采用流变学方法研究聚酰胺酸6FDA-TFDB溶液的降解行为

张恩菘; 代学民; 刘学; 杨文轲; 刘巍; 董志鑫; 邱雪鹏; 姬相玲

doi:10.11777/j.issn1000-3304.2017.17074

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采用流变学方法研究聚酰胺酸6FDA-TFDB溶液的降解行为

研究论文 | 更新时间：2021-01-27

- 采用流变学方法研究聚酰胺酸6FDA-TFDB溶液的降解行为
- Degradation Behavior of 6FDA-TFDB Poly(amic acid) Solution via Rheological Method
- 高分子学报 2017年第9期页码：1497-1505
- 作者机构：
  
  1.中国科学院长春应用化学研究所高分子物理与化学国家重点实验室
  2.高分子复合材料工程实验室长春 130022
  3.中国科学院大学北京 100049
- 作者简介：
  
  姬相玲, E-mail:xlji@ciac.ac.cnXiang-ling Ji, E-mail:xlji@ciac.ac.cn
- 基金信息：
  
  国家重点基础研究发展计划（973计划）(2014CB643604);国家自然科学基金(51173178)
- DOI：10.11777/j.issn1000-3304.2017.17074
  中图分类号：
- 纸质出版日期：2017-9-20，
  
  收稿日期：2017-4-5，
  
  修回日期：2017-5-25，
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张恩菘, 代学民, 刘学, 杨文轲, 刘巍, 董志鑫, 邱雪鹏, 姬相玲. 采用流变学方法研究聚酰胺酸6FDA-TFDB溶液的降解行为[J]. 高分子学报, 2017,(9):1497-1505.

En-song Zhang, Xue-min Dai, Xue Liu, Wen-ke Yang, Wei Liu, Zhi-xin Dong, Xue-peng Qiu, Xiang-ling Ji. Degradation Behavior of 6FDA-TFDB Poly(amic acid) Solution via Rheological Method[J]. Acta Polymerica Sinica, 2017,(9):1497-1505.
张恩菘, 代学民, 刘学, 杨文轲, 刘巍, 董志鑫, 邱雪鹏, 姬相玲. 采用流变学方法研究聚酰胺酸6FDA-TFDB溶液的降解行为[J]. 高分子学报, 2017,(9):1497-1505. DOI： 10.11777/j.issn1000-3304.2017.17074.

En-song Zhang, Xue-min Dai, Xue Liu, Wen-ke Yang, Wei Liu, Zhi-xin Dong, Xue-peng Qiu, Xiang-ling Ji. Degradation Behavior of 6FDA-TFDB Poly(amic acid) Solution via Rheological Method[J]. Acta Polymerica Sinica, 2017,(9):1497-1505. DOI： 10.11777/j.issn1000-3304.2017.17074.

摘要

合成了一种聚酰胺酸6FDA-TFDB溶液，利用流变仪研究其在不同影响因素（如：温度、升温速率、溶剂含水量等）下的流变行为，发现聚酰胺酸溶液的降解在高温区和低温区存在不同的行为.通过Andrade公式获得不同条件下聚酰胺酸溶液的黏流活化能，并比较其差异，同时对溶剂水含量在不同温度区域下对聚酰胺酸降解速率的影响也进行了深入的分析，从而建立一种半定量比较不同条件下聚酰胺酸溶液降解速率的方法.

Abstract

As a precursor of polyimide

poly(amic acid) (PAA) has significant influence on the properties of the final materials. The stability of PAA solution under different conditions is also important to control the properties of PI. In this work

soluble 6FDA-TFDB PAA was synthesized and its solution was obtained. Using FTIR

H-NMR and GPC techniques

the molecular information of PAA was obtained. The degradation behavior was investigated by rheometer under different conditions (temperature

heating rate

water content

etc

.). It was found that the degradation rate in a high temperature region was much faster than that in a low temperature region

and a critical temperature was found to exist between these two temperature regions. Influence of added water amount in PAA solution on degradation behavior was also considered. In order to analyze precisely the influence of water amount on PAA degradation behavior

the amount of water in DMAc was analyzed by Karl Fischer method and demonstrated that it was too small to influence the relevant results. It was found that water accelerated the degradation rate of PAA solution in the low temperature region

but was irrelevant in the high temperature region. Based on Andrade equation

the viscous-flow activation energy was obtained and compared to evaluate the degradation rate of PAA in solution under different conditions

through a semi-quantitative way. Different results were found at low/high storage temperatures:at low storage temperature the viscosity of PAA solution was kept constant at first

then increased to a maximum and finally decreased; at high storage temperature it decreased gradually to a low value and remained constant. Based on degradation mechanism of PAA chains

the degradation behavior under different conditions was explained. This work provides a guide to tune the solution properties of PAA

and also to control the properties of polyimide materials.

关键词

聚酰胺酸降解行为流变仪黏度黏流活化能

Keywords

Poly (amic acid)Degradation behaviorRheometerViscosityViscous-flow activation energy

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