及反应时间进行实验设计。通过软件优化得到编码方程,得出最佳反应工艺条件为:反应温度112℃,草酸质量分数36%,反应时间2. 5 h;在最佳工艺条件下得到的纤维素纳米纤丝的结晶度为65%,长度为1～1000 nm纤维素纳米纤丝含量为91. 6%,与预测值91. 4%相符合,表明编码方程合理有效。
The response surface method was used to design the conditions for preparing nanocellulose crystals by oxalic acid hydrolysis and three important affecting factors oxalic acid mass fraction,reaction temperature and time were designed by Design-Export software. The codinge quation was obtained by software optimization,the optimal reaction conditions were as follows: reaction temperature was 112℃,oxalic acid concentration was 36%,reaction time was 2. 5 h,the homogenization time was 50 min,the crystallinity of nanocellulose obtained under the optimal process condition in the experiment was 65%,and nanocellulose crystals accounted for 91. 6% of the yield of nanocellulose products,which was consistent with the predicted value of 91. 4%. The results indicated that the coding equation was reasonable and effective.
The response surface method was used to design the conditions for preparing nanocellulose crystals by oxalic acid hydrolysis and three important affecting factors oxalic acid mass fraction,reaction temperature and time were designed by Design-Export software. The codinge quation was obtained by software optimization,the optimal reaction conditions were as follows: reaction temperature was 112℃,oxalic acid concentration was 36%,reaction time was 2. 5 h,the homogenization time was 50 min,the crystallinity of nanocellulose obtained under the optimal process condition in the experiment was 65%,and nanocellulose crystals accounted for 91. 6% of the yield of nanocellulose products,which was consistent with the predicted value of 91. 4%. The results indicated that the coding equation was reasonable and effective.
引文
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[2]Beck-Candedo S,Roman M,Gray D G.Effect of Reaction Conditions on the Properties and Behavior of Wood Cellulose Nanocrystal Suspensions[J].Biomacromolecules,2005,6(2):1048.
[3]Lin N,Dufresne A.Nanocellulose in Biomedicine:Current Status and Future Prospect[J].European Polymer Journal,2014,59:302.
[4]Chirayil C J,Mathew L,Thomas S.Review of Recent Research in Nano Cellulose Preparation from Different Lignocellulosic Fibers[J].Reviews on Advanced Materials Science,2014,37(1):20.
[5]Siqueira G,Bras J,Dufresne A.Cellulosic Bionanocomposites:AReview of Preparation,Properties And Applications[J].Polymers,2010,2(4):728.
[6]Dong Fengxia,LIU Wen,LIU Hongfeng.Preparation and Application of Nanocellulose[J].China Pulp&Paper,2012,31(6):68.董凤霞,刘文,刘红峰.纳米纤维素的制备及应用[J].中国造纸,2012,31(6):68.
[7]Wang Fumin,Li Qun,Wang Aijiao,et al.Preparation and Application of TEMPO Oxidized Cellulose Nanofibers[J].Tianjin Paper,2017(1):31.王福敏,李群,王爱姣,等.TEMPO氧化纤维素纳米纤维的制备及应用[J].天津造纸,2017(1):31.
[8]Iwamoto S,Nakagaito A N,Yano H,et al.Optically Transparent Composites Reinforced with Plant Fiber-Based Nanofibers[J].Applied Physics A,2005,81(6):1109.
[9]Yamanaka S,Watanabe K,Kitamura N,et al.The Structure and Mechanical Properties of Sheets Prepared from Bacterial Cellulose[J].Journal of Materials Science,1989,24(9):3141.
[10]Tang L R,Ou Wen,Lin W Y,et al.Optimization of Acid Hydrolysis Processing of Nanocellulose Crystal Using Response Surface Methodology[J].Chemistry&Industry of Forest Products,2011,31(6):61.唐丽荣,欧文,林雯怡,等.酸水解制备纳米纤维素工艺条件的响应面优化[J].林产化学与工业,2011,31(6):61.
[11]Chen Liheng.Study on the hydrolysis of lignocellulosic enzymes based on acid treatment and the properties of nanocellulose[D].Guangzhou:South China University of Technology,2016.陈理恒.基于酸处理的木质纤维酶水解及纳米纤维素特性的研究[D].广州:华南理工大学,2016.
[12]Hu H X,Qiu K Q.The Imaging Information Implied in The Graph of Particles Size Distribution[J].Physical Testing&Chemical Analysis,2006,42(2):72.胡汉祥,丘克强.激光粒度分析结果在形貌分析中的应用[J].物化检验(物理分册),2006,42(2):72.
[13]Wang Jie,Hu Yunchu,Xu Chenhao,et al.Controllable preparation and characterization of nanocellulose size and morphology[J].Journal of Central South University of Forestry and Technology,2015,35(5):133.王洁,胡云楚,徐晨浩,等.纳米纤维素尺寸和形态的可控制备与表征[J].中南林业科技大学学报,2015,35(5):133.
[14]Dai Dasong.Preparation,Characterization and Application of Cannabis Nanocellulose[D].Fuzhou:Fujian Agriculture and Forestry University,2011.戴达松.大麻纳米纤维素的制备,表征及应用研究[D].福州:福建农林大学,2011.
[15]Yuwawech K,Wootthikanokkhan J,Wanwong S,et al.Polyurethane/Esterified Cellulose Nanocrystal Composites as a Transparent Moisture Barrier Coating for Encapsulation of Dye Sensitized Solar Cells[J].Journal of Applied Polymer Science,2017,134(45):45010.
[16]Liu Xiao,Dong Haizhou,Hou Hanxue.Preparation and Characterization of Peanut Shell Nanocellulose[J].Modern Food Science&Technology,2015(3):172.刘潇,董海洲,侯汉学.花生壳纳米纤维素的制备与表征[J].现代食品科技,2015(3):172.
[17]Xu X,Liu F,Jiang L,et al.Cellulose Nanocrystals Vs.Cellulose Nanofibrils:A Comparative Study on Their Microstructures and Effects as Polymer Reinforcing Agents[J].ACS Applied Materials&Interfaces,2013,5(8):2999.
[18]Yu H Y,Zhang H,Song M L,et al.From Cellulose Nanospheres,Nanorods to Nanofibers:Various Aspect Ratio Induced Nucleation/Reinforcing Effects on Polylactic Acid for Robust-Barrier Food Packaging[J].ACS Applied Materials&Interfaces,2017,9(50):43920.