Crystallization kinetics and equilibrium melting temperature of poly(ether ketone ketone) with high terephthalate content utilizing fast scanning calorimetry
Crystallization kinetics and equilibrium melting temperature of poly(ether ketone ketone) with high terephthalate content utilizing fast scanning calorimetry
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利用快速扫描量热法研究高对苯二甲酸酯含量聚醚酮酮的结晶动力学和平衡熔融温度
DOI：
10.1016/j.polymer.2023.125810
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发表时间：
2023
期刊：
影响因子：
4.6
通讯作者：
Moore, Robert B.
中科院分区：
文献类型：
--
作者：
Pomatto, Michelle E.;Moore, Robert B.
使用快速扫描量热法（FSC）分析结晶动力学，并测定对苯二甲酸酯/对苯二甲酸酯（T/I）比为80/20的KEPSTAN PEKK 8001（PEKK 80/20）的平衡熔融温度（Tmo）。收集KEPSTAN 8001和KEPSTAN 7002的定量1H、定性13 C和2D HSQC NMR光谱，以确认线性拓扑结构和共聚单体组成。利用FSC，首次利用间断等温结晶法在200 °C至310 °C的大温度范围内报告了PEKK 80/20的等温结晶动力学。PEKK 80/20的结晶动力学表现出抛物线行为，在260 °C下发生最快速的结晶。与具有较低T/I比的PEKK共聚物的早期研究（即，PEKK 70/30和60/40），观察到PEKK 80/20的结晶快达1至2个数量级（即，以常规DSC无法达到的速率）。使用零熵产生温度（TZEP）测定PEKK 80/20的Tmoof，首次允许准确测定382 °C的平衡熔融温度。将该值与加热速率范围（500 K/s -20，000 K/s）内的传统Hoffman-Weeks线性外推法进行比较，以阻止加热时的熔体重组。由于在使用常规DSC的缓慢加热扫描期间不可避免的晶体重组，Tmousing FSC的该新值显著高于通常参考的文献值368 °C。讨论了PEKK 80/20等温结晶后观察到的双熔融峰行为，并将其理解为是由于在相对缓慢的加热速率下加热期间的重组，如常规DSC通常观察到的那样。
Fast scanning calorimetry (FSC) was used to analyze the crystallization kinetics and determine the equilibrium melting temperature (Tmo) of KEPSTAN PEKK 8001 (PEKK 80/20) with a terephthalate to isophthalate (T/I) ratio of 80/20. Quantitative1H, qualitative13C and 2D HSQC NMR spectroscopy for KEPSTAN 8001 and KEPSTAN 7002 were collected to confirm linear topology and comonomer composition. Utilizing FSC, the isothermal crystallization kinetics for PEKK 80/20 are reported for the first time over a large temperature range from 200 °C to 310 °C utilizing an interrupted isothermal crystallization method. The crystallization kinetics of PEKK 80/20 exhibits parabolic behavior with the most rapid crystallization occurring at 260 °C. Compared to earlier studies of PEKK copolymers with lower T/I ratios (i.e., PEKK 70/30 and 60/40) using conventional DSC, PEKK 80/20 is observed to crystallize up to 1 to 2 orders of magnitude faster (i.e., at rates inaccessible with conventional DSC). The Tmoof PEKK 80/20 was determined utilizing the zero-entropy-production temperature (TZEP) allowing for the first time an accurate determination of the equilibrium melting temperature of 382 °C. This value was compared to a traditional Hoffman-Weeks linear extrapolation over a range of heating rates (500 K/s – 20,000 K/s) to arrest melt-reorganization upon heating. Due to unavoidable crystalline reorganization during slow heating scans with conventional DSC, this new value for Tmousing FSC is significantly higher than the commonly referenced literature value of 368 °C. The double melting peak behavior observed after isothermal crystallization of PEKK 80/20 is discussed and understood to be due to reorganization during heating at relatively slow heating rates, as commonly observed with conventional DSC.
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聚（芳基醚酮）及其共聚物的晶体形态和相鉴定。
影响因子：
5.5
作者：
R. Ho;Stephen Z. D. Cheng;B. Hsiao;K. Gardner
通讯作者：
K. Gardner
影响因子：
4.4
作者：
Al Lafi, Abdul G.;Alsayes, Ghina
通讯作者：
Alsayes, Ghina
影响因子：
4.6
作者：
GARDNER, KH;HISAO, BS;FARON, KL
通讯作者：
FARON, KL
影响因子：
4.4
作者：
A. Toda
通讯作者：
A. Toda
DOI：
10.1016/b978-1-4377-4463-7.10004-1
发表时间：
2012-01-01
期刊：
PEEK BIOMATERIALS HANDBOOK
影响因子：
--
作者：
Reitman, Maureen;Jaekel, David;Kurtz, Steven M.
通讯作者：
Kurtz, Steven M.