Synthesis of acyl chitin derivatives and miscibility characterization of their blends with poly(ε-caprolactone)

Synthesis of acyl chitin derivatives and miscibility characterization of their blends with poly(ε-caprolactone)
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DOI:
10.1016/j.carbpol.2009.10.014
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发表时间:
2010-03-17
影响因子:
11.2
通讯作者:
Nishio, Yoshiyuki
Nishio, Yoshiyuki
中科院分区:
化学1区
文献类型:
--
作者:
Sugimoto, Masao;Kawahara, Mariko;Nishio, Yoshiyuki

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以蟹壳甲壳素为原料,在N,N-二甲基乙酰胺-LiCl溶液中,与不同的酰氯反应,合成了侧链碳数为2-6的具有不同取代度的甲壳素衍生物。NMR分析定量地证明了不仅C3/C6羟基质子的酰化,而且C2氨基质子的酰化。采用差示扫描量热法对酰基甲壳素与聚己内酯(PCL)共混物的溶液浇铸膜进行了表征。共混聚合物对达到相容性所需的临界总取代度随N的增加而降低。随着酯基取代度的增加,增溶程度明显提高,但与酰胺基取代度的相关性较小。与纤维素酯/PCL共混物系统类似,与PCL的重复单元一起考虑的几丁质组分的酯侧基的结构亲和力可能是实现可溶解性的关键因素。(C)2009爱思唯尔有限公司保留所有权利。
Chitin derivatives having a normal acyl group (side-chain carbon number, N = 2-6) at different degrees of substitution (DS) were synthesized by a homogenous reaction of crab-shell chitin with various acyl chlorides in N,N-dimethylacetamide-LiCl solution. NMR analysis quantitatively demonstrated the acylations not only for C3/C6 hydroxy protons but also for C2 amino proton(s). Solution cast blend films of the acyl chitin products with poly(epsilon-caprolactone) (PCL) were provided for the miscibility characterization by differential scanning calorimetry. The critical total-DS required for attaining a miscibility of the blending polymer pair decreased with an increase in N. The degree of miscibility was enhanced definitely with an increase in ester-DS, but it made less correlation with amide-DS. In analogy with cellulose ester/PCL blend systems, a structural affinity of the ester side-group of the chitinous component considered with a repeating unit of PCL may be a crucial factor for the miscibility attainment. (C) 2009 Elsevier Ltd. All rights reserved.