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连续自成核退火热分级技术在分析聚丙烯缺陷结构的分布中的应用及优化

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

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【作者】 亢健杨锋陈金耀曹亚李惠林向明

【Author】 KANG Jian,YANG Feng,CHEN Jin-yao,CAO Ya,LI Hui-lin,XIANG Ming *(State Key Laboratory of Polymer Materials Engineering,Polymer Research Institute of Sichuan University,Chengdu 610065,China)

【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

【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(iPP)方面的应用较少。本文深入研究了iPP的自成核结晶熔融行为,得到了iPP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Ts1、在自成核温度(Ts)的停留时间、相邻Ts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iPP来说,理想的SSA热分级条件为:Ts1=167℃,ts=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 iPP was designed,and the influence of important parameters(the first thermal treatment temperature Ts1;holding time ts;temperature gap between adjacent Ts,ΔT;fractionation temperature region) on the fractionation results and efficiency,were thoroughly studied.The results showed that,for iPP samples,the optimal thermal parameters are Ts1=167℃,ts=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
【Key words】 SSAPolypropyleneStereo-defect distribution
  • 【文献出处】 高分子通报 ,Polymer Bulletin , 编辑部邮箱 ,2013年09期
  • 【分类号】TQ325.14
  • 【被引频次】5
  • 【下载频次】467
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