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基于几丁质的聚氨酯弹性体的X射线衍射研究。

XRD studies of chitin-based polyurethane elastomers.

作者信息

Zia Khalid Mahmood, Bhatti Ijaz Ahmad, Barikani Mehdi, Zuber Mohammad, Sheikh Munir Ahmad

机构信息

Department of Chemistry, University of Agriculture, Faisalabad 38040, Pakistan.

出版信息

Int J Biol Macromol. 2008 Aug 15;43(2):136-41. doi: 10.1016/j.ijbiomac.2008.04.009. Epub 2008 Apr 16.

Abstract

Chitin-based polyurethane elastomers (PUEs) were synthesized by step growth polymerization techniques using poly(epsilon-caprolactone) (PCL) varying diisocyanate and chain extender structures. The viscosity average molecular weight (M(v)) of chitin was deduced from the intrinsic viscosity and found; M(v)=6.067 x 10(5). The conventional spectroscopic characterization of the samples with FTIR, (1)H NMR and (13)C NMR were in accordance with proposed PUEs structure. The crystalline behavior of the synthesized polymers were investigated by X-ray diffraction (XRD), differential scanning calorimetery (DSC) and loss tangent curves (tan delta peaks). The observed patterns of the crystalline peaks for the lower angle for chitin in the 2theta range were indexed as 9.39 degrees, 19.72 degrees, 20.73 degrees, 23.41 degrees and 26.39 degrees. Results showed that crystallinity of the synthesized PUEs samples was affected by varying the structure of the diisocyanate and chain extender. Crystallinity decreased from aliphatic to aromatic characters of the diisocyanates used in the final PU. The presence of chitin also favors the formation of more ordered structure, as higher peak intensities was obtained from the PU extended with chitin than 1,4-butane diol (BDO). The value of peak enthalpy (DeltaH) of chitin was found to be 47.13 J g(-1). The higher DeltaH value of 46.35 J g(-1) was found in the samples extended with chitin than BDO (39.73 J g(-1)).

摘要

基于几丁质的聚氨酯弹性体(PUEs)通过逐步增长聚合技术合成,使用了具有不同二异氰酸酯和扩链剂结构的聚(ε-己内酯)(PCL)。从特性粘度推导出几丁质的粘均分子量(M(v)),结果为:M(v)=6.067×10⁵。通过傅里叶变换红外光谱(FTIR)、¹H核磁共振(¹H NMR)和¹³C核磁共振(¹³C NMR)对样品进行的常规光谱表征与所提出的PUEs结构一致。通过X射线衍射(XRD)、差示扫描量热法(DSC)和损耗角正切曲线(tanδ峰)研究了合成聚合物的结晶行为。在2θ范围内几丁质较低角度处观察到的结晶峰模式的索引角度为9.39°、19.72°、20.73°、23.41°和26.39°。结果表明,合成的PUEs样品的结晶度受二异氰酸酯和扩链剂结构变化的影响。在最终聚氨酯中使用的二异氰酸酯从脂肪族到芳香族特性,结晶度降低。几丁质的存在也有利于形成更有序的结构,因为用几丁质扩链的聚氨酯比用1,4-丁二醇(BDO)扩链的聚氨酯获得更高的峰强度。发现几丁质的峰焓(ΔH)值为47.13 J g⁻¹。在用几丁质扩链的样品中发现的较高ΔH值为46.35 J g⁻¹,而用BDO扩链的样品为39.73 J g⁻¹。

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