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Preparation of water-soluble cellulose derivatives using TEMPO radical-mediated oxidation at extended reaction time
Reactive & Functional Polymers ( IF 5.1 ) Pub Date : 2020-10-24 , DOI: 10.1016/j.reactfunctpolym.2020.104768
Raluca Ioana Baron , Sergiu Coseri

Four types of cellulosic samples, including cotton linters, microcrystalline, never-dried sulfite pulp, and viscose, were tested as potential sources to prepare cellulose-based derivatives, able to be used in homogeneous systems. In this way, by employing water as a solvent, can surpass one of the major drawbacks of native cellulose, its recalcitrance towards common solvents. The chosen derivatization procedure implies the chemical oxidation using 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) radical, sodium hypochlorite, and sodium bromide. Following this treatment, each cellulose sample was processed in such a way as to maximize the content of water-soluble fractions. Therefore, for each cellulose type (except viscose), we could isolate three oxidized samples All of these samples were thoroughly characterized using spectral analyses (FT-IR, 1H NMR, 13C NMR), content of negatively charged groups, and degree of polymerization. The morphology of the oxidized products has been evaluated by means of scanning electron microscopy (SEM), and crystallinity was assessed by using X-ray diffraction (XRD). The thermal analyses for the pure and oxidized cellulose samples were also performed. The limit of the solubility in water for the oxidized fractions was checked by using a low-voltage electron microscopy (LVEM).



中文翻译:

用TEMPO自由基介导的氧化反应在延长的反应时间制备水溶性纤维素衍生物

测试了四种类型的纤维素样品,包括棉短绒,微晶纤维,从未干燥的亚硫酸盐浆和粘胶纤维,作为制备纤维素基衍生物的潜在来源,可用于均质系统。这样,通过使用水作为溶剂,可以克服天然纤维素的主要缺点之一,即它对普通溶剂的顽固性。选择的衍生化程序意味着使用2,2,6,6-四甲基哌啶-1-氧基(TEMPO)基,次氯酸钠和溴化钠进行化学氧化。在该处理之后,以使水溶性级分的含量最大的方式处理每个纤维素样品。因此,对于每种纤维素类型(粘胶纤维除外),我们可以分离出三个氧化的样品。所有这些样品均使用光谱分析(FT-IR,1 H NMR,13 C NMR),带负电基团的含量和聚合度。通过扫描电子显微镜(SEM)评估了氧化产物的形态,并通过X射线衍射(XRD)评估了结晶度。还对纯的和氧化的纤维素样品进行了热分析。氧化级分在水中的溶解度极限是通过使用低压电子显微镜(LVEM)检查的。

更新日期:2020-11-04
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