改性过硫酸铵氧化法高效制备羧基化纤维素纳米晶体。
Modified ammonium persulfate oxidations for efficient preparation of carboxylated cellulose nanocrystals.
机构信息
Key Laboratory of Rubber-Plastics, Ministry of Education/Shandong Provincial, Key Laboratory of Rubber-plastics, Qingdao University of Science & Technology, Qingdao 266042, China.
Key Laboratory of Rubber-Plastics, Ministry of Education/Shandong Provincial, Key Laboratory of Rubber-plastics, Qingdao University of Science & Technology, Qingdao 266042, China; State Key Laboratory of Polymer Materials Engineering, Sichuan University, Chengdu 610065, China.
出版信息
Carbohydr Polym. 2020 Feb 1;229:115572. doi: 10.1016/j.carbpol.2019.115572. Epub 2019 Nov 10.
Ammonium persulfate (APS) was able to produce carboxylated cellulose nanocrystals (CNCs-COOH) directly from the raw materials of cellulose. However, the industrial production of CNCs-COOH by this method is obstructed by the lower preparation efficiency. Herein, by the activation via N,N,N',N'-tetramethylethylenediamine (TMEDA) and ultrasonic assisted disintegration, modified APS method to extract CNCs-COOH from pulp was presented. A high yield (up to 62.5 %), low usage of APS (8.5 g APS per gram pulp) and less reaction time (6 h) was achieved. The as-prepared CNCs-COOH exhibited high carboxyl group content (1.45 mmol/g) and high crystallinity index of 93 %. The reaction mechanism has been studied, and the results show that with the addition of TMEDA, SOcan be converted to free radicals and hydrogen peroxide more quickly. Our studies suggested that modified APS method may be a suitable and economic alternative for the preparation of CNCs-COOH.
过硫酸铵（APS）能够直接从纤维素原料生产羧基化纤维素纳米晶体（CNC-COOH）。然而，由于较低的制备效率，该方法在工业上制备 CNC-COOH 受到阻碍。在此，通过 N,N,N',N'-四甲基乙二胺（TMEDA）的活化和超声辅助崩解，提出了一种从纸浆中提取 CNC-COOH 的改良 APS 方法。该方法的产率较高（高达 62.5%），APS 的用量较低（每克纸浆 8.5 g APS），反应时间较短（6 h）。所制备的 CNC-COOH 具有较高的羧基含量（1.45 mmol/g）和较高的结晶度指数（93%）。研究了反应机制，结果表明，加入 TMEDA 后，SO 可以更快地转化为自由基和过氧化氢。我们的研究表明，改良 APS 法可能是一种合适且经济的替代方法，用于制备 CNC-COOH。
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