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Preparation and characterization of water-redispersible nanofibrillated cellulose in powder form

机译:粉末状水分散性纳米原纤化纤维素的制备与表征

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Water-redispersible, nanofibrillated cellulose (NFC) in powder form was prepared from refined, bleached beech pulp (RBP) by carboxymethylation (c) and mechanical disintegration (m). Two routes were examined by altering the sequence of the chemical and mechanical treatment, leading to four different products: RBP-m and RBP-mc (route 1), and RBP-c and RBP-cm (route 2). The occurrence of the carboxymethylation reaction was confirmed by FT-IR spectrometry and C-13 solid state NMR (C-13 CP-MAS) spectroscopy with the appearance of characteristic signals for the carboxylate group at 1,595 cm(-1) and 180 ppm, respectively. The chemical modification reduced the crystallinity of the products, especially for those of route 2, as shown by XRD experiments. Also, TGA showed a decrease in the thermal stability of the carboxymethylated products. However, sedimentation tests revealed that carboxymethylation was critical to obtain water-redispersible powders: the products of route 2 were easier to redisperse in water and their aqueous suspensions were more stable and transparent than those from route 1. SEM images of freeze-dried suspensions from redispersed RBP powders confirmed that carboxymethylation prevented irreversible agglomeration of cellulose fibrils during drying. These results suggest that carboxymethylated and mechanically disintegrated RBP in dry form is a very attractive alternative to conventional NFC aqueous suspensions as starting material for derivatization and compounding with (bio)polymers.
机译:通过羧甲基化(c)和机械崩解(m)由精制的漂白山毛榉浆(RBP)制备粉末状的水可再分散的纳米原纤化纤维素(NFC)。通过更改化学和机械处理的顺序检查了两条路线,得出了四种不同的产品:RBP-m和RBP-mc(路线1)以及RBP-c和RBP-cm(路线2)。通过FT-IR光谱和C-13固态NMR(C-13 CP-MAS)光谱确认了羧甲基化反应的发生,并且在1,595 cm(-1)和180 ppm处出现了羧酸根基团的特征信号,分别。如XRD实验所示,化学改性降低了产品的结晶度,尤其是对于路线2的产品。另外,TGA显示出羧甲基化产物的热稳定性降低。然而,沉降测试表明,羧甲基化对于获得水可再分散的粉末至关重要:与方法1相比,方法2的产品更易于在水中重新分散,其水悬浮液更稳定,更透明。再分散的RBP粉末证实,羧甲基化可防止干燥过程中纤维素原纤维不可逆的团聚。这些结果表明,干燥形式的羧甲基化和机械崩解的RBP是常规NFC水性悬浮液的一种非常诱人的替代品,它是用于衍生化和与(生物)聚合物混合的原料。

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