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材料研究学报  2009, Vol. 23 Issue (3): 242-250    
  研究论文 本期目录 | 过刊浏览 |
1H固体核磁共振技术对管材用Cr系催化剂催化乙烯共聚物及不同耐压等级管材料的研究
历伟1;严小伟1;王靖岱1;阳永荣1;Alina Buda2; Blumich BERNHARD2
1.浙江大学化学工程与生物工程学系 杭州 310027
2. Institute of Technical and Macromolecular Chemistry; WTH Aachen University; Worringerweg 1; 52074 Aachen; Germany
Cr-catalyzed ethylene copolymers studied by solid-state 1H NMR techniques: the influence of hexene content and different duration grades polyethylene pipe
LI Wei 1;  YAN Xiaowei 1;  WANG Jingdai 1;  YANG Yongrong 1; Alina BUDA 2; Blumich BERNHARD 2
引用本文:

历伟 严小伟 王靖岱 阳永荣 Alina Buda Blumich BERNHARD. 1H固体核磁共振技术对管材用Cr系催化剂催化乙烯共聚物及不同耐压等级管材料的研究[J]. 材料研究学报, 2009, 23(3): 242-250.
, , , , , . Cr-catalyzed ethylene copolymers studied by solid-state 1H NMR techniques: the influence of hexene content and different duration grades polyethylene pipe[J]. Chin J Mater Res, 2009, 23(3): 242-250.

全文: PDF(975 KB)  
摘要: 

以基于Cr系催化剂、不同己烯含量的管材用乙烯己烯共聚物为研究对象, 应用1H固体NMR技术测定了其室温下的相结构参数以及不同温度下的相结构变化. 研究发现, 随着共聚单体含量的增加, NMR结晶相组分的含量降低,  界面区和无定形区组分含量增加, 且两者在NMR测定的长周期中所占的比例也增加. 提出了以界面区含量和无定形区含量的比例随温度的变化作为定性判断非晶区中链段运动受限程度的依据. 此外, 采用相同的1H固体NMR技术研究了不同耐压等级聚乙烯管材料基体树脂的聚集态结构. 发现室温下随着管材料耐压等级的增加, 结晶相组分含量减少而其他两组分含量增加, 且NMR测定的长周期中结晶相组分所占比例降低而其他两组分比例升高. 实验结果证明, 上述定性判断非晶区中链段运动受限程度的判据与材料的耐压等级有较好的对应关系.

关键词 材料检测与分析技术1H固体核磁共振聚乙烯管材料聚集态结构己烯含量    
Abstract

Using different  1H solid--state NMR techniques, the Cr--catalyzed ethylene--hexene copolymer with different hexene content was investigated, and the effects of comonomer content on the phase composition, molecular
mobility and domain size of the copolymer were studied. The results showed that the mass fraction of crystalline phase was decreased with the hexene content increasing, while the fractions of the other two components were
increased. Meanwhile, the fraction of the interface and amorphous component was increased in the NMR long period. Furthermore, we choose the variance of MI/MA , the ratio of mass fraction of interface component to the fraction of amorphous component, with temperature as the qualitative determination of the confined degree of the segment in non--crystalline  region. Cr--catalyzed PE copolymer for pipe application with different duration grade was investigated. It was found that the mass fraction of rigid component decreased with the duration-grade increasing, while the fractions of the other two components increased. The same trend of the fraction in NMR long period was illustrated by the 1H spin diffusion result. The variance of  MI/MA showed great correspondence to the duration grade of the materials.

Key wordsmeasurement and analysis for materials    1H solid-state NMR    ethylene--hexene copolymer    phase structure   
hexene content
收稿日期: 2008-11-11     
ZTFLH: 

TG111

 
基金资助:

国家自然科学基金20676114、20490205, 国家高技术研究发展计划2007AA030208, 浙江省自然科学基金Y406293资助项目, CSC--DAAD(PPP, 2004)合作项目.

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