含不溶组分的聚烯烃材料分子结构和交联度原位测量技术

刘琳; 刘煦; 冯留海; 任冬雪; 于佩潜; 俞越; 陈林枫; 丛蓉娟

doi:10.11777/j.issn1000-3304.2026.26200

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含不溶组分的聚烯烃材料分子结构和交联度原位测量技术

研究论文 | 更新时间：2026-11-03

- 含不溶组分的聚烯烃材料分子结构和交联度原位测量技术
- In situ Characterization of Molecular Structure and Crosslinking Degree in Polyolefin Materials Containing Insoluble Components
- 高分子学报 2026年页码：1-11
- 作者机构：
  
  北京低碳清洁能源研究院北京 102201
- 作者简介：
  
  通信作者:E-mail: 20098502@ceic.com
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2026.26200
  中图分类号：
- 收稿：2026-06-04，
  
  录用：2026-07-31，
  
  网络首发：2026-11-02，
- 稿件说明：
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刘琳, 刘煦, 冯留海, 任冬雪, 于佩潜, 俞越, 陈林枫, 丛蓉娟. 含不溶组分的聚烯烃材料分子结构和交联度原位测量技术. 高分子学报, doi: 10.11777/j.issn1000-3304.2026.26200.

Liu, L.; Liu, X.; Feng, L. H.; Ren, D. X.; Yu, P. Q.; Yu, Y.; Chen, L. F.; Cong, R. J. In situ characterization of molecular structure and crosslinking degree in polyolefin materials containing insoluble components. Acta Polymerica Sinica (in Chinese), doi: 10.11777/j.issn1000-3304.2026.26200.
刘琳, 刘煦, 冯留海, 任冬雪, 于佩潜, 俞越, 陈林枫, 丛蓉娟. 含不溶组分的聚烯烃材料分子结构和交联度原位测量技术. 高分子学报, doi: 10.11777/j.issn1000-3304.2026.26200. DOI： CSTR： 32057.14.GFZXB.2026.7714.

Liu, L.; Liu, X.; Feng, L. H.; Ren, D. X.; Yu, P. Q.; Yu, Y.; Chen, L. F.; Cong, R. J. In situ characterization of molecular structure and crosslinking degree in polyolefin materials containing insoluble components. Acta Polymerica Sinica (in Chinese), doi: 10.11777/j.issn1000-3304.2026.26200. DOI： CSTR： 32057.14.GFZXB.2026.7714.

摘要

聚烯烃因其成本低廉、性能易于通过分子结构及组成按需调控等优势，广泛应用于人类生活的多个领域. 然而，聚烯烃材料中常含有无机杂质或后期添加多种助剂和无机填料等，在采用高温液相色谱法测试聚烯烃分子结构及分布时，这些物质(杂质)必须先通过高温趁热过滤有效地分离剔除，从而极大地增加了测试难度. 为避免样品中的杂质影响测试结果和损坏仪器(如色谱柱，检测器)，本研究提出了一种原位分析方法，通过引入过滤组件，实现样品高温溶解与杂质的分离过程同步进行. 该方法仅需在样品制备阶段人工使用金属过滤组件包裹样品，其余测试流程均由仪器自动完成，操作简便、流程高效. 通过对含碳黑和含杂质的聚烯烃样品测试，结果表明，该方法具有优异的分离效果和实际可行性. 在测试过程中仪器(如泵压)运行保持正常，对颗粒物极其敏感的光散射信号稳定，且测试数据具有良好的重复性和准确度. 此外，该过滤组件还可应用于交联聚乙烯样品交联度的测定，单个样品平均测试时间仅为54 min，相较于ASTM D2765-16标准方法至少24 h的测试周期，效率显著提升. 该方法也为聚乙烯氧化效应分析及含不溶组分的其他聚合物体系中的表征原位测试提供了新途径.

Abstract

Polyolefin products are extensively utilized across numerous sectors of human life thanks to their low cost and tunable properties through molecular structure engineering. However

the existence of various additives and inorganic fillers

purposefully or unintentionally added into the polyolefins during synthesis and subsequent fabrication process

has been a challenge for all of high-temperature liquid chromatographic techniques. Removal of these impurities

via

bench-top high-temperature filtration prior to the actual chromatographic analyses significantly increases analytical complexity. Herein

in situ

analytical method integrating sample dissolution and impurity separation

via

a customized Filter Assembly is proposed. Only the initial sample preparation requires manual operation

whereas all subsequent experimental procedures may be automatically implemented

endowing the method with simplicity and high efficiency. Experimental results demonstrated that the proposed strategy can effectively eliminate impurity interference

and deliver accurate and well-reproducible data. Furthermore

this innovation is also suitable for quantifying the degree of cross-linking in cross-linked polyethylene samples with or without inorganic filler. The average testing time per sample is shortened to 54 min

in sharp contrast to the minimum 24 hour required by the standard ASTM D2765-16 method. Moreover

this developed approach provides a promising alternative for investigating the oxidation behavior of polyethylene and the characterization of other po

lymer systems containing insoluble components in the target solvent system.

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