纳米纤维素的形貌及快速表征方法的比较
Comparison of Morphology and Fast Characterization Methods of Nanocellulose
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摘要: 以商品南方松溶解浆、漂白桉木浆为原料,采用硫酸水解法、纤维素酶预处理法、2,2,6,6-四甲基哌啶氧自由基(TEMPO)氧化法以及机械法分别制备了纳米纤维素,利用透射电镜(TEM)、原子力显微镜(AFM)详细表征了不同方法制备的纳米微晶纤维素(CNC)和纳米纤丝纤维素(CNF).采用了多种商品粒度仪快速定性表征了纳米纤维素的大小,CNC为棒状纳米晶须结构,直径约为20 nm,长度为10~200 nm;CNF一般为网状结构,尺寸较大且分布较宽,单根CNF直径从几纳米到几百纳米不等.依据离心分离以及布朗运动制备的2种仪器非常适合半定量快速表征非网状结构的纳米微晶纤维素,实验重复性也很好.Abstract: In this study, nanocellulose was prepared by acid hydrolysis, cellulase enzyme pretreatment, TEMPO oxidation and mechanical fibrillation techniques using commercial southern pine dissolving pulp and bleached eucalyptus pulp as raw materials, respectively. This study intended to provide relatively complete morphological pictures of several kinds of wood nanocellulose including cellulose nanocrystals (CNC) and cellulose nanofibrils (CNF) produced by most commonly used processes. TEM and AFM were applied to provide visual examinations of several nanocellulose samples. Commercial particle sizing instruments were evaluated for quick particle sizing the samples. It was found that CNC were mainly rodlike nano-whiskers with diameter of approximately 20 nm and length ranging from 10 to 200 nm as expected, and CNF were fibril network particles with a diameter ranging from several nanometers to several hundred nanometers, respectively. The instruments based on the centrifuge and a Brownian motion showed good repeatability in particle sizing. Both instruments were well suited to semi-quantitative characterize non network particles even with large aspect ratios such as CNC, but further study is required before they can be used for characterizing network particles such as CNF.