Application and Optimization of Successive Self-nucleation and Annealing Fractionation on the Analysis of iPP Tacticity

Jian KANG; Feng YANG; Jin-yao CHEN; Ya CAO; Hui-lin LI; Ming XIANG

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Application and Optimization of Successive Self-nucleation and Annealing Fractionation on the Analysis of iPP Tacticity

更新时间：2022-09-18

- Application and Optimization of Successive Self-nucleation and Annealing Fractionation on the Analysis of iPP Tacticity
- Polymer Bulletin Vol. 26, Issue 9, Pages: 168-176(2013)
- 作者机构：
  
  四川大学高分子材料工程国家重点实验室，四川大学高分子研究所，成都　610065
- 作者简介：
- 基金信息：
- DOI：
  CLC：
- Published：2013-09，
  
  Received：23 May 2013，
  
  Revised：01 July 2013，
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Jian KANG, Feng YANG, Jin-yao CHEN, Ya CAO, Hui-lin LI, Ming XIANG. Application and Optimization of Successive Self-nucleation and Annealing Fractionation on the Analysis of iPP Tacticity. [J]. Polymer Bulletin 26(9):168-176(2013)
DOI：

Jian KANG, Feng YANG, Jin-yao CHEN, Ya CAO, Hui-lin LI, Ming XIANG. Application and Optimization of Successive Self-nucleation and Annealing Fractionation on the Analysis of iPP Tacticity. [J]. Polymer Bulletin 26(9):168-176(2013) DOI：

摘要

连续自成核退火热分级法(SSA)具有制样简单、无需溶剂、测试耗时较短、设备较廉价等优点

在乙烯/α-烯烃共聚物等领域取得了广泛的应用

是表征其分子结构规整性分散情况的有力研究方法

但它在等规聚丙烯(

PP)方面的应用较少。本文深入研究了

PP的自成核结晶熔融行为

得到了

PP自成核行为的温度范围

并在此基础上深入研究了SSA热分级法的各个条件(首个自成核温度T

、在自成核温度(T

)的停留时间、相邻T

温度间隔ΔT、SSA分级温度范围等)对最终SSA热分级能力、分级时间的影响

建立了SSA热分级的实验条件与分级效率、分级能力之间的联系。结果表明

对于多数

PP来说

理想的SSA热分级条件为:T

=167℃

=15min

ΔT=4℃

升降温速率=20℃/min

热分级温度范围167~139℃。其中

扫描温度范围对分级效率的影响最大。对于具有不同规整度的PP来说

须有针对性选择上述关键参数

才能达到分级效率与分级能力的平衡。

Abstract

Owning to the advantages such as easy-sampling

free of solvent

high efficiency and relative low cost of the required instruments

Successive Self-nucleation and Annealing (SSA) fractionation has been widely applied in the analysis of ethylene/α-olefin copolymers. However

it has rarely been successfully applied in the analysis of PP. In this study

the self-nucleation behavior of PP had been studied. Based on the results

obtained

a SSA thermal protocol for

PP was designed

and the influence of important parameters (the first thermal treatment temperature T

; holding time t

; temperature gap between adjacent T

ΔT; fractionation temperature region) on the fractionation results and efficiency

were thoroughly studied. The results showed that

for

PP samples

the optimal thermal parameters are T

=167℃

=15min

ΔT=4℃

cooling/heating rate=20℃/min

fractionation temperature region=167-139℃. The variation of fractionation temperature region plays a most important role in determining the efficiency of SSA. For iPP with different tacticity

one must flexibly modify the parameters above

to achieve a balance between efficiency and fractionation results.

关键词

SSA热分级聚丙烯立构缺陷分布

Keywords

SSAPolypropyleneStereo-defect distribution

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Shandong Provincial Key Laboratory of Olefin Catalysis and Polymerization, Key Laboratory of Rubber-Plastics (Ministry of Education), School of Polymer Science and Engineering, Qingdao University of Science and Technology

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