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Rapid characterization of high-impact ethylene–propylene copolymer composition by crystallization extraction separation: comparability to standard separation methods
International Journal of Polymer Analysis and Characterization ( IF 1.9 ) Pub Date : 2020-09-24 , DOI: 10.1080/1023666x.2020.1821151
Ljiljana Jeremic 1 , Andreas Albrecht 1 , Martina Sandholzer 1 , Markus Gahleitner 1
Affiliation  

Abstract High-impact copolymers of propylene and ethylene are complex materials with several components and at least two different phases, a crystalline polypropylene (PP) matrix and a predominantly amorphous ethylene–propylene copolymer (EPC) normally present as disperse particles. Next to overall composition analysis and morphology studies, fractionation into crystalline and amorphous components followed by further analysis of those components is the most important characterization technique for this technically very relevant class of copolymers. This process, involving separation into xylene cold-soluble (XCS) and insoluble fractions and follow-up determination of intrinsic viscosities (IV) as well as ethylene (C2) content is, however, tedious and time-consuming. A far more rapid approach is presented here through the separation of the amorphous and crystalline fractions of PP in 1,2,4-trichlorobenzene (TCB) using the crystallization extraction technique and the Crystex QC instrument. As the standard methods and Crystex technique are using different solvents (xylene and decalin versus TCB), correlations need to be established in order to be able to compare the results. Based on nine structurally very different polymers, respective correlation curves were developed and predictions for 95% confidence intervals were calculated statistically. In addition, these correlation curves were validated by testing over 100 different PP samples covering a broad range of all tested characteristics. The results show agreement and comparability between the traditional test methods techniques and the Crystex technique inside statistically calculated prediction intervals at 95% over a broad range of all tested characteristics (XCS, C2 and IV).

中文翻译:

通过结晶萃取分离快速表征高抗冲乙烯-丙烯共聚物组合物:与标准分离方法的可比性

摘要 丙烯和乙烯的高抗冲共聚物是具有多种组分和至少两个不同相的复杂材料,即结晶聚丙烯 (PP) 基质和通常以分散颗粒形式存在的主要是无定形的乙烯-丙烯共聚物 (EPC)。除了整体组成分析和形态研究之外,分馏成结晶和无定形组分,然后对这些组分进行进一步分析,是这种技术上非常相关的共聚物类别的最重要表征技术。然而,该过程涉及分离成二甲苯冷溶物 (XCS) 和不溶物部分以及特性粘度 (IV) 和乙烯 (C2) 含量的后续测定,但既繁琐又耗时。通过使用结晶萃取技术和 Crystex QC 仪器分离 1,2,4-三氯苯 (TCB) 中 PP 的无定形和结晶级分,这里提出了一种更快速的方法。由于标准方法和 Crystex 技术使用不同的溶剂(二甲苯和十氢化萘与 TCB),因此需要建立相关性以便能够比较结果。基于九种结构非常不同的聚合物,开发了各自的相关曲线,并对 95% 置信区间的预测进行了统计计算。此外,这些相关曲线通过测试 100 多个不同的 PP 样品进行了验证,这些样品涵盖了广泛的所有测试特性。
更新日期:2020-09-24
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