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草酸水解制备纤维素纳米纤丝工艺条件的优化
Optimization of Process Conditions for Preparing Nanocellulose Crystals by Oxalic Acid Hydrolysis
  
DOI:10.11980/j.issn.0254-508X.2019.01.004
关键词:  草酸  纤维素纳米纤丝  响应面  最佳工艺
Key Words:oxalic acid  nanocellulose crystal  response surface method  optimum process
基金项目:国家自然科学基金项目(No.31570569);广东省基金博士启动纵向协同创新项目(No.2017A030310341);制浆造纸工程国家重点实验室项目(No.2017QN01)。
作者单位
李兵云 华南理工大学制浆造纸工程国家重点实验室广东广州510640 
耿青杰 华南理工大学制浆造纸工程国家重点实验室广东广州510640 
王冉冉 华南理工大学制浆造纸工程国家重点实验室广东广州510640 
付时雨* 华南理工大学制浆造纸工程国家重点实验室广东广州510640 
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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。
Abstract: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.
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